NMR Mann

1
NMR Spectroscopy in the Liquid and Gas Phase

BY B.E. MANN
Introduction
In order to reduce the length of individual chapters, this report on NMR Spectroscopy has been divided into two chapters: Solution and Gas Phase NMR Spectroscopy and Solid-state NMR Spectroscopy. FolloTiving the criteria established in earlier volumes, only books and reviews directly relevant to this chapter are included, and the reader who requires a complet 2 list is referred to the Specialist Periodical Reports Nuclear Magnetic Resonance, where a complete list of books and reviews is given. Reviews which are of direct relevance to a section of this Report are included in the beginning of that section rather than here. Papers where only H, *H, I3C,I9F,and/or P NMR spectroscopy is used are only included when they make a non-routine contribution, bu.: complete coverage of relevant papers is still attempted where nuclei other than these are involved. Several reviews have been published which are relevant to this review: Connectivitks in molecules by INADEQUATE: recent developments, which contains Si and IX3W NMR spectra,2 Temperature measurements using nuclear magnetic; resonance, which describes various thermometers based on IH, I3C, I5N, Sn and 207Pb,3 Multiquantum filters and order in tissue, which contains 23NaNMR ~pectroscopy,~ Applications of advanced experimental techniques: high pressure NMR and computer sim~lations,~ NMR relaxation as a 2H method for characterisation and study of transition metal hydride systems in solution,6 NMR relaxation studies of polynuclear hydrides derivative^',^ A Half-century of nonclassical organometallic chemistry: A personal perspective,* NMR studies of metal complexes and clusters with carbonyls and phosphines,
Nuclear Magnetic Resonance, ed. G.A. Webb (Specialist Periodical Reports), The Royal Society of Chemistry, Cambridge, 2002, Vol. 31; 2003, Vol. 32. J. Buddrus and J. Lambert, Magn. Reson. Chem., 2002,40,3. A.G. Webb, Ann. Rep. N M R Spectrosc., 2002,45, 1. G. Navon, H. Shinar, U. Eliav and Y. Seo, N M R in Biomedicine, 2001,14, 112. L. Helm and A.E. Merbach, J . Chem. Soc., Dalton Trans., 2002,633. V.I. Bakhmutov, Rec. Adv. Hydride Chem., 2001,375. S. Aime, W. Dastru, R. Gobetto and A. Viale, Rec. Adz:. Hydride Chem., 2001, 351. F.A. Cotton, Znorg. Chem., 2002,41,643. B.T. Heaton, Mod. Coord. Chem., 2002,89.
Spectroscopic Properties of Inorganic and OrganometallicCompounds, Volume 36 0The Royal Society of Chemistry, 2003
1
Spectroscopic Properties of Inorganic and Organometallic Compounds
Adventures in organometallic NMR: steric restraints, slowed rotations, and skeletal rearrangements, Applications of pulsed-gradient spin-echo (PGSE) diffusion measurements in organometallic chemistry, Metal ion-assisted interactions involving biological molecules. From small complexes to metalloproteins,12 l13Cd and 207PbNMR spectroscopic studies of calcium-binding proteins,l3 Local and band susceptibility on JC-d hybridised organic-inorganic system disclosed by site-selective NMR,I4 and Relaxation and dynamics of molecules in the liquid crystalline phases? A number of papers have been published which are too broadly based to fit into a later section and are included here. NMR chemical shifts have been calculated for H2,N2,NH3, CH4,C2H4, HCN, MeCN and H20. The magnetic shielding has been calculated for [CO3l2-, [NO3]-, [SO,]- and [N3]-.17 Ca(N5)2and Calculated and experimental 15N shifts of NaN5, KN5, Mg(N5)2, Zn(N& have been reported.ls 31P and 35ClPGSE diffusion studies have been applied to phosphine ligands and selected organometallic complexes. The lWHg and 207Pb NMR correlation times from direct determination of l19Sn,195Pt, spin-lattice and spin-spin relaxation times has been described.203He, B, 21Ne, 27Aland 69GaNMR chemical shifts have been calculated for icosahedral closoborane, -alane and -gallane dianions with endohedral noble gas atoms and their lithium salts.21The nuclear magnetic shielding polarisabilitiesof N2, F2, CO, HF, HCl, HCN, HNC and C2H2have been computed.22 The 19F NMR chemical shieldings of M1F2,M1 = Zn, Cd, Pb, M2F3,M2 = Al, Ga, In, and SnF4,have been studied by the GIAO-B3LYP method.23
Stereochemistry
This section is subdivided into eleven parts which contain NMR information about Groups 1 and 2 and transition-metal complexes presented by Groups according to the Periodic Table. Within each Group, classification is by ligand type.
lo
l2 l3 l4 l6 l7 l9
2o
21
22
23
M.J. McGlinchey, Can. J . Chem., 200479, 1295. M. Valentini, H. Ruegger and P.S. Pregosin, Helu. Chim. Acta, 2001,84,2833. 0.Yamauchi, A. Odani and S. Hirota, Bull. Chem. Soc. Jpn., 2001,74,1525. T.E. Clarke and H.J. Vogel, Methods Mol. Biol. (Totowa, N.J.), 2002,173,205. A. Kawamoto, K. Miyagawa and K. Kanoda, Kotai Butsuri, 2002,37,326. R.Y. Dong, Prog. Nucl. Magn. Reson. Spectrosc., 2002,41,115. T. Kupka, B. Rusk and R.E. Botto, J . Phys. Chem. A, 2002,106,lO 396. M. Grayson, J. Mol. Struct., 2002,602603,429. L.A. Burke, R.N. Butler and J.C. Stephens, J . Chem. Soc., Perkin Trans. 2,2001,1679-1684. E. Martinez-Viviente, H. Ruegger, P.S. Pregosin and J. Lopez-Serrano, Organometallics, 2002,21, 5841. W.R. Carper, Z. Meng and N.M. Palko, J . Mol. Liq., 2002, % ) I 7. ! , ! O.P. Charkin, N.M. Klimenko, D. Moran, A.M. Mebe, D.O. Charkin and P.V. Scheyer, Inorg. Chem., 2001,40,6913. A. Rizzo and J. Gauss, J . Chem. Phys., 2002,116,869. S.H. Cai, Z. Chen, Z.W. Chen and H.L. Wan, Chem. Phys. Lett., 2002,362,13.
1 : N M R Spectroscopy in the Liquid and Gas Phase
Complexes of Groups 1 and 2. - s7Rb-'29Xe spin exchange and relaxation rates have been measured at high pressure and high magnetic field.24'J('H-'H) and 3J(M-X)coupling constants have been examined as fingerprints for hydrogen bond type.25The 7Li NMR spectra of [Li2C4Ph2(SiMe3)2]indicate that the two lithium atoms are considerably shielded by the ring current.26 NMR data have also been reported for [LiBu"], (6Li),27 [LiCH2-2-( 1-Me-imidazole)], (6Li),2 [Li(THF),] [Li{ C(SiR3)Ph2}2], (7Li, 29Si),2 [CuLi2R2(CN)], (6Li),30 [({ (S)-a-(PhCHMe)(CH2CH= CHLi)N})L&, (7Li),3 [LiButLiCsH3-2,6-(C6H2' 2,4,6-Pr'3)2], (7Li),32[MLi2XAr2], (M = Cu, Ag, Au; 6Li),33 (l), (7Li),34 [Li{ Si({NCH2Bu'}2C6H4-1,2)R}L], 29Si),35( B ~ ~ ~ M e s i ) ~ M L i=, Si, Ge; (7Li, [ (M l 29Si),36 [Na{ C(SiMe3)Ph2}],,(23Na, 29Si),37 [Cs(PC4Me4)],(133Cs).38 and
2.1
pi
6Li'H HOESY experiments have shown that in (2), lithium prefers the fivemembered chelate while sodium prefers the six-membered hel late.^' I5N T I measurements have been used to study Li' binding to the nitrogens in polyphosphazene~.~' 7Li'H HOESY has been applied to probe solvent-celluloseinteractions in cellulose di~solution.~' relaxation characteristics in the 1 7 0 NMR The spectra of Na+ and K + water clusters have been reported.4223Naand 3'PNMR
24 25
26
27
28
29 30 31 32
33
34
35
36 31
38
39 40 41
C.V. Rice and D. Raftery, J. Chem. Phys., 2002,117,5632. J.E. Del Bene, S.A. Perera, R.J. Bartlett, I. Alkorta, J. Elguero, 0. Mo and M. Yanez, J. Phys. Chem. A , 2002,106,9331. A. Sekiguchi, T. Matsuo and M. Tanaka, Organometallics, 2002,21, 1072. J.L. Rutherford, D. Hoffmann and D.B. Collum, J. Am. Chem. SOC.,2002,124,264. S.O. Nilsson Lill, D. Pettersen, M. Amedjkouh and P. Ahlberg, J. Chem. SOC.,Perkin Trans. I , 2002,3054. M.S. Hill and P.B. Hitchcock, Organometallics, 2002,21, 220. M. Yamanaka, S. Mori and E. Nakamura, Bull. Chem. SOC.Jpn., 2002,75,1815. P.C. Andrews, S.M. Calleja and M. Maguire, J. Chem. SOC.,Dalton Trans., 2002,3640. N.J. Hardman, B. Twamley, M. Stender, R. Baldwin, S. Hino, B. Schiemenz, S.M. Kauzlarich and P.P. Power, J . Organomet. Chem., 2002,643,46 1. C.M.P. Kronenburg, J. Jastrzebski, J. Boersma, M. Lutz, A.L. Spek and G. van Koten, J. Am. Chem. SOC.,2002,124,ll 675. C.M. Cui, J.A.R. Schmidt and J. Arnold, J. Chem. Soc., Dalton Trans., 2002,2992. X.P. Cai, B. Gehrhus, P.B. Hitchcock, M.F. Lappert and J.C. Slootweg, J. Organomet. Chem., 2002,643,272. M. Nakamoto, T. Fukawa, V.W. Lee and A. Sekiguchi, J. Am. Chem. Soc., 2002,124,15 160. M.S. Hill and P.B. Hitchcock, J . Organomet. Chem., 2002,664, 182. F. Nief and L. Ricard, J. Organomet. Chem., 2002,642,208. A. Johansson, G. Hilmersson and 0. Davidsson, Organometallics, 2002,21,2283. T.A. Luther, M.K. Harrup and F.F. Stewart, ACS Symp. Ser., 2003,834,409. E. Brendler, S. Fischer and H. Leipner, Cellulose (Dordrecht, Neth.), 2001,8,283.
spectra have been used to study the time course of myocardial sodium accumulation after burn trauma.43 The phase behaviour of a mixture of phospholipid bicelles has been investigated using 2H, 23Naand 31P NMR s p e c t r o ~ c o p y'H ~ .~ and 13CNMR chemical shifts have been calculated for Ag+, K + and Rb+ salts of hydroorotate (2,6-dioxo-1,2,3,6-tetrahydropyrimidine-4-carboxylate) anion.45 ''Rb MRI has been used to follow Rb+ uptake in pig hearts.46 NMR data have also been reported for [Li4B(N-2-pyridyl)3(NH-2-pyridyl)(THF)3],' 1B),47 (7Li, [LiMg(NPr'2)2(OR)]2, (7Li),48 [Ar,(NSiMe3)2Li],, (29Si),49 [PhCH2NLiN(SiMe3)CH2Ph], (7Li,29Si),50 [Li{ ~ - N ( s i M e ~ ) ~ }N(SiMe3)2}], (7Li),5 ~Ca{ [Li{ Si[(NCH2B~t)2C6H4-R}(THF)2], (7Li, 29Si),5 [(C6H41,2] 1-OMe-2NSiMe3)Li(OEt2)12, (7Li),53 [(BU'~S~FL~NBU')~(OE~~)], (29Si),54 [l,S{(Me3SiN)Li(THF)}2CloH6], (7Li, 29Si),55[{Me2Si(2,6-Pri2C6H3)NLi}2]2, ('Li, 29Si),56[2-PhC6H4NLi2In, [2-PhC6H4N{B(NMe2)2}2],[2-PhC6H4N(SiMe3)2], (7Li, "B, 29Si), [Li{ N(C6H3Me2-2,6)CC( SiMe3)Si( SiMe3)2N(C6H3Me2(7Li),5 [Li2{ C6H4- ,3-(CH2NC6H3-2,6-Pri2)2}], (7Li),5 1 2,6)}(tmeda)], [Yb{ (N{SiMe3}CPh)2CH-pLi(THF)}2], (7Li,29Si),60 Me2(MeO)SiNC(Ad)[Li{ CHSiMe3}2], (7Li, 29Si),61 [Li2(THF){ P(O)(NBU')~(NHBU')}]~, (7Li),62 (7Li, (3), 29Si),63 [CyPSe3Li2(tmeda)2], (77Se),64 [(THF)2Li2{ ~ P ( S ~ ) ( N B U ' ) ~(7Li,, P }~] 77Se),65 [Li(tmeda)*][T~(NBu')P(~-NBu')~P(NBu')T~], (7Li, 125Te),66 [ { A S ( N B U ~ ) ~ ) ~ ( '~ ~iI ) , ~ ~ L ~ , [{ S~(P-NCY)~(P-N)}~{ Li(THW3], ( 7 ~ i ,1 4 W 8
G.R. Okroyan, D.F. Kushnarev, G.A. Kalabin and A.G. Proidakov, J . Struct. Chem., 2002, 43, 242. " P.J. Sikes, P. Zhao, D.L. Maass and J.W. Horton, J . A p p l . Physiol., 2002,91,2695. 44 C.B. Tan, B.M. Fung and G.J. Cho, J . Am. Chem. SOC., 2002,124,ll 827. 4 5 S. Bekiroglu and 0. Kristiansson, J . Chem. SOC., Dalton Trans., 2002, 1330. 46 V.V. Kupriyanov, B. Xiang, J. Sun, 0.Jilkina, G. Dai and R. Deslauriers, Magn. Res. Med., 2001, 46,963. 47 U. Braun, T. Habereder, H. Noth, H. Piotrowski and M. Warchhold, Eur. J . Znorg. Chem., 2002, 1132. 48 K.J. Drewette, K.W. Henderson, A.R. Kennedy, R.E. Mulvey, C.T. O'Hara and R.B. Rowlings, Chem. Commun., 2002,1176. 49 C. Knapp, E. Lork, P.G. Watson and R. Mews, Znorg. Chem., 2002,41,2014. 5 0 H. Sachdev and C. Preis, Eur. J . Znorg. Chem., 2002,1495. A.R. Kennedy, R.E. Mulvey and R.B. Rowlings, J . Organomet. Chem., 2002,648,288. s 2 X.P. Cai, B. Gehrhus, P.B. Hitchcock, M.F. Lappert and J.C. Slootweg, J . Organomet. Chem., 2002,651,149. 53 G.B. Deacon, C.M. Forsyth and N.M. Scott, Eur. J . Znorg. Chem., 2002,1425. s4 M. Jendras, U. Klingebiel and M. Noltemeyer, J . Organomet. Chem., 2002,646, 134. " L.H. Gade, C.H. Galka, K.W. Hellmann, R.M. Williams, L. De Cola, I.J. Scowen and M. McPartlin, Chem.-Eur.J., 2002, 8, 3732. 5 6 M.S. Hill and P.B. Hitchcock, Organometallics, 2002,21,3258. " C. Neumann, A. Schulz, T. Seifert, W. Storch and M. Vosteen, Eur. J . Znorg. Chem., 2002, 1040. '* R.J. Bowen, M.A. Fernandes, P.B. Hitchcock, M.F. Lappert and M. Layh, J . Chem. SOC.,Dalton Trans., 2002,3253. 5 9 S. Daniele, P.B. Hitchcock, M.F. Lappert, T.A. Nile and C.M. Zdanski, J . Chem. SOC.,Dalton Trans., 2002, 3980. 6 o A.G. Avent, A.V. Khvostov, P.B. Hitchcock and M.F. Lappert, Chem. Commun., 2002,1410. 6 1 F. Antolini, B. Gehrhus, P.B. Hitchcock and M.F. Lappert, Angew. Chem., Znt. Ed. Engl., 2002,41, 2568. A. Armstrong, T. Chivers, M. Krahn, M. Parvez and G. Schatte, Chem. Commun., 2002,2332. 6 3 H. Sachdev, C. Wagner, C. Preis, V. Huch and M. Veith, J. Chem. SOC.,Dalton Trans., 2002,4709. 64 R.P. Davies and M.G. Martinelli, Znorg. Chem., 2002,41, 348. G.G. Briand, T. Chivers, M. Krahn and M. Parvez, Znorg. Chem., 2002,41,6808. 6 6 G.G. Briand, T. Chivers and M. Parvez, Angew. Chem., Int. Ed. Engl., 2002,41,3468.
42
1: N M R Spectroscopy in the Liquid and Gas Phase
[M{ N(SiMe3) CC6H3-2,6-Me2}2SiSiMe3], = (29Si),69 Li+ in polyacrylonitrilebased electrolytes, (7Li),70 containing lipophilic nucleosides, (7Li),7 [{(2-0-4Li ' Me-q~inoline)Li}~(THF)~], (7Li),72 Li-crown ether complexes, (7Li),73 [M3L3], {M = Li, Na; L = (4); 7L1,23Na},74 [LisK6M(Pr'3SiP)6(0SiMe3)2], = Sr, Ba; (M 7Li,29Si),75( B u ' ~ S ~ O ) ~(29Si),76 Cs+ in phosphonato cavitands, (133Cs).77 [ N ~ ~ ] ,and
2.2 Complexes of Group 2. - Two relevant reviews have appeared: '43CaNMR of calcium-binding protein^'^ and 'Shape and dynamics of calcium-binding protein investigation by I5NNMR ela ax at ion'.^^ The quadrupole moments of 41Caand 4'Sc have been determined.80 Evidence of a near-critical solvation effect on rotational correlation time of 'Be NMR TIof [Be(acacb] has been obtained in liquid and supercritical C02.81 The 'H and I3C NMR signals of bacteriochlorophyll a have been assigned.82 NMR chemical shifts of [ML,], M = Mg, Ca, Sr, Ba, L = [2,6-Pri2C6H3NCMeCHCMeNC6H32,6-Pr12]- point to increased ionicity of the ligand-metal bond in the order M g < c a < S ~ - < B MgC12has been shown to be an efficient relaxation agent for a.~~ amino acids and some carboxylic acids.84NMR data have also been reported for Be" [Be40{OC(O)Ph},], ('Be, '70),8s complexes of 3-HO-1,2-Me2-4-pyridone
67 68 69 70 71 72 73 74 75 76 77
78 79 80
81 82
83
84
A. Bashall, A.D. Bond, A.D. Hopkins, S.J. Kidd, M. McPartlin, A. Steiner, R.Wolf, A.D. Woods Dalton Trans., 2002, 343. and D.S. Wright, J. Chem. SOC., F. Garcia, D.J. Linton, M. McPartlin, A. Rothenberger, A.E.H. Wheatley and D.S. Wright, J. Chem. SOC., Dalton Trans., 2002,481. J.D. Farwell, P.B. Hitchcock and M.F. Lappert, Chem. Commun., 2002,456. H. Tsutsumi, K. Takase, Y. Sumiyoshi, K. Onimura and T. Oishi, Solid State Ionics, 2002, 147, 317. M. Cai, X. Shi, V. Sidorov, D. Fabris, Y.-f. Lam and J.T. Davis, Tetrahedron, 2002,58, 661. S.T. Liddle and W. Clegg, J. Chem. SOC.,Dalton Trans., 2002,3923. E. Karkhaneei, M.H. Zebrajadian and M. Shamsipur, J. Inclusion Phenom. Macrocyclic Chem., 2001,40,309. M. Capo, J.M. Saa and A. Alvarez, Chem. Commun., 2002,1982. M. Westerhausen, S. Weinrich, G. Kramer and H. Piotrowski, Inorg. Chem., 2002,41,7072. H.W. Lerner, S. Scholz and M. Bolte, Organometallics, 2002,21, 3827. P. Delangle, J.-C. Mulatier, B. Tinant, J.-P. Declercq and J.-P. Dutasta, Eur. J . Org. Chem., 2001, 3695. T. Drakenberg, Methods Mol. Biol. (Totowa, N . J . ) , 2002, 173,217. J.M. Werner, I.D. Campbell and A.K. Downing, Methods Mol. Biol.(Totowa, N.J.), 2002, 173, 285. T. Minamisono, K. Matsuta, K. Minamisono, S. Kudo, M. Ogura, S. Fukuda, K. Sato, M. Mihara, M. Fukuda, S. Takeda and S.Y. Zhu, 2. NaturSorsch., A: Phys. Sci., 2002,57, 595. T. Umecky, M. Kanakubo and Y. Ikushima, J . Phys. Chem. B, 2002,106,11 114. Z.Y. Wang, Y. Muraoka, M. Shimonaga, M. Kobayashi and T. Nozawa, J. Am. Chem. Soc., 2002, 124,1072. S. Harder, Organometallics, 2002,21,3782. J.P. Tian, Y.W. Yin, H.B. Sun and X.F. Luo, J . Magn. Reson., 2002,159,137.
Spectroscopic Properties o Inorganic and Organometallic Compounds f

+
and 1-(3-H0-2-furanyl)ethanone, (9Be),86 Be2 complexes of [(02P)3(NH)3]3-, (9Be),87 [(Me2NNSiMe3)2Mg], and (29Si).88 2.3 Complexes of Group 3, the Lanthanides, and Actinides. - The quadrupole moment of 41Sc,89 the magnetic moment of 48Sc,90 and have been determined. Three isomers of [Tm/Cg2] have been studied by I3C NMR ~pectroscopy.~~ 1J(89Y3'P)= 144 Hz and *J(31P'H) = 201 Hz in [(THF){1,3{P ].~~ NMR chemical shifts have been cal(Me3Si)2C5H3}2YH ( S ~ B U ' ~ ) )235U culated for some diamagnetic uranium corn pound^.^^ NMR data have also been reported for [{HB(~,~-Bu',M~-C~HN~)~}Y~(~-D)]~, (2H, '71Yb),94 [Li(THF)4] [Yb{CH(SiMe3)2}3], (7Li, 29Si, 17'Yb),95 [Y(q5:q'-C5Me4CH2SiMe2NBu')(p-2C4H30)]2, (89Y),96 [(q5-C5Hs)2Y { N(SiMe3)2PPh2}2CH2], (29Si),97 [(q6-3,5Me2C5H3BNMe2)2Y( p-C1)2Li]2, (7Li, 1B),9 [( { (Et2CH2CH2NCMe)2CH} MgBr)2ScBr], (45Sc),99[Sc(a~ac)~( p-Cy7Si802)]2, (29Si),1 [ScX,( OPMe3)6-,]3-", O0 (45Sc),101 [Y{(p-OPt)2M(OPri)4}3], (M = Nb, Ta; 89Y),102 and [Yb(NPh)2(THF)4],(171Yb).103 2.4 Complexes of Group 4. - The 'H and 13Cchemical shifts of [(q5-C5H5)2Zr(pMe)AlMe3][Me2A10] and [(q5-C5H5)2ZrMe] [Me2A10] have been calculated and compared with e~periment."~ The size of the ion pair, [(q5-C5H5)2Zr(pMe)A1Me3][Me2A10], has been determined by PFG NMR spectroscopy.105
R.J.F. Berger, M.A. Schmidt, J. Juselius, D. Sundholm, P. Sirsch and H. Schmidbaur, 2.Naturforsch., B: Chem. Sci., 2001,56,979. 86 F. Cecconi, C.A. Ghilardi, A. Ienco, P. Mariani, C. Mealli, S. Midollini, A. Orlandini and A. Vacca, Inorg. Chem., 2002,41,4006. 87 H. Maki, M. Tsujito, H. Nariai, M. Watanabe, M. Sakurai and T. Miyajima, Phosphorus Res. Bull., 2001,12, 155; H. Maki, M. Tsujito, H. Nariai, M. Watanabe, M. Sakurai and T. Miyajima, Phosphorus Res. Bull., 2001,12, 161. 88 H. Sachdev, Eur. J. Inorg. Chem., 2002,2681. 89 S . Kudo, S. Fukuda, K. Sato, M. Mihara, M. Fukuda, K. Matsuta and T. Minamisono, K U R R I f KR-74, Proceedings o the Specialist Research Meeting on New Developments in Solid State Physics with Probes o Radiations and Nuclei, 2001,2001,96. f 90 Y. Kawamura, M. Sasaki, S. Watanabe, S. Ohya, T. Ohtsubo, J. Goto, S. Muto and T. Izumikawa, KURRI-KR-74, Proceedings o the Specialist Research Meeting on New Developments in Solid f State Physics with Probes of Radiations and Nuclei, 2001,2001,76. 91 T. Kodama, N. Ozawa, Y. Miyake, K. Sakaguchi, H. Nishikawa, I. Ikemoto, K. Kikuchi and Y. Achiba, J. Am. Chem. Soc., 2002,124,1452. 92 M. Westerhausen, S. Schniederbauer, M. Hartmann, M. Warchhold and H. Noth, 2. Anorg. Allg. Chem., 2002,628,330. 93 G. Schreckenbach, Inorg. Chem., 2002,41,6560. 94 G.M. Ferrence and J. Takats, J. Organomet. Chem., 2002,647,84. 95 P.B. Hitchcock, A.V. Khvostov and M.F. Lappert, J. Organomet. Chem., 2002,663,263. 96 S. Arndt, A. Trifonov, T.P. Spaniol, J. Okuda, M. Kitamura and T. Takahashi, J. Organomet. Chem., 2002,647,158. 97 M.T. Gamer and P.W. Roesky, J. Organomet. Chem., 2002,647,123. 98 B. Wang, X.L. Zheng and G.E. Herberich, Eur. J. Inorg. Chem., 2002,31. 99 A.M. Neculai, D. Neculai, H.W. Roesky, J. Magull, M. Baldus, 0. Andronesi and M. Jansen, Organometallics, 2002,21,2590. 100 V. Lorenz, A. Fischer and F.T. Edelmann, J. Organomet. Chem., 2002,647,245. 101 N.J. Hill, W. Levason, M.C. Popham, G. Reid and M. Webster, Polyhedron, 2002,21,1579. 102 S. Mishra, U.M. Tripathi, A. Singh and R.C. Mehrotra, J. Chin. Chem. SOC.(Taipei), 2002,49, 335. 103 P.B. Hitchcock, A.V. Khvostov, M.F. Lappert and A.V. Protchenko, J. Organomet. Chem., 2002, 647, 198. 104 E. Zurek and T. Ziegler, Organometallics, 2002,21,83.
85
'H-'H TOCSY and 'H-IH NOESY have been used to study the structures of a series of substituted indenyl titanium and zirconium complexes.' O6 The reactivity of some substituted cyclopentadienyl zirconium chloride/[MeAlO], towards H2 has been correlated with 91Zrchemical shifts.'07 'H-'H NOESY has been used to identify [{q5-1-(2-MeOC6H4)-indenyI)zZrC121.108 is a correlation There of 13CNMR and IR data for a zirconacyclopropene.'09 The coordinative interaction of various organoaluminiums with [ZrC14] has been studied using 'H and 27Al NMR spectroscopy.'" NMR data have also been reported for [(q5CSHS)Z~(C"-H)~BCSH~~], ("B),"' [Ti(CH2SiMe3)(NMe2){ MeN(CH2-2(29Si, pyrrole)2}], ( 14N),'' [MeSi{ SiMe2N(C6H4-4-Me)}3SnZr(q5-C5H5)2Me], ' 19Sn), ' [ I Z ~ ~ A ~ ( C L ~ - O ) ( ~ - O M ~ ) ~ C ~(27Al),1T H[(q5-C5Me5)Hf(q4' ~ M ~ (l4 F ) ~ ] , ' C ~ H I O ) ( C H ~ S ~ M ~ ~ ) ] ' (5), (29Si),1 [{(Me3Si)2N}(C2H4Si2Me4N)("Si),' , T~(CSCR)~], I5N, 29Si),"7 [(2,6-PrL2C6H3)N ("B, = Hf(THF)2(SiPh3)2], (29Si),1 ' [(q5-C5H3C5H8)2Ti(q2-Me3SiCICSiMe3)], (29Si),' 9 (6), (15N),'2o [(q5-C5H5){q5l (Et3SiCH2CH2)3SiC5H4}TiC12], (29Si),'21( ) (15N),122 (29Si),123 7, (8), [(q5-C5H5)(OC)*FeCH2SiMe20ZrCl(q5-C5H5)2], (29S1),124 [(q5-C5H5)2Zr(lr-02BC6H2-2,4,6Me3)], (1'B),'25[(q5-C5Me5)(q6-C5H5BCH =CHPh)ZrC12], (I'B),126(9),(''B),127 [ThTi2( p-O)(p3-OEt)8(OEt)2], (205Tl),1 [{ 9-(Me3Si)fl~orenyl)~O~ 2(TiOB~f)4], (29Si),' 9 [(H2C = CH)Cy6Si7Ol2TiOPr'],(29si),' [ ( Z ~ ~ N C I I ~ ) C ("N),'~31, 2 30 ~~] and [(Me2NCH2CH2NMe2)HfC12{ Si(SiMe3)3}], (29Si).32 '
'05
'06 '7 0
'08
log 'lo
''I
''' 'I4 '' '' '' '

12'
l9
120
122
123
124
125
126
127
128 129
'30
13'
D.E. Babushkin and H.H. Brintzinger, J. Am. Chem. SOC.,2002,124,12 869. Y.-H. Yu, W. Xia, H.-Y. Ma, X.-C. Tao, J.-L. Huang and Y.-L. Qian, Huaxue Xuebao, 2002,60, 347. R. Blom, 0.Swang and R.H. Heyn, Macromol. Chem. Phys., 2002,203,381. H.Y. Ma, J.L. Huang and Y.L. Qian, J. Organomet. Chem., 2002,650,114. F.X. Buzin, F. Nief, L. Ricard and F. Mathey, Organometallics, 2002,21,259. Y. Shiraki, Y. Nakamoto and Y. Souma, J. Mol. Catal. A: Chem., 2002,187,283. E.R. Ding, F.-C. Liu, S.M. Liu, E.A. Meyers and S.G. Shore, Inorg. Chem., 2002,41,5329. Y.H. Li, A. Turnas, J.T. Ciszewski and A.L. Odom, Inorg. Chem., 2002,41,6298. M. Lutz, M. Haukka, T.A. Pakkanen and L.H. Gade, Organometallics, 2002,21,3477. P. Sobota, S. Przybylak, J. Utko and L.B. Jerzykiewcz, Organometallics, 2002,21, 3497. C. Visser, A. Meetsma and B. Hessen, Organometallics, 2002,21, 1912. H.S. Sun, V.V. Burlakov, A. Spannenberg, W. Baumann, P. Arndt and U. Rosenthal, Organometallics, 2002,21,3360. B. Wrackmeyer, A. Pedal1 and J. Weidinger, J. Organomet. Chem., 2002,649,225. I. Castillo and T.D. Tilley, J. Organomet. Chem., 2002,643,431. M. HoraEek, P. StpniEka, S. Gentil, K. Fejfarova, J. Kubita, N. Pirio, P. Meunier, F. Gallou, L.A. Paquette and K. Mach, J. Organomet. Chem., 2002,656,81. C. Holtke, G. Erker, G. Kehr, R. Frohlich and 0.Kataeva, Eur. J . Inorg. Chem., 2002,2789. R. Andris, E. de Jesus, F.J. de la Mata, J.C. Flores and R. Gomez, Eur. J. Inorg. Chem., 2002, 228 1. D. Huerlander, R. Frohlich and G. Erker, J . Chem. SOC.,Dalton Trans., 2002,1513. H.G. Alt, R. Ernst and I.K. Bohmer, J. Organomet. Chem., 2002,658,259. M. Hofmann, W. Malisch, D. Schumacher, M. Lager and M. Nieger, Organometallics, 2002,21, 3485. J.E. Balkwill, S.C. Cole, M.P. Coles and P.B. Hitchcock, Inorg. Chem., 2002,41,3548. B.Y. Lee and G.C. Bazan, J. Organomet. Chem., 2002,642,275. A.J. Ashe, tert., H. Yang, X.D. Fang and J.W. Kampf, Organometallics, 2002,21,4578. T.J. Boyle, C.A. Zechmann, T.M. Alam, M.A. Rodriguez, C.A. Hijar and B.L. Scott, Inorg. Chem., 2002,41,946. H.M. Lindemann, M. Schneider, B. Neamann, H.G. Stammler, A. Stammler and P. Jutzi, Organometallics, 2002,21,3009. M.D. Skowronska-Ptasinska, M.L.W. Vcrstenbosch, R.A. van Santen and H.C.L. Abbenhuis, Angew. Chem., Int. Ed. Engl., 2002,41,637. X.-B. Xie and T. Hughbanks, Inorg. Chem., 2002,41, 1824.
(q5-C5Me5)CI,Zr VN
"3
Complexes of Group 5. - The 31P and "V NMR spectra of [BU'S~(CH~PM~~)~V(CO)~(NO)] coupling.' 3 3 NMR data have also show "V been reported for [(2,6-mes2C6H3N )(2,6-mes2C6H3NH)Ta{ = Si(SiMe3)3}CI], [MeB(C6F5)3]-, ("B, 29Si),134 [Si(CHzCH2CH2SiMe{ CH2CH2CH2SiMe(CH2CH2CH2SiMe2-4-C5H4NNbC12{q5-C5H4SiMe3})2}2)4], (11C),136 (29Si),1 (lo), (ll), (11B),137 (12), (7Li),138 [(Me2N)3Ta{Si(SiMe3)3}Cl], (29Si),139 [($C5H5)Ta( NBu')(NHBu')Cl], = (I5N),l4O [(q5-C5Me5)TaCl{ N(C6H3-2,6= Pri2)}Si(SiMe3)3] [Li(THF)3]+, and ('Li, 29Si).141 The I4N NMR signals of the terminal and bridging imido groups of some imidovanadium complexes show marked differences in their lineshapes that could be used as an additional criterion for signal assignment.142NMR data have also been reported for [(A~Bu~N)~V(NCE~)N~(THF)~], S; s1V),143 (E = 0,
132 133 134 135
2.5
136 137 138 139
140 141 142
143
D. Frank, J. Baumgartner and C. Marschner, Chem. Commun., 2002,1190. T.W. Hayton, P.J. Duff, P. Legzdins, S.J. Rettig and B.O. Patrick, Inorg. Chem., 2002,41,4114. J. Gavenonis and T.D. Tilley, Organometallics, 2002,21, 5549. J.M. Benito, E. de Jesus, F.J. de la Mata, J.C. Flores, R. Gomez and P. Gomez-Sal, J . Organomet. Chem., 2002,664,258. K.S. Cook, W.E. Piers and R. McDonald, J. Am. Chem. Soc., 2002,124,5411. K.S. Cook, W.E. Piers, P.G. Hayes and M. Parvez, Organometallics, 2002,21,2422. J.A.R. Schmidt and J. Arnold, Organometallics, 2002,21, 3426. Z.Z. Wu, H. Cai, X.H. Yu, J.R. Blanton, J.B. Diminnie, H.J. Pan and Z.L. Xue, Organometallics, 2002,21,3973. M.C. Burland, T.W. Pontz and T.Y. Meyer, Organometallics, 2002,21,1933. U. Burckhardt, G.L. Casty, J. Gavenonis and T.D. Tilley, Organometallics, 2002,21,3108. D. Gudat, U. Fischbeck, F. Tabellion, M. Billen and F. Preuss, Magn. Reson. Chem., 2002, 40, 139. J.K. Brask, V. Dura-Vila, P.L. Diaconescu and C.C. Cummins, Chem. Commun., 2002,902.
I: N M R Spectroscopy in the Liquid and Gas Phase
(10)
(11)
(12)
(13), (5'V),'44 1: complexes between aryl hydroxamic acids and vanadate, (15N, 51V),145 [VO(C6H4-1-0-2-CH = NCH2C02)(1,2-02C6H4)], (51V),146vanadyl complexes of 2-C5H4NCH= NNHCS2CH2Ph, (51V),147 [NbL(p-"N)Li(THF)I2, (L = tridentate aryloxy ligand, 15N),'48 (14), (29Si).'49 and
(13)
(14)
Lithiation of [{ (V0)2(0H)2(C404)(phen)2}H20]n been confirmed by 'Li has NMR spectroscopy.' 5 0 Ion pairing between [Bun4N] and [V3O9I3-has been demonstrated by "V NMR spectroscopy.' 5 1 1 0 7 NMR spectroscopy has been used to estimate the oxygen-central ion binding in the products of hydrolysis of [MF,], M = Nb, Ta, As, Sb.152NMR data have also been reported for chiral terpene-derived vanadatranes, ("N, 1 7 0 , "V),' 53 [VO(02)(heida)]-, ("V), 5 4 [VO(benzohydroxamato),], (51V),1 [V02] +, (51V),'5 6 [V02(maltolate)2]-, (51V),157KloHSLn(PMoSW4V2039)2'nH20r (51V),'58KloH5Ln(PMo7W2V2039)2*
+
144 145 146 147 148 149 1 so 151 152 153 154 155
156
157 158
M.R. Maurya, S. Khurana, W.J. Zhang and D. Rehder, J. Chem. SOC., Dalton Trans., 2002,3015. J.H. Bell and R.F. Pratt, Inorg. Chem., 2002,41,2747. B. Baruah, S. Das and A. Chakravorty, Inorg. Chem., 2002,41,4502. M.R. Maurya, S. Khurana, W.J. Zhang and D. Rehder, Eur. J. Inorg. Chem., 2002,1749. H. Kawaguchi and T. Matsuo, Angew. Chem., Int. Ed. Engl., 2002,41,2792. M.D. Fryzuk, B.A. MacKay, S.A. Johnson and B.O. Patrick, Angew. Chem.,Int. Ed. Engl., 2002, 41,3709. L.W. Huang, C.J. Yang and K.J. Lin, Chew.-Eur.J., 2002,8, 396. E.E. Hamilton, P.E. Fanwick and J.J. Wilker, J. Am. Chem. SOC.,2002, 124,78. E.G. Win, A.N. Zozulin and Y.A. Buslaev, Dokl. Phys. Chem., 2002,384,109. G. Wagner, R.Herrmann and A.J.L. Pombeiro, Znorg. Chim. Acta, 2002,336,147. T.S. Smith and V.L. Pecoraro, Znorg. Chem., 2002,41,6754. P. Yang, G.-Y.Han, X.-L. Jin and S.-R. Chen, Huaxue Xuebao, 2002,60,1072. X. Lu, Electrochim. Acta, 2001,46,428 1. B. Song, N. Aebischer and C. Orvig, Znorg. Chem., 2002,41,1357. B.-b. Zhou, H.-y. Ma, Y.-h. Wang, Y.-k. Shan and Y.-d. Wei, Zhongguo Xitu Xuebao, 2002,19, 393.
10
nH20, (51V), ' [VS( OSiPh3)3], ("V), '6o [Et4N]3[ { V2S202(S2CNEt2)2}2K], (5'v),161 [VS4CUn]n-,(51V),162 [V2S6CU6](PPh3)6,(51V).163 and
2.6 Complexes
of
Group
6.
The
H-H
distance
in
[{1,2-
C6H4(NSiMe3)2}Mo(=NPh)(H2)(PMe3)2] estimated from 'J('H2H) and has been
Tl(min). 64 The electron-donating potential of various trispyrazolyl borates and cyclopentadienyl ligands, L, has been studied by I3C NMR spectroscopy in [LW(CO)2(C=CR)].165 The alkyne 6(13C) chemical shifts for [W(q2RC=CR){S(2-0-3-R-5-MeGH2)2}C12] are at 233.1 to 244.5.' 66 The NMR chemical shifts of [ M o ( ~ ~ - C ~ H ~ ) ~ ] c a 1 c ~ l a t e d .Analysis of the 'H have been l~~ NMR spectrum of [(q6-C6H6)Cr(CO)3] has shown that the effective aromaticity is about 25% enhanced over that of benzene.168NMR data have also been reported for (15), ("B, 183W),169 [MoMe202L2],(170, 95M0),170 (16), (183W),'71 [(OC)5MInX(THF)],(M = Cr, Mo, W; "'In),' 7 2 [(q5-C5H5)(OC)3MSnC6H3-2,6C6H2-2,4,6-Me3], = Cr, Mo, W; 119Sn),'731-M1(C0)3(q4-SnM29)]4-, = (M [ (MI Cr, Mo, W; M2 = Sn, Pb; 9 5 M ~ , '17Sn, lI9Sn,207Pb),'74 (OC)5Cr}2Pb(PR3)21, [{ (207Pb),175(17), (15N),'76 [(q5-C5H5)2M02Fe3(CO)8(p3-Se)2(q5-CCPhCCPh) (77Se),177 (18), (95Mo),178 W(CO), complexes of diazaphospholes, (Ig3W),l9 7
159
'
160 161
162
163 164
165 166
167
168 169 170
171
172
173
174
175 176
177
178 179
B.-b. Zhou, Y.-h. Wang, H.-y. Ma, Y.-k. Shan, X.-q. Xu and Y.-d. Wei, Fenzi Kexue Xuebao, 2002,17,87. F. Preuss and P. Werle, Z . Naturforsch., B: Chem. Sci., 2002,57,726. H.P. Zhu, C.N. Chen, X.F. Zhang, Q.T. Liu, D.Z. Liao and L.C. Li, Znorg. Chim. Acta, 2002,328, 96. J.4. Ye, F.-k. Zheng, Z. Chen, H.-c. Xie, Z.-w. Chen and P.-q. Huang, Bopuxue Zazhi, 2001, 18, 315. F.-k. Zheng, G.-c. Guo, G.-w. Zhou, X. Zhang and J.-s. Huang, Jiegou Huaxue, 2001,20,489. T.M. Cameron, C.G. Ortiz, I. Ghiviriga, K.A. Abboud and J.M. Boncella, J. Am. Chem. Soc., 2002,124,922. B. Schwenzer,J. Schleu, N. Burzlaff, C. Karl and H. Fischer, J. Organomet. Chem., 2002,641,134. Y. Takashima, Y. Nakayama, H. Yasuda, A. Nakamura and A. Harada, J. Organomet. Chem., 2002,654,74. M. Kaupp, T. Kopf, A. Murso, D. Stalke, C. Strohmann, J.R. Hanks, F.G.N. Cloke and P.B. Hitchcock, Organometallics, 2002,21, 5021. R.H. Mitchell, Z. Brkic, D.J. Berg and T.M. Barclay, J . Am. Chem. SOC.,2002,124, 11 983. Z. Bajko, J. Daniels, S. Hap and M. Nieger, Organometallics, 2002,21, 5182. F.E. Kiihn. M. Groarke, 8. Bencze, E. Herdtweck, A. Prazeres, A.M. Santos, M.J. Calhorda, C.C. Romiio, I.S. Gongalves, A.D. Lopes and M. Pillinger, Chem.-Eur. J., 2002,8,2370; M. Groarke, I.S. Gongalves, W.A. Herrman and F.E. Kiihn, J. Organomet. Chem., 2002,649,108. A. Fuchs, D. Gudat, M. Nieger, 0. Schmidt, M. Sebastian, L. Nyulaszi and E. Niecke, Chem.-Eur. J.,2002,8,2188. P. Rutsch, G. Renner, G. Huttner and S. Sandhoefner, Z . Naturforsch., B: Chem. Sci., 2002,57, 757. B.E. Eichler, A.D. Phillips, S.T. Haubrich, B.V. Mork and P.P. Power, Organometallics, 2002,21, 5622. J. Campbell, H.P.A. Mercier, H. Franke, D.P. Santry, D.A. Dixon and G.J. Schrobilgen, Znorg. Chem., 2002,41,86. P. Rutsch and G. Huttner, 2. Naturforsch., B: Chem. Sci.,2002,57,25. B.M. Trost, K. Dogra, I. Hachiya, T. Emura, D.L. Hughes, S. Krska, R.A. Reamer, M. Palucki, N. Yasuda and P.J. Reider, Angew. Chem., Znt. Ed. Engl., 2002,41,1929. P . Mathur, M.O. Ahmed, J.H. Kaldis and M.J. McGlinchey, J. Chem. SOC.,Dalton Trans., 2002, 619. D. Gudat, S. Hap and M. Nieger, J. Organomet. Chem., 2002,643,181. L. Szarvas, Z. Bajko, S. Fusz, S. Burck, J. Daniels, M. Nieger and D. Gudat, 2. Anorg. Allg. Chem., 2002,628,2303.

Mo(C0)3 complexes of bis(2-picolyl)amine, C5M0),'8o [M0(CO)~(phenylazopyridine)21, (95M0),181 (19), (119Sn).182 and
+ PPh,
11
cis-
P- B' Ph2 H2
dPPh3
3J(31PMoMo31P)= 16 Hz through the Mo2 quadrupole bond in [Moz(OAc){N,N'-(2-MeOC6H4)2formamidinate}C12(PMe3)].' linear rela83 A tionship has been found between the 31P chemical shift and n in [W&&-n (PR3),].'84 The solvation of Li+ in the presence of [PMo12040]3-has been examined by 7LiNMR spectroscopy.l 8 A series of systematic DFT calculations have been conducted on [SiW9M304$, M = Mo, V, Nb, and 183W chemical shifts calculated.18631P 51VNMR spectroscopy has been used to show that and [a-P2W s062]6-, 3-P2W 8 \ 7 3 0 6 2 ] - and [a-P2W1 7 v 0 6 2 ] 7- are stable in [a1,2, 1 aqueous solution.' 87 The application of Is3W NMR spectroscopy to polyoxometallates has been discussed.188NMR data have also been reported for [(PI-'A~N)~Mo = N]-, ('5N),189 [Cr{ A1(OPri)4}2{Nb(OPr')6}],(27Al),190 =N [M o ( N C ~ H ~ - ~ , ~ - M ~ ~ ) ( S ~ C N E ~ 9'Mo),'9 ' [Mo402(p'SCH2C02)6' (I4N, ~ ) ~ ] ,
D.R. van Staveren, E. Bothe, T. Weyhermuller and N. Metzler-Nolte, Eur. J . Inorg. Chem., 2002, 1518. 181 M.N. Ackermann, S.R. Kiihne, P.A. Saunders, C.E. Barnes, S.C. Stallings, H.D. Kim, C. Woods and M. Lagunoff, Inorg. Chim. Acta, 2002,334,193. 18' J. Heinicke, K. Steinhauser, N. Peulecke, A. Spannenberg, P. Mayer and K. Karaghiosoff, Organometallics, 2002,21,912. 1 8 3 Y.Y. Wu, J.D. Chen, L.S. Liou and J.C. Wang, Inorg. Chim. Acta, 2002,336,71. S. Jin, J. Adamchuk, B.S. Xiang and F.J. DiSalvo, J. Am. Chem. Soc., 2002,124,9229. 18' M. Takamoto, T. Ueda and S. Himeno, J. Electround. Chem., 2002,521,132. X. Lopez, C. Bo and J.M. Poblet, J. Am. Chem. SOC.,2002,124,12 574. 18' K. Nomiya, H. Torii,T. Hasegawa,Y. Nemoto, K. Nomura, K. Hashino, M. Uchida,Y. Kato, K. Shimizu and M. Oda, J. Inorg. Biochem., 2001,86,657. 188 Y. Chen, L. Qu and J. He, Huaxue Tongbao,2002,65, w53/1. J.P.F. Cherry, F.H. Stephens, M.J.A. Johnson, P.L. Diaconescu and C.C. Cummins, Inorg. Chem., 2001,40,6860. S . Mishra and A. Singh, Transition Met. Chem. (Dordrecht, Neth.), 2002,27,541.
180
-"'
12
(SCH2C02)2I4-, (95M0),'92 [H2ZnMo60 (OCH2)3CMe}2], (95Mo),1 18{ [Ti(OH2)-P2MoW16061]6-, (183W),'94[P2W18-nMOn062]6-, (183W),195 [(CeO)3(H20)2(As-W9034)12],(183W),'96 Fell', Pd" and Cu" complexes of [PW9034]9-, V", (51v, 183w),197 [(03,W I 1Si)Ln(02CCH2NH2)3Ln(SiW lo-, (183W),' 9 8 Sm 99 (M containing polyoxotungstosilicate, (183W),1 [{ (qS-CsHs)Ti}MW11039]n-, = B, Ga, Ge; 183W),200 peroxotitanium heteropoly complexes, (183W),201 [Si W11Ti040]6-, (183W),202 [(a- W10Ti2039)2] (183W),203 [P{Ti(02)}21,2-P lo-, w10038]'-, (183W),204 [SiWll(Nb02)039]5-, (183W),205 [GeWloMoNb040]-, (183W),206 PhCONH(CH2)3Si}20SiWl1039]4-, [RzMWi &In-, (M [{ (183W),207 = Si, Ge, B, Ga; 183W),208 [PW11039(0sN)]4-, (I5N, 183W),209 [AlW12040]5-, (183W),21 [{(qS-CsMes)Rh}(a-1,2' (27Al),210[a-(FeC1)2(FeOH2)P2W150~9]11-, P2w16v2062)]6-, ( V , 183W),212 [Cr(Te4)3]3-,(125Te).213 and
2.7 Complexes of Group 7. - 'H, NOESY and Tl NMR measurements show hydrogen bonding in (20).24 Density functional calculations of 55MnNMR l parameters have been r e p ~ r t e d . ~ " The 55Mnand '19Sn chemical shifts of [(4XC6H4)3SnMn(CO)5] correlate l6 The molecular size and purity of [(OC)4ReClL]4, L = [{ 5,15-(4-NC5H4C~C)2-10,20-(4-Eto*cc6H4)-por191
192 193 194 19s 196 197
198
199
200 201 202 203
204 205 206 207
208 209
210
211 212 213 214
21s 216
M. Minelli, M. Le Hoang, M. Kraus, G. Kucera, J. Loertscher, M. Reynolds, N. Timm, M.Y. Chiang and D. Powell, Znorg. Chem., 2002,41,5954. W.B. Yang, C.Z. Lu, S.F. Lu and H.H. Zhuang, Helu. Chim. Acta, 2002,85,2417. B. Hasenknopf, R. Delmont, P. Herson and P. Gouzerh, Eur. J . Inorg. Chem., 2002,1081. C. Ratiu, A.R. Tomsa, A. Koutsodimou, P. Falaras and T. Budiu, Polyhedron, 2002,21, 353. B. Keita, Y.Jean, B. Levy, L. Nadjo and R. Contant, New J . Chem., 2002,26,1314. L.-h. Bi, W.-h. Zhou and F.-t. Mu, Synth. React. Znorg. Met.-Org. Chem., 2002,32, 1127. L.G. Detusheva, L.I. Kuznetsova, M.A. Fedotov, V.A. Likholobov, L.S. Dovlitova, A.A. Vlasov and V.V. Malakhov, Russ. J . Coord. Chem., 2001,27,838. S.-y. He, D. Zhang, J.-s. Zhao, Y.-f. Wei, F.-x. Dong and Q.-z. Shi, Wuji Huaxue Xuebao, 2002,18, 171. S.-X. Liu, Y.-G. Li, Z.-B. Han, E.-B. Wang, Y. Zeng and Z.-L. Li, Gaodeng Xuexiao Huaxue Xuebao, 2002,23,777. X.Wang, J. Li, J. He and J. Liu, Metal-Based Drugs, 2001,8, 179. Q.-J. Shan, J. Gong and L.-Y. Qu, J . Coord. Chem., 2002,55, 319. R.-H. Ma, C.-T. Liu and L.-Y. Qu, Yingyong Huaxue, 2002,19,342. K. Nomiya, M. Takahashi, J.A. Widegren, T. Aizawa, Y. Sakai and N.C. Kasuga, J . Chem. SOC., Dalton Trans., 2002,3679. F.X. Gao, T. Yamase and H. Suzuki, J . Mol. Catal. A : Chem., 2002,180,97. R.-h. Ma, C.-t. Liu and L.-y. Qu, Wuji Huaxue Xuehao, 2002, 18,275. Q.Y. Wu, S.Wang, D. Li and X.F. Xie, Inorg. Chem. Commun., 2002,5,308. M. Li, P.Wu, X. Lin and E. Wang, Chemical Journal on Znternet [online computerjile], 2001,3, No pp. given. http://www.chemistrymag.org/cJi/2001/037033nc.htm. Z. Sun, J. Liu, J. Ma and J. Liu, Metal-Based Drugs, 2001,8,257. H. Kwen, S.Tomlinson, E.A. Maatta, C. Dablemont, R. Thouvenot, A. Proust and P. Gouzerh, Chem. Commun., 2002,2970. W.A. Neiwert, J.J. Cowan, K.I. Hardcastle, C.L. Hill and I.A. Weinstock, Znorg. Chem., 2002,41, 6950. T.M. Anderson, X.Zhang, K.I. Hardcastle and C.L. Hill, Znorg. Chem., 2002,41,2477. K. Nomiya, Y. Sakai and T. Hasegawa, J . Chem. SOC., Dalton Trans., 2002,252. P. Sekar and J.A. Ibers, Znorg. Chem., 2002,41,450. T. Beringhelli, G. D'Alfonso, M. Panigati, P. Mercandelli and A. Sironi, Chem.-Eur. J., 2002,8, 5340. M.Buhl, Theor. Chem. Acc. 2002,107,336. D. Christendat, I. Wharf, A.M. Lebuis, I.S. Butler and D.F.R. Gilson, Inorg. Chim. Acta, 2002, 329, 36.
1 : N M R Spectroscopy in the L q i and Gas Phase iud
13
phyrin}Zn] has been determined using pulsed field gradient NMR spectros c ~ p y . ~ ' second order 31P The NMR spectrum of [MeC(CH2PPh2)3Re(CO)2(q1P4X3)]+ has been analysed.218The magnetic shieldings of [Mn04]- have been calculated for 1 0 55Mn.219 31P 7 and The NMR spectrum of cis-[ReCl(NCHC6H44-X)(d~pe)~]+ been analysed as ABCD.220 NMR data have also been has ("B)," [Mn(C0)&(C6H4-4reported for [{(q5-C5H4Me)Mn(CO)2}2(p-BC1)2], Me)2H], (29Si),2 [MnCl(COh{PhP(CH2)2S(CH2)2S(CH2)2PPh2}], (5SMn),2 (21),224 [Tc(CNBU')~(PP~~)~]+, (99Tc),225and [Re6(p3-Se)s(PEt3)s(NCsH4-4CH2CH2-4-C5H4N)l2+, (77Se).226
H-N,
H -(OC),Re, , -1 H ?
-
N Re, Pe(CO), 7
H?CO),H
Se-seqse Se SeSi (OC),Re':#:'Re(C0)3
d,
2.8 Complexes of Group 8. - 'H TI measurements have been performed on [MH6I4-, M = Fe, R u . ~ 'A remarkably large geometry dependence of cal~ culated 57FeNMR chemical shifts has been reported.228DFT calculations of 9 9 Rchemical shifts with all-electron and effective core potential basis sets have ~ been published.229NMR spectroscopy has been used to observe trialkylphosphite-Pd" and Ru" complexes in supercritical C02.230 'H NMR spectrum of The [(qs-CsMeS)R~(H2)2(SbPh3)] shows a T1 corresponding to a H2 complex. 'J(2H'H) = 9.3 Hz.2313H NMR spectroscopy has been used to determine 'J(3H'H) in [(q5-C5H5)Ru{ R2P(CH2),PR2}(H2)]. 2 3 2 Replacement of the dppm + ligand in [{q5-CSH4(CH2)2NMe2H}Ru(dppm)H] two less donating P(OPh)3 with ligands reduces the strength of the intramolecular Ru-H - H-N dihydrogen
+
217 218 219 220 221 222 223 224 225 226 227 228 229 230 231 232
W.H. Otto, M.H. Keefe, K.E. Splan, J.T. Hupp and C.K. Larive, Inorg. Chem., 2002,41,6172. E. Guidoboni, 1. de 10s Rios, A. Ienco, L. Marvelli, C. Mealli, A. Romerosa, R. Rossi and M. Peruzzini, Inorg. Chem., 2002,41,659. M. Buhl, J . Phys. Chem. A , 2002,106,lO 505. M. da Silva, J. da Silva and A.J.L. Pombeiro, Inorg. Chem., 2002,41,219. H. Braunschweig, M. Colling, C.H. Hu and K. Radacki, Angew. Chem., Znt. Ed. Engl., 2002,41, 1359. R. Shiozawa, H. Tobita and H. Ogino, J . Organomet. Chem., 2002,650,91. B. Heuer, M.L. Matthews, G. Reid and M. Ripley, J. Organomet. Chem., 2002,655,55. A. Bacchi, W. Baratta, F. Calderazzo, F. Marchetti and G. Pelizzi, Inorg. Chem., 2002,41,3894. E. Freiberg, W.M. Davis, A. Davison and A.G. Jones, Inorg. Chem., 2002,41,3337. B.K. Roland, C. Carter and Z.P. Zheng, J. Am. Chem. Soc., 2002,124,6234; 9955. D.E. Linn, jun., G.M. Skidd and S.N. McVay, Inorg. Chem., 2002,41,5320. M. Buhl, F.T. Mauschick, F. Terstegen and B. Wrackmeyer, Angew. Chem., Int. Ed. Engl., 2002, 41,2312. A. Bagno and M. Bonchio, Eur. J. Inorg. Chem., 2002,1475. Y. Kayaki, T. Suzuki, Y. Noguchi, S. Sakurai, M. Imanari and T. Ikariya, Chem. Lett., 2002,424. H. Aneetha, M.J. Tenorio, M.C. Puerta and P. Valerga, J. Organomet. Chem., 2002,663,151. J.K. Law, H. Mellows and D.M. Heinekey, J. Am. Chem. Soc., 2002,124,1024.
14
bond.233The use of Ig70ss.atellitesubspectra in 'H and 31P{1H} NMR spectra of triosmium carbonyl clusters has been discussed.234 - * HM interactions in XH = CPh2)] [H(~-H)OS~(CO)~~(HN have been investigated using Tl measurem e n t ~ Similarly [H(~-H)OS~(CO)~~L] .~~~ derivatives were examined and 1870s NMR data reported.236There is a correlation between the 13CNMR chemical shift of the bridging carbon and 3J(1H1H) compounds such as (22).237 in The chemical shift of the CH of [(Cy3P)2C12Ru=CHER] inversely related to the is electronegativity of E.238 NMR data have also been reported for [(pH)M3(C0)9(C-CR)],(M = Ru, 0 s ; 29Si),239 (q5-C5H5)Fe(C0)2}2B(c6H2-2,4,6[{ Me3)], (' 1B),240 [(q5-C5H5)Fe(C0)2B(C6H2-2,4,6-Me3)Br], (1'B),241[(q5-C5H5)Fe(CO)2BClSi(SiMe3)3], ( B),242 [(q5-C5H5)Fe(C0)2B02C6H202BFe(CO)2(q 5C5H5)], (11B),243 [(q5-C5H4Me)Fe(C0)2B02C6C14], (11B),244 (23),(11B),245[(q5C5H5)Fe(C0)2SiMe20H],(29Si),246 [(q5-C5H5)Fe(CO)2Si(OMe)Ph2], (29Si),247 [(q5-C5H5)Fe(CO)2SiMePhCH2SiMe2CH2SiMe2Fe(CO)2(q5-C5H5)], (29Si),248 [{ (r15-C5H5)Fe(Co),}2siH(OH)], (29si),249 ( 1 - 5 5 F ( 0 } ( l C ) C - i 2 ] [{ r 5 C H ) e C ) 2 C - O ( L S H ) , (29Si),250 R u ( P P ~ ~ ) ~ ( C O ) C ~ ( S ~ M ~(29Si),251 ] , [ ~)~NM~ [(q5-C5H5)Ru(PR3)2SiX3], (29Si),252[(q5-C5Me5)Ru(CO)2SiMe2SiMe3], (29Si),253(24), (29Si),254[(q5C5H5)Ru(PPh3)2SnX3],('19Sn),255 (11B).256 and (25),
233 234 235
236 237 238 239 240 2 41 242 243 244 245 246
247 248 249 250 251 252 253 254 255
Y.F. Lam, C.Q. Yin, C.H. Yeung, S.M. Ng, G.C. Jia and C.P. Lau, Organometallics, 2002, 21, 1898. M.J. Stchedroff, S. Aime, R. Gobetto, L. Salassa and E. Nordlander, Magn. Reson. Chem., 2002, 40,107. S. Aime, E. Diana, R.Gobetto, M. Milanesio, E. Valls and D. Viterbo, Organometallics, 2002,21, 50. S . Aime, F. Bertone, R. Gobetto, L. Milone, A. Russo, M.J. Stchedroff and M. Milanesio, Inorg. Chim. Acta, 2002,334,448. T. Farrell, A.R. Manning, G. Mitchell, J. Heck, T. Meyer-Friedrichsen, M. Malessa, C. Wittenburg, M.H. Prosenc, D. Cunningham and P. McArdle, Eur. J. Inorg. Chem., 2002,1677. J. Louie and R.H. Grubbs, Organometallics, 2002,21,2153. F.J. Zuno-Cruz, A.L. Carrasco and M.J. Rosales-Hoz, Polyhedron, 2002,21, 1105. S . Aldridge, D.L. Coombs and C. Jones, Chem. Commun., 2002,856. D.L. Coombs, S. Aldridge and C. Jones, J. Chem. Soc., Dalton Trans., 2002,3851. H.Braunschweig, M. Colling, C. Kollann and U. Englert, J. Chem. Soc., Dalton Trans., 2002, 2289. S . Aldridge, R.J. Calder, A. Rossin, A.A. Dickinson, D.J. Willock, C. Jones, D.J. Evans, J.W. Steed, E.M. Light, S.J. Coles and M.B. Hursthouse, J. Chem. Soc., Dalton Trans., 2002,2020. S. Aldridge, R.J. Calder, R.E. Baghurst, M.E. Light and M.B. Hursthouse, J. Organomet. Chem., 2002,649,9. A. Wacker, C.G. Yan, G. Kaltenpoth, A. Ginsberg, A.M. Arif, R.D. Ernst, H. Pritzkow and W. Siebert, J. Organomet. Chem., 2002,641, 195. W .Malisch, M. Hofmann, G. Kaupp, H. Kap and J. Reising, Eur. J. Inorg. Chem., 2002,3235; W. Malisch, M. Hofmann, M. Nieger, W.W. Scholler and A. Sundermann, Eur. J . Inorg. Chem., 2002,3242. J.S. McIndoe and B.K. Nicholson, J. Organomet. Chem., 2002,648,237. Y.Q. Zhang and K.H. Pannell, Organometallics, 2002,21,503. W. Malisch, M. Vogler, D. Schumacher and M. Nieger, Organornetallics, 2002,21,2891. W. Malisch, M. Vogler, H. Kab and H.-U. Wekel, Organometallics, 2002,21,2830. T.N. Choo, W.-H. Kwok, C.E.F. Rickard, W.R. Roper and L.J. Wright, J. Organomet. Chem., 2002,645,235. S.T.N. Freeman, L.L. Lofton and F.R. Lemke, Organometallics, 2002,21,4776. M. Okazaki, K. Satoh, T.Akagi, M. Iwata, K.A. Jung, R. Shiozawa, H. Okada, K. Ueno, H. Tobita and H. Ogino, J. Organomet. Chem., 2002,645,201. H. Hashimoto, Y. Hayashi, I. Aratani, C. Kabuto and M. Kira, Organometallics, 2002,21,1534. E.M. Moura, H.G.L. Siebald and G.M. de Lima, Polyhedron, 2002,21,2323.
15
The 'H and 13Cchemical shifts of [(q5-C5H5)0s{q2-HC=CC(OH)R2}(PPri3)] + have been measured and ~ a l c u l a t e d . ~ ~ ' NMR data have been reported for 57Fe P) some sila-[ llferrocenophanes and a phospha-[ llferrocenophane. 25(57Fe31 = 3.4 Hz for [Fe(q5-C5H4)2PN(CMe2CH2)2CH2].258 of borylation of The products [Fe(q5-C5H4SnMe3)2] have been characterised using I1B and '19SnNMR spect r o ~ c o p y . ~ ' ~ has been applied to the study of ion pairing for [RuCl(q6PGSE arene)(Me-Duphos)]+.260 Detailed assignment of 'H and 13CNMR signals of [RuCI(L){ PPh2(CH2)3-q6-C6H5}] been reported.261 13Cchemical shifts for has the p3-C in complexes such as [{ C O ( ~ ~ - C ~ H ~ ) } ~ { Fe(CO)(CNR)2}(p3-S)(p3-CS)] are between 6 354 and 359.262Low frequency 'H chemical shifts and NOE cross peaks have been used to show that the dppz protons of (26) insert in d(GTCGAC)2.263 Thermal and solvent effects on 6(57Fe) [Fe(CN)5(NO)]2of and [Fe(CN)6]4- have been The 'H NMR signals of [C4HsN2Fe2(C0)6] have been completely assigned.26 NMR data have also been reported for [(q5-C5Mes)(OC)2FeAs{ C(N2)SiMe3}C(OSiMe3) CPh2}], { = (' ' B),2 C(q5-C5H5)Fe(q5(29Si),2 [(q5-C5H5)Fe{ q5-C5H4BH( y)}], bip
256
257
258
259
260
261
262
264
266
C.E.F. Rickard, W.R. Roper, A. Williamson and L.J. Wright, Organometullics, 2002, 21, 1714; 4862. J.J. Carbo, P. Crochet, M.A. Esteruelas, Y. Jean, A. Lledos, A. M. Lopez and E. Oiiate, Organometallics, 2002,21,305. B. Wrackmeyer, O.L.Tok, A. Ayazi, F. Hertel and M. Herberhold, 2.Naturforsch., B: Chem. Sci., 2002,57, 305. J.A. Gamboa, A. Sundararaman, L. Kakalis, A.J. Lough and F. Jakle, Organometullics, 2002,21, 4169. Y. Chen, M. Valentini, P.S. Pregosin and A. Albinati, Inorg. Chim. Acta, 2002,327,4. P.D. Smith, T. Gelbrich and M.B. Hursthouse, J. Organomet. Chem., 2002,659,l. A.R. Manning and A.J. Palmer, J. Organomet. Chem.,2002,651,60. A. Frodl, D. Herebian and W.S. Sheldrick, J. Chem. SOC.,Dalton Trans., 2002,3664. M. Biihl and F.T. Mauschick, Phys. Chem. Chem. Phys., 2002,4,5508. A. Zimniak, J. Organomet. Chem., 2002,645,274. L. Weber, L. Pumpenmeier, H.G. Stammler, B. Neumann and P. Lonnecke, J. Organomet. Chem., 2002.643,81.
16
C5H4CH2CO2SnBun3)I6,(119Sn),268 [(q5-C5H5)Fe{q5-CsH4-1-CH2NMe2-2si(CbH4-4-F)3}], (29Si),269[{(q5-C5H5)Fe(q5-CsH4COS)}2SnB~n2], (119Sn),270 [{ (q5-C5H5)Fe(q5-C5H4CH = CHC02SnBun2)}2],(' '9Sn),2 ferrocenyl amines bearing boryl and silyl substituents, (57Fe),272 [Fe(q5-C5H4n0CHPhCHPhO)2], (' 1B),27 [Fe{ q5-C5Me4GeSi(SiMe3)3}2], (29Si),2 [{q5-C5H4SnMe(C6H2-2,4,674 Me&}Fe{ q5-C5H4(p-AlMe2)2Me}],(27Al, '19Sn),275 [Fe(q5-C5H4)2SnB~'2], (' 19Sn),2 [(q5-C5H4)Fe{ q5-C5H4( SiMe2)3}],, (29Si),2 [(q5-C5Me5)Fe(q6,q6C5H5BMe)M(q5-C5H5)],'+, = Co, Ru, 0 s ; 11B),278 (M [(q6-PhC6Hs)Ru(en)C1]+, (1sN),279 [{(p-RTe)Fe2(Co),}2(p4-se)], (77Se,125Te),280 [{(p-RTe)Fe2(C0)6}2(p4S)], (' 25Te),28 [( OC)4Fe( p-dppm)PtC12( CNR)], (195Pt),282[Fe3( p3-E){p3Sb(C6H2Me3-2,4,6)}(COk], = Se, Te; 77Se, 125Te),283 (E and [Ru(6-0-5,8quinolinedione)(CO)3Cl], (' 5N), 84
2+
H02C -
(26)
57FeNMR chemical shifts and chemical shielding anisotropies have been calculated for some heme protein model systems.28s'H NMR spectroscopy has been used to detect immobilised water molecules within a strong distal hydro267
269
270
271
272
273
274 275
276
277
278
279 280
281
282
283
284
285
K.B. Ma, F.F. de Biani, M. Bolte, P. Zanello and M. Wagner, Organometallics, 2002,21,3979. V. Chandrasekhar, S. Nagendran, S. Bansal, A.W. Cordes and A. Vij, Organometallics, 2002,21, 3297. C. Beyer, U. Bohme, C. Pietzsch and G. Roewer, J . Organomet. Chem., 2002,654,187. W.-G. Lu and J.-X. Tao, Fenxi Ceshi Xuebao, 2002,21,70. W.-G. Lu, J.-X. Tao, X.-Y. Li and Y.-Z. Wang, Wuli Huaxue Xuebao, 2001,17,836. B. Wrackmeyer, H.E. Maisel and M . Herberhold, Z . Naturforsch., B: Chem. Sci., 2001,56, 1373. S. Aldridge, C. Bresner, LA. Fallis, S.J. Coles and M.B. Hursthouse, Chem. Commun., 2002, 740; 1158. W.P. Freeman, J.M. Dysard, T.D. Tilley and A.L. Rheingold, Organometallics, 2002,21,1734. T. Baumgartner, F. Jakle, R. Rulkens, G. Zech, A.J. Lough and I. Manners, J . Am. Chem. SOC., 2002,124,lO 062. A. Berenbaum, F. Jakle, A.J. Lough and I . Manners, Organometallics, 2002,21,2359. K . Temple, S. Dziadek and I . Manners, Organometallics, 2002,21,4377. A.R. Kudinov, D.A. Loginov, Z.A. Starikova and P.V. Petrovskii, J . Organomet. Chem., 2002, 649, 136. H.M. Chen, J.A. Parkinson, S. Parsons, R.A. Coxall, R.O. Gould and P.J. Sadler, J . Am. Chem. SOC.,2002,124, 3064. L.-c. Song, Q.-m. Hu, H.-t. Fan, M.-y. Tang and G.-1. Lu, Organometallics, 2002,21,2468. L.-c. Song, Q.-m. Hu, B.-w. Sun, M.-y. Tang, J. Yang and Y.-j. Hua, Organometallics, 2002, 21, 1627. M. Knorr, I. Jourdain, G. Crini, K. Frank, H. Sachdev and C. Strohmann, Eur. J . Inorg. Chem., 2002,2419. S.N. Konchenko, N.A. Pushkarevsky and M. Scheer, J . Organomet. Chem., 2002,658,204. P.I. Anderberg, M.M. Harding, I.J. Luck and P. Turner, Inorg. Chem., 2002,41, 1365. Y. Zhang, J.H. Mao and E . Oldfield, J . Am. Chem. Soc., 2002,124,7829.
I : N M R Spectroscopy in the Liquid and Gas Phase
17
gen-bonding network of substrate-bound human heme oxygenase-1.286 The NH protons in [RU(NH=NH)(P(OE~)~}~]'+at 6 15.36 and 16.76 with 3J(1H'H) are = 32.5 Hz.287A linear correlation has been observed between the 13Cchemical shifts of 4,4'-carbon atoms of bipyridine ligands and oxidation potentials in [R~(bipy)~L]*+.~~~ The 31P coordination shifts of [(R3P)Ru(porphyrinate)(CO)] correlate with pK, values for [HPR3] + . 2 8 9 I5NNMR studies of [Ru(edta)(NO)] support the NO+ character of coordinated NO.290NMR data have also been reported for [{ FB(0N = CRCR = NO)3BF}Fe]2+, (11B),291 cis,trans[R~(bipy)(NO~)~{ NO(OH)}], (15N),292 ruthenium polypyridine complexes, and (99Ru).293
+
2.9 Complexes of Group 9. - The inhibiting influence of aromatic solvents on the activity of asymmetric hydrogenations has been studied by NMR spectroscopy, including lo3Rh NMR NMR data have also been (lo3Rh, [(q5reported for [{HB(3,5-Me2C3HN2)3}RhH(SnPh3)(PR3)], '9Sn),295 C5Me5)Rh( PMe3)( Me)( CNSiPh3)]+ , (29Si),2 [HC{ SiMe2N(2-MeOC6H4)}3Sn96 (Li)Rh(q4-C8H *)Cl], (29Si, 19Sn),2 [( Et3P)3( H)21r= SiH{C6H2-2,6-( C6H2-2,4,6Me3)2}] +, (29Si),298 [{ PhB(CH2PPh2)3}IrH2Si(C8H15)(C6H2-2,4,6-Pr'3)], = (29Si),299 [(q'-C5Me5)(Me3P)Ir(SiPh3)(CO)J (29Si).300 and +, Predictions of "B chemical shifts of [{ HB(3-R'-5-R2-C3HN2)3}Rh(C0)2] have been compared with experimental values.301 There is a correlation between Rh-P distances, 6(31P)and 'J(Io3Rh3lP) for [Rh{q5-C5H5)Fe(q5-C5H4COCHCOR)}(CO)(PPh3)].302 and 31P 'H pulsed gradient spin echo diffusion data and 'H,'9F-HOESY have been applied to complexes such as (27).When the anion is [B{ 3,5-(F3C)2CbH3}4]-, cation and anion diffuse together, but when the anion is [PF& they do not.303 For [(q5-C5Me5)(L)Ir PR], 6(31P) = and 2J(31P31P) are
R.T. Syvitski, Y.M. Li, K. Auclair, P.R.O. de Montellano and G.N. La Mar, J. Am. Chem. Soc.,
2002,124,14 296.
287 288 289 290 291
292
293
294 295
296
297
298
299
300 301
jo2
G. Albertin, S. Antoniutti, A. Bacchi, M. Boato and G. Pelizzi,J. Chem. SOC., Dalton Trans., 2002, 3313. X. Xiao, J. Sakamoto, M. Tanabe, S. Yamazaki, S. Yamabe and T. Matsumura-Inoue, J. Electroanal. Chem., 2002,527,33. E. Stulz, M. Maue, N. Feeder, S.J. Teat, Y.-F. Ng, A.D. Bond, S.L. Darling and J.K.M. Sanders, Inorg. Chem., 2002,41,5255. A. Wanat, T. Schneppensieper, A. Karocki, G. Stochel and R. van Eldik, J. Chem. SOC.,Dalton Trans., 2002,941. Y.Z. Voloshin, V.E. Zavodnik, O.A. Varzatskii, V.K. Belsky,A.V. Palchik, N.G. Strizhakova, 1.1. Vorontsov and M.Y. Antipin, J. Chem. Soc., Dalton Trans., 2002,1193. D.A. Freedman, D.E. Janzen, J.L. Vreeland, H.M. Tully and K.R. Mann, Inorg. Chem., 2002,41, 3820. M.I.J. Polson, J.A. Lotoski, K.O. Johansson, N.J. Taylor, G.S. Hanan, B. Hasenknopf, R. Thouvenot, F. Loiseau, R.Passalaqua and S. Campagna, Eur. J. Inorg. Chem., 2002,2549. D. Heller, H.J. Drexler, A. Spannenberg, B. Heller, J.S. You and W. Baumann, Angew. Chem.,Int. Ed. Engl., 2002,41, 777. V. Circu, M. Fernandes and L. Carlton, Inorg. Chem.,2002,41,3859. F.L. Taw, P.S. White, R.G. Bergman and M. Brookhart, J. Am. Chem. SOC., 2002,124,4192. M. Lutz, C. Galka, M. Haukka, T.A. Pakkanen and L.H. Gade, Eur. J. Inorg. Chem., 2002,1968. R.S. Simons, J.C. Gallucci, C.A. Tessier and W.J. Youngs, J. Organornet. Chem., 2002,654,224. J.D. Feldman, J.C. Peters and T.D. Tilley, Organometallics, 2002,21,4065. S.R. Klei, T.D. Tilley and R.G. Bergman, Organometallics, 2002,21,4648. C.E. Webster and M.B. Hall, Inorg. Chim. Acta, 2002,330,268. J. Conradie, G.J. Lamprecht, S. Otto and J.C. Swarts, Inorg. Chim. Acta, 2002,328, 191.
18
diagnostic for the E and 2 forms.3o4The 7Li NMR spectrum of (28) shows 'J(I9F7Li)= 101 Hz.~" The analysis of the ABMX spin system in the 31P NMR has been ~ ) ] spectrum of [ C O ~ ( C O ) ~ ( ~ - H C = C C H ~ P P ~ ~ C H ~ P P ~proposed as a student experiment.306 NMR data have also been reported for [(q4C4Me4)Co(q6-3,5-Me2C5H3BSnMe3)], ("B, '19Sn),307 [Iflq4-CsH 12)(p-OSiMe3)12, (29Si),308 [(q5-C5Me5)Co(pz3BH)], (11B),309 [($-But2C5H3)Rh(PMe3)(Se4)], (lo3Rh),310 [(q5-C5Me4SiMe2CH2PMe2)MBr], = Rh, Si; 29Si),311 (M [(q5-2-menthyl-4,7-Me2-indenyl)Rh(CO)J, (103Rh),312 and [(q4-cod)Ir(PCy3)(0SiMe3)], (29Si).313
The effect of temperature and pressure on the 59C0NMR chemical shift, the I2C/I3Cisotope shift and 1J(59C013C) [Co(CN),I3- has been reported.314The of I3C chemical shift of the cyanide in (29) is at 6(I3C)= 81.5.j15 The ion-pair of [C~(en)~]'+ d-tartrate gives two 59C0 with NMR signals.316 59C0 NMR spectroscopy has been shown to be useful to the study of selective interactions of Co(II1) complex ions in lyotropic systems.317 The configurations of the four geometric mer-isomers of [Co{ H2NCH2CH2NH( CH2)3NH2} (H2NCH2CMe2NH2)C1I2 +, and of two symmetric isomers of [ C O ( ~ - N H ~ C H ~ C ~ H+~3N9) have been , 1 ~C~~] determined using two-dimensional NMR spectroscopy. The determination of
303 304
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306 307 308 309 310 3 11 312
313 314 315
316 311 318 319
D. Drago, P.S. Pregosin and A. Pfaltz, Chem. Commun., 2002,286. A.T. Termaten, T. Nijbacker, M. Schakel, M. Lutz, A.L. Spek and K. Lammertsma, Organometallics, 2002,21,3196. M.L. Lehaire, R. Scopelliti, H. Piotrowski and K. Severin, Angew. Chem., Int. Ed. Engl., 2002,41, 1419. C. Cordier, R. Thouvenot, H. Amouri and M. Gruselle, J. Chem. Ed., 2002,79,234. G.E. Herberich, T.S.B. Baul and U. Englert, Eur. J. Inorg. Chem., 2002,43. W.X. Liu, P.L. Rinaldi, L. Galya, J.E. Hansen and L. Wilczek, Organometallics, 2002,21,3250. T.J. Brunker, A.R. Cowley and D. OHare, Organometallics, 2002,21,3123. Q. Kong and G. Jin, Chin. Sci. Bull., 2002,47, 187. S.R. Klei, T.D. Tilley and R.G. Bergman, Organometallics, 2002,21,4905. H. Schumann, 0.Stenzel,S. Dechert, F. Girgsdies, J. Blum, D. Gelman and R.L. Halterman, Eur. J . Inorg. Chem., 2002,211. I. Kownacki, M. Kubicki and B. Marciniec, Inorg. Chim. Acta, 2002,334,301. D.G. Gillies, L.H. Sutcliffe and A.J. Williams, Magn. Reson. Chem., 2002,40, 57. T. Yagi, H. Hanai, T. Komorita, T. Suzuki and S. Kaizaki, J . Chem. SOC.,Dalton Trans., 2002, 1126. L.L. Borer, J.G. Russell and R.E. Settlage, J . Chem. Educ., 2002,79,494. M. Iida, Rec. Res. Develop. Phys. Chem., 2000,4,35. X.-m. Yuan, Q.-j.Zhu, Z. Tao and J.-x. Zhang, Huaxue Xuebao, 2002,60,121. J.-x. Zhang, H.-r. Guo, Z. Tao, Q.-j. Zhu and X.-q. Luo, Wuji Huaxue Xuebao, 2002,18,915.
19
enantiomer composition of amino acid esters by using a Co(II1) porphyrin shift reagent has been described.320'H NOESY has been used to demonstrate tetramer formation from two bis-phosphine substituted Zn" porphyrin units and two Rh"' tetraphenylporphyrin units.321The optimal parameters for 31P detected lo3RhHMQC NMR spectroscopy of AMX spin systems have been derived and applied to adducts of [Rh2{02CC(OMe)(CF3)Ph}4] with PPh3 and a chiral p h ~ s p h a n eThe~ ~ . ~ enantiomeric ratios of phosphine selenides have been determined by 'H, 13C, 31Pand 77Se NMR spectroscopy by coordination to [Rh2{02CC(OMe)(CF3)Ph}4].323 NMR data have also been reported for trans[C~(PPh~)(acac)~L]+, (59Co),324[Rh("NH3)5{SC(NMe2)2}]3+, ('5N),325 and [Rh(terpy)(phen)(N3)I2 ( 14N).326 +,
2.10 Complexes of Group 10. - A relevant review has appeared: 'Overall view of the use of chiral platinum(I1) complexes as chiral derivatizing agents for the enantiodiscrimination of unsaturated compounds by IssPt NMR. 3 2 7 The enantiomeric excess determination of a-amino acids by 19F NMR spectroscopy of their N,N-Me2-(CF3CHPh)amine-C,N palladium complexes has been described.328NOESY NMR results have shown how complexed 42{(2R,5R)-2,5-Me2-phospholano}2C6H4 interacts with the aryl ligand in PdBr(C6H4-4-CN).329 enantiomeric excess of a-amino acids has been deterThe mined by 19F NMR spectroscopy using [(p-Cl)~{ C6H4-2MeCPh(CF3)CNMe2}2Pd2].330 relative cation-anion positions in [M(q1,q2The C8H120Me)(pz2XH2)] M = Pd, Pt,33' and [M(q',q2-C8H120Me)(2,6+, R2C6H3N= CMeCMe = NCbH3R2-2,6)]+, = Pd, Pt,332have been determined M
320
321 322
323
324
325
326
327
328
329
330 33 1
M. Claeys-Bruno, M. Bardet and J.-C. Marchon, C.R. Chim., 2002,521. E. Stulz, Y.-F. Ng, S.M. Scott and J.K.M. Sanders, Chem. Commun., 2002,524. D. Magiera, W. Baumann, I.S. Podkorytov, J. Omelanczuk and H, Duddeck, Eur. J. Inorg. Chem., 2002,3253. S . Malik, H. Duddeck, J. Omelanczuk and M.I. Choudhary, Chirality, 2002,14,407. M. Ogita, Y. Yamamoto, T. Suzuki and S. Kaizaki, Eur. J . Inorg. Chem., 2002,886. C.G. Barry, E.C. Turney, C.S. Day, G. Saluta, G.L. Kucera and U. Bierbach, Inorg. Chem., 2002, 41,7 159. W.K. Seok, H.N. Lee, M.Y. Kim, T.M. Klapotke, Y. Dong and H. Yun, J . Organomet. Chem., 2002,654,170. G . Uccello-Barretta, R. Bernardini, F. Balzano and P. Salvadori, Chirality, 2002,14,484. F. Levrat, H. Stoeckli-Evans and N. Engel, Tetrahedron: Asymmetry, 2002,13,2335. D. Drago and P.S. Pregosin, Organometallics,2002,21, 1208. F. Levrat, H. Stoeckli-Evans and N. Engel, Tetrahedron: Asymmetry, 2002,13,2335. B. Binotti, G. Bellachioma, G. Cardaci, A. Macchioni, C. Zuccaccia, E. Foresti and P. Sabatino, Organometallics, 2002,21,346.
20
by I9F,'H HOESY. The 'H NMR spectra of [Pt2Mes(p-A1Me)2]have been analysed as [AXn]2.333Trans-[PtC12(amine)(q2-C2H4)] and [PtC13(q2-C2H4)] [amineH], containing binaphthyl secondary amines, are efficient chiral derivatizing agents for the enantiodiscrimination for chiral alkenes by 195Pt NMR spectroscopy.334 A large 1J(205T1-'95Pt) has been detected for [(NC)4PtTl(phen),(solv)] by 205Tl NMR 31PCOSY has been NMR applied to [T12Pd12(CO)9(PEt3)9]2+.336 data have also been reported for [HPt { P(3-C6H4S03Na)3}3] (195pt),3 cis-[( PHCyl)(H)Pt(p-PCy2)]2, (19spt),3 , ('5N),339 [Pd{ P(CH2CH2PPh2)3}(SnC13)1 CSnC131, [Pd(phen)2Mel+, [Pt{ P(CH2CH2PPh2)3}Cl] (Il9Sn, 195Pt),340[{ PtMe3(9-methyladenine)}3], +, (195pt),341 [{ Ph2PC(NPr')2A1Me2}2PtMe2], (195Pt),342 [PtMe2{1(Me2(30), [(tmeda)Pt(OH)(OMe)Me2], NCH2CH2NCH)CloH7}], ( 195Pt),343 (119Sn),344 (195Pt),345 [PtC13(CH2CH2CH20H)]-, (195Pt),346 [(tmeda)Pt(q3-CH2CHCHq')PtX(tmeda)] +, (195Pt),347Pt { CH(PPh3)[C(0)R1]}C14(NH2R2)], [ (195Pt),348 (31), (195Pt),349[{PhPt(PEt3)2C=CSiPh2C=C}2Pt(PBu"3)2], (29Si),350 (32), (195Pt),3 52 (195Pt),3 [{ Me02CCHRNHCH2-4-C6H2-2,6-(CH2NMe2)}PrBr], [(Me3P)2PtSiPh2C(C02Me)=C C02Me], (29Si),353(33), (195Pt),354 [(q2-2C6H4PPh2)Pt(p-2-C6H4PPh2)Hg] (195Pt, 199Hg),355 +, (34), (29Si),356 [(q4+
332 333
334
335
336
337 338
339
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343 344
34s
346
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3s4
G. Bellachioma, B. Binotti, G. Cardaci, C. Carfagna, A. Macchioni, S . Sabatini and C. Zuccaccia, Inorg. Chim. Acta, 2002,330,44. K. Angermund, M. Buhl, E. Dinjus, U. Endruschat, F. Gassner, H.-G. Haubold, J. Hormes, G. Kohl, F.T. Mauschick, H. Modrow, R. Mortel, R. Mynott, B. Tesche, T. Vad, N. Waldofner and H. Bonnemann, Angew. Chem., Int. Ed. Engl., 2002,41,4041. G. Uccello-Barretta, R. Bernardini, F. Balzano, F. Venturelli, A.M. Caporusso and P. Salvadori, Eur. J . Org. Chem., 2001,3651. G. Ma, A. Fischer and J. Glaser, Eur. J. Inorg. Chem., 2002, 1307. S.A. Ivanov, R.V. Nichiporuk, E.G. Mednikov and L.F. Dahl, J . Chem. SOC., Dalton Trans., 2002, 41 16. D.S. Helfer and J.D. Atwood, Organometallics, 2002,21,250. P. Mastrorilli, C.F. Nobile, F.P. Fanizzi, M. Latronico, C.H. Hu and U. Englert, Eur. J. Inorg. Chem., 2002,1210. B. Milani, A. Marson, E. Zangrando, G. Mestroni, J.M. Ernsting and C.J. Elsevier, Inorg. Chim. Acta, 2002,327, 188. D. Fernandez, M.I. Garcia-Seijo, T. Kegl, G. Petocz, L. Kollar and M.E. Garcia-Fernandez, Inorg. Chem., 2002,41,4435. X. Zhu, E. Rusanov, R. Kluge, H. Schmidt and D. Steinborn, Inorg. Chem., 2002,41,2667. M.P. Coles and P.B. Hitchcock, Chem. Commun., 2002,2794. M. Crespo, M. Font-Bardia, S . Pkrez and X. Solans, J . Organomet. Chem., 2002,642, 171. M.C. Janzen, H.A. Jenkins, M.C. Jennings, L.M. Rendina and R.J. Puddephatt, Organometallics, 2002,21,1257. V.V. Rostovtsev, L.M. Henling, J.A. Labinger and J.E. Bercaw, Inorg. Chem., 2002,41,3608. S . Otto and L.I. Elding, J . Chem. SOC.,Dalton Trans., 2002,2354. G. Bandoli, A. Dolmella, N.G. Di Masi, F.P. Fanizzi, L. Maresca and G. Natile, Organometallics, 2002,21,4595. N.A. Bokach, S.I. Selivanov, V.Y. Kukushkin, J. Vicente, M. Haukka and A.J.L. Pombeiro, Organometallics, 2002,21, 3744. S . Crementieri, P. Leoni, F. Marchetti, L. Marchetti and M. Pasquali, Organometallics, 2002,21, 2575. W.-Y. Wong, C.-K. Wong, G.-L. Lu, K.-W. Cheah, J.-X. Shi and Z.-Y. Lin, J . Chem. SOC., Dalton Trans., 2002, 4587. M. Crespo, J. Granell, X. Solans and M. Font-Bardia, Organometallics, 2002,21, 5140. G. Guillena, G. Rodriguez, M. Albrecht and G. van Koten, Chem.-Eur. J., 2002,8,5368. M. Tanabe and K. Osakada, J. Am. Chem. SOC., 2002,124,4550. V. Jacob, T.J.R. Weakley and M.M. Haley, Angew. Chem., Int. Ed. Engl., 2002,41,3470.
21
cod)Pt(C=CSiMe3)2], (29Si,'95Pt),357 [Pt(C=CPh)(SiMe3)(NMe2CH2CH2PPri2)], (29Si),358 [Pt(C=CPh)2{(Ph2PCH2)2SiMe2}], (29Si,195Pt),359 (29Si),360 (35), [(q2~od)Pt(SiMeCl~)(p-Cl)]~, 195Pt),361 (29Si, [{Ni(PPh3)}2{p-[q2-CH2 CHSiMe(p= NH)14}1, (29si),36 [(Ph3P)2Pt(q2-CH2 C = CF2)], = (195Pt),363 CPt3(pPBut2)3(CO)2(CH2 CH2)]+, = (195Pt),364 (36),(11B).365 and
The interaction of [Pt(NH3)2{(02C)2C4H6}] with glutathione has been investigated by 'H,15NHSQC NMR spectroscopy.366NOE has been used to differentiate between E- and Z-isomers of cis-[PtC&{NH = C M ~ ( O B U " ) ) ~ ] nearly A .~~~ linear relationship has been established for some tris(1-cyclohepta-2,4,6-trieny1)phosphine of Rh' and Pt" between 6(lo3Rh) 8(195Pt).368 full 'H, 13Cand and A 31P NMR analysis has been reported for dipalladium complexes of monoalkyl (a-anilinobenzyl)phosphonates.369 NMR data have also been reported for Nil*
355 356 351 358 359 360
361 362 363 364
365 366 361 368
369
M.A. Bennett, M. Contel, D.C.R. Hockless, L.L. Welling and A.C. Willis, Znorg. Chem., 2002,41, 844. M. Theil, P. Jutzi, B. Neumann, A. Stammler and H.-G. Stammler, J. Organomet. Chem., 2002, 662, 34. M. Herberhold, T. Schmalz, W. Milius and B. Wrackmeyer,J. Organomet. Chem., 2002,641,173. K.R. Flower, V.J. Howard, R.G. Pritchard and J.E. Warren, Organometallics, 2002,21, 1184. M. Benito, 0.Rossell, M. Seco, G. Muller, J.T. Ordinas, M. Font-Bardia and X . Solans, Eur. J. Inorg. Chem., 2002,2477. H. Hashimoto, Y. Sekiguchi, T. Iwamoto, C. Kabuto and M. Kira, Organometallics, 2002, 21, 454. A.K. Roy and R.B. Taylor, J . Am. Chem. Soc., 2002,124,9510. H. Maciejewski, M. Kubicki, B. Marciniec and A. Sydor, Polyhedron, 2002,21, 1261. D. Lentz, N. Nickelt and S. Willemsen, Chem.-Eur. J.,2002,8, 1205. P. Leoni, F. Marchetti, M. Pasquali, L. Marchetti and A. Albinati, Organometallics, 2002, 21, 2176. B.Y. Lee, Y .H. Kim, H.J. Shin and C.H. Lee, Organometallics, 2002,21, 348 1. Q. Liu, J. Lin, J.-y. Zhang, L.-g. Zhu and Z.-j. Guo, Wuji Huaxue Xuebao, 2002,18,37. N.A. Bokach, V.Y. Kukushkin, M.L. Kuznetsov, D.A. Garnovskii, G. Natile and A.J.L. Pombeiro, Znorg. Chem., 2002,41,2041. M. Herberhold, T. Schmalz, W. Milius and B. Wrackmeyer, 2. Naturforsch., B: Chem. Sci., 2002, 57, 255. L. Tusek-Bozic and A. Lycka, Magn. Reson. Chem.,2002,40,175.
22
complexes of famotidine, (15N),3 Pd" complexes of oxybenziporphyrin, 70 (15N),37CPd(S2SiMe2)(PEt3)2], (29Si),3 [M{ P(C7H7)3}2(Se2C2B10H10)], (M = Pd, 72 Pt; 77Se, 195Pt),3 [Si{ CH2CH2CH2SiMe2C=CCH2CMe(CH2PPh2)2PdC12}4], (29Si),374 platinum complexes with bridging 1-Me-cytosinate ligands, (195Pt),3 cis-[ PtC12(NH3)(1,4,7,10,13-pentaoxo16-aza-cyclooctadecane-N)], (195Pt),3 76 trans-[Pt(R1NH2)(R2NH2)C12], (195Pt),377 complexes with phenylalanine, Pt" (195Pt), Pt " complexes of 1-P-D-ribofuranosyl- 1,2,4-triazole-3-carboxamide, (15N,195Pt),379 and Pb" complexes of nitrogen macrocycles, ("'Pt, 207Pb),380 Pt" [Pt2(bipy)2(pL-4,7-dihydro-7-oxo[ triazoloc1,5-a]pyridine)], (195Pt),381 1,2,4] Pt" and Pt'" complexes of 1,2,4-triazolo-[1,5-a]-pyrimidines, (15N),3 Pt" complexes of methylthyminate,(195Pt),383 [PtC15(NH= CEtON = CHC6H4-2-OH)]-, (195Pt),384 trans-[PtC&{NH = C(OH)Et},], (195Pt),3 [M,Hg2{ 2,9-(Ph2P)2-1,lO8s hen}^]^+, (M = Pd, Pt; "'Pt, 199Hg),386 [Pt(S3C7H14)(dppe)12+, (195Pt),387 * [Pt(SPh)2(cis-Ph2PCH = CH PPhl)], (195Pt),388 cis-[ { 2,4,6(Me3Si)3C6H2PMe2} Se2], (77Se, "'Pt), 2Pt [{ (C7H7)3P} M { Se2C2(C02Me)2}], 2 (M = Pd, Pt; 77@87Se, 195Pt),390[P(CH2CH2PPh2)3PtCl]+, (195Pt),391 (195Pt),392 [Pt X4(oxalat o)I2 , [PtC12( oxalato ) ~ ] , (195Pt),39 3 [Pt(SeCN)2( x a l a t o ) ~ ] ~ (77Se, 19sPt),394[PtCl{ MeS(CH2)3Te(CH2)3SMe}], ~ -,
*
370 371 372

373
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375
376
377
378
379 380
381
382
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388 389 390
391
392
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M. Baranska, E. Gumienna-Kontecka, H. Kozlowski and L.M. Proniewicz, J . Inorg. Biochem., 2002,92, 112. M. Stcpien, L. Latos-Grazynski, T.D. Lash and L. Szterenberg, Inorg. Chem., 2002,41,6892. T. Komuro, T. Matsuo, H. Kawaguchi and K. Tatsumi, Chem. Commun., 2002,988. M. Herberhold, T. Schmalz, W. Milius and B. Wrackmeyer, 2. Anorg. Allg. Chem., 2002,628, 979. R.A. Findeis and L.H. Gade, J. Chem. SOC.,Dalton Trans., 2002,3952. G . Kampf, M. Willermann, E. Freisinger and B. Lippert, Znorg. Chim. Acta, 2002,330, 179. B.A.J. Jansen, P. Wielaard, H. den Dulk, J. Brouwer and J. Reedijk, Eur. J. Inorg. Chem., 2002, 2375. S. Shamsuddin, M.S. Ali, S. Huang and A.R. Khokhar, J. Coord. Chem., 2002,55,659. L.F. Krylova, T.A. Pavlushko and A.A. Baluev, Zh. Neorg. Khim., 2001,46,1888. E. Szlyk, I. Lakomska, J. Kobe, A. Surdykowski, T. Glowiak and J. Sitkowski, Polyhedron, 2002, 21,2001. R.V. Singh, S.C. Joshi, S. Kulshrestha, P. Nagpal and A. Bansal, Metal-Based Drugs, 2001,8,149. M.A. Haj, M. Quiros and J.M. Salas, J. Chem. SOC.,Dalton Trans., 2002,4740. E. Szlyk, L. Pazderski, I. Lakomska, A. Surdykowski, T. Glowiak, J. Sitkowski and L. Kozerski, Polyhedron, 2002,21, 343; E. Szlyk, I. Lakomska, A. Surdykowski, T. Glowiak, L. Pazderski, J. Sitkowski and L. Kozerski, Inorg. Chim. Acta, 2002,333,93. M.J. Rauterkus, I. Puscasu and B. Krebs, Inorg. Chim. Acta, 2002,339,438. T.N.A. Bokach, M. Haukka, A.J.L. Pombeiro, S.N. Morozkina and V.Y. Kukushkin, Inorg. Chim. Acta, 2002,336,95. K.V. Luzyanin, M. Haukka, N.A. Bokach, M.L. Kuznetsov, V.Y. Kukushkin and A.J.L. Pombeiro, J . Chem. SOC.,Dalton Trans., 2002, 1882. V.J. Catalano, M.A. Malwitz and B.C. Noll, Inorg. Chem., 2002,41,6553. G.J. Grant, D.F. Galas, I.M. Poullaos, S.M. Carter and D.G. Van Derveer, J. Chem. SOC.,Dalton Trans., 2002,2973. R.H. Vaz, R.M. Silva, J.H. Reibenspies and O.A. Serra, J. Braz. Chem. SOC.,2002,13,82. K. Nagata, N. Takeda and N. Tokitoh, Angew. Chem., Znt. Ed. Engl., 2002,41,136. M. Herberhold, T. Schmalz, W. Milius and B. Wrackmeyer, 2. Naturforsch., B: Chem. Sci.,2002, 57, 53. H. Wachtler, W. Schuh, K.-H. Ongania, H. Kopacka, K. Wurst and P. Peringer, J. Chem. SOC., Dalton Trans., 2002,2532. J.G. Uttecht, C. Nather and W. Preetz, 2.Anorg. Allg. Chem., 2002,628,2329. J.G. Uttecht, C. Nather and W. Preetz, 2. Anorg. Allg. Chem., 2002,628,2585; J.G. Uttecht and W. Preetz, 2. Anorg. Allg. Chem., 2002,628,965.
I : N M R Spectroscopy in the Liquid and G a s Phase
23
(125Te, 195Pt),395 Pt" complexes with bile acids, (19sPt).396 and

2.11 Complexes of Group 11.- 19F,'H-HOESYand PGSE NMR spectroscopy
'H has been applied to (37)and (38).397 NMR spectroscopy has been used to determine the ring conformation of [CuLi2Br{ C6&(CH2NMeCH2CH2NMe)2}2].398 NMR data have also been reported for [Li(THFhNCCu{C(SiMe3)3}]2, 29Si).9 9 (7Li,
CH2Ph
Low-temperature I3C NMR spectroscopy of [Ag(CN)2]- shows 1J('07Ag,13C) and 'J(lWAg,13C). I3C, 14N, 77Seand '25Te NMR spectra were recorded for NMR spec[Me3Te]X, X = [N3]-, [OCNl-, [SCNl-, [SeCN]-.400 The 31P trum of [ A U ~ ( A U C ~ ) ~ ( ~ ~ p-PBu' '=~ { - P B U ) C(NMe2)2}6]4+is of the [AB2C]2 type.401For some phosphine selenide complexes of Au', there is a strong correlation between the 31P chemicals shifts and the C-P-C angle in the p h o ~ p h i n e s . ~ ~ ~ NMR data have also been reported for [AgCN] complexes of thiourea, (15N, 107Ag),403 [(EtzO)Li(N(C6H3-2,6-PrI2) CMe}2CCuI]2, (7Li),404 [(THF)2Cu3= Li21 (NBut)3S} { 2], (7Li),40 [HB{ 3,5-(F3C)2C3HN2}3AgSn(N3)( Pr"2ATI)], (I 9Sn),406Ag { MeC(CH2PPh2)3} [ XI, (1WAg),40 7copper sulfide clusters, (63Cu),40
394 395 396 397
398
399
400
401
402 403 404
405 406 407
J.G. Uttecht and W. Preetz, 2. Anorg. Allg. Chem., 2002,628, 1477. M. Hesford, W. Levason, S.D. Orchard and G. Reid, J. Organomet. Chem., 2002,649,214. J.J. Criado, J.L. Manzano and E. Rodriguez-Fernandez, Rec. Res. Develop. Lipids, 2001,4,63. A. Burini, J.P. Fackler, R. Galassi, A. Macchioni, M.A. Omary, M.A. Rawashdeh-Omary, B.R. Pietroni, S. Sabatini and C. Zuccaccia, J . Am. Chem. SOC.,2002,124,4570. C.M.P. Kronenburg, C.H.M. Amijs, J. Jastrzebski, M. Lutz, A.L. Spek and G. van Koten, Organometallics, 2002,21,4662. C. Eaborn, S.M. El-Hamruni, M.S. Hill, P.B. Hitchcock and J.D. Smith, J. Chem. SOC., Dalton Trans., 2002, 3975. T.M. Klapotke, B. Krumm, P. Mayer, H. Potrowski, 1. Schwab and M. Vogt, Eur. J. Inorg. Chem., 2002,2701. L. Weber, U. Lassahn, H.-G. Stammler, B. Neumann and K. Karaghiosoff, Eur. J . Inorg. Chem., 2002,3272. M.S. Hussain and A.A. Isab, J. Chem. Crystallogr.,2001,30,731. S . Ahmad, A.A. Isab and W. Ashraf, Inorg. Chem. Commun., 2002,5,816. J. Prust, H. Hohmeister, A. Stasch, H.W. Roesky, J. Magull, E. Alexopoulos, I. Uson, H.-G. Schmidt and M. Noltemeyer, Eur. J. Inorg. Chem.,2002,2156. B. Walfort, T. Auth, B. Degel, H. Helten and D. Stalke, Organometallics, 2002,21,2208. H.V.R. Dias and A.E. Ayers, Polyhedron, 2002,21,611. J.A. Montes, S. Rodriguez, D. Fernandez, M.I. Garcia-Seijo, R.O. Gould and M.E. GarciaFernandez, J. Chem. SOC.,Dalton Trans., 2002, 1110.
24
2.12 Complexes of Group 12. - The 13CNMR spectrum of 15Nlabelled (39) is AAX.41 The 199Hg shielding tensors of methylmercury halides have been determined.416The y-cis effect in the 199Hg NMR spectrum of substituted vinylmercury halides has been di~cussed.~'' NMR data have also been reported for [2-NCsH4SiMe2C(SiMe3)2MClIn, = Cd, n = 2; M = Hg, n = 1; 29Si,'l3Cd, (M 199Hg),41 [(MeHg)3(C3N3S3)1, (199Hg),419 [( 1,2'C6F4Hg)3(HCONMe2)2] (199Hg),420 [{ H(Pri3Si)2Si}2Hg], (29Si, and 199Hg).421
9
Detailed one-dimensional and two-dimensional NMR studies have been used to show that the major configuration of Zn1'2-xylyl-bicyclamacetate is cisV l t r a r ~ s - 1The conformation of the zinc-porphyrin in the myoglobin heme .~~~ pocket has been investigated by "N NMR spectroscopy.423'I3Cd NMR isotropic shielding calculations have been performed to analyse the experimentally
408
409 410 4 11 412
413 414
4 15
416 417
418 419 420
42 1
422
42 3
G.W. Luther, tert., S.M. Theberge, T.F. Rozan, D. Rickard, C.C. Rowlands and A. Oldroyd, Environ. Sci. Technol.,2002,36, 394. C.-W. Liu, C.-M. Hung, J.-C. Wang and T.-C. Keng, J. Chem. SOC.,Dalton Trans., 2002,3482. P. Sekar, F.P. Arnold and J.A. Ibers, Inorg. Chem., 2002,41,577. A.A. Isab, S. Ahmad and M. Arab, Polyhedron, 2002,21, 1267. T.S. Cameron, A. Decken, I. Dionne, M. Fang, I. Krossing and J. Passmore, Chem.-Eur.J., 2002, 8,3386. S. Ahmad and A.A. Isab, Inorg. Chem. Commun.,2002,5,355. C.W. Liu, I.J. Shang, C.M. Hung, J.C. Wang and T.C. Keng, J. Chem. SOC., Dalton Trans., 2002, 1974. M. Westerhausen, T. Bollwein, K. Karaghiosoff, S. Schneiderbauer, M. Vogt and H. Noth, Organometallics, 2002,21,906. J. Jokisaari, S. Jarvinen, J. Autschbach and T. Ziegler, J. Phys. Chem. A , 2002,106,9313. F.S.H. Vieco, N.M. Hiramatsu, E. Tedeschi, D.d.B. Rezende and 1.P.d.A. Campos, J. Chem. Res., S., 2002,25. C. Eaborn, M.S. Hill, P.B. Hitchcock and J.D. Smith, J. Chem. SOC.,Dalton Trans.,2002,2467. F. Cecconi, C.A. Ghilardi, S. Midollini and A. Orlandini, J. Organomet. Chem., 2002,645, 101. I.A. Tikhonova, F.M. Dolgushin, K.I. Tugashov, P.V. Petrovskii, G.G. Furin and V.B. Shur, J. Organomet. Chem., 2002,654,123. D. Bravo-Zhivotovskii, M. Yuzefovich, N. Sigal, G. Korogodsky, K. Klinkhammer, B. Tumanskii, A. Shames and Y. Apeloig, Angew. Chem., Znt. Ed. Engl., 2002,41,649. X.Y. Liang, J.A. Parkinson, M. Weishaupl, R.O. Gould, S.J. Paisey, H.-S. Park, T.M. Hunter, 2002,124,9105. C.A. Blindauer, S. Parsons and P.J. Sadler, J. Am. Chem. SOC., Z.X. Liang, J.M. Nocek, K. Huang, R.T. Hayes, I.V. Kurnikov, D.N. Beretan and B.M. Hoffman, J. Am. Chem. SOC.,2002,124,6849.
25
determined chemical shift.424The I5N chemical shift perturbation of an RNA oligomer on the addition of Cd2+has been used to determine the metal binding '13Cd NMR spectroscopy has been used to study the Cd2+binding sites on algae and higher plant tissues.426 The oxidative dimerisation of metallothionein has been studied by 'H, "'Cd and '13CdNMR spectroscopy.427Il3Cd NMR spectroscopy has been used to establish the location of Co" in apometal10thionein.~~' 31Pand 199Hg The NMR spectra of [Hg3(dppm)3]4+ have been analysed and 'J('99Hg'99Hg) determined.429NMR data have also been reported for [{ Me2Si(p-NBut)2P s ( N P h ) - ~ - N - ~ - s } ~ z n ] , = (29Si),430 complexes of 2Cd" pyridineformamide N(4)-methylthiosemicarbazone, (113Cd),43 [Cd(cyclam)12+, [{ C ~ H ~ N } CCd" ~ (I5N, 11'Cd),432 ~ - B U ' C H ~ N - ~ - ( M ~ S C H ~ C H ~ ) ~ N+,(113Cd),433 ] complexes of peptides, (113Cd),434 mono-thiocyanate complexes of Cd" containing bulky nitrogen based polydentate ligands, (' 13Cd),43 Cd" complexes of dehydroacetic acid, (113Cd),436 complexes of aspartate, ("'Cd, 113Cd),437 Cd" Cd" and Hg" complexes of 2-pyridineformamide 3-piperidyl-thiosemicarbazone, (' 13Cd, 199Hg),438 and Cd" and Hg" complexes of 2-formylpyrrole, (I13Cd, 199Hg)-439
3
Dynamic Systems
This section is in three main parts: (i) 'Fluxional Molecules', dealing with rate processes involving no molecular change, (ii) 'Equilibria', dealing with the use of NMR spectroscopy to measure the position of equilibria and ligand-exchange reactions, including solvation, and (iii)'Course of Reactions', dealing with the use of NMR spectroscopy to monitor the course of reactions. Each section is ordered by the Periodic Table. Four relevant reviews have appeared: 'Nuclear magnetic resonance studies of
424
425
426
427 428
429
430
431
432
433
434
435
436
437
438
439
M. Krauss, L. Olsen, J. Antony and L. Hemmingsen, J. Phys. Chem., B, 2002,106,9446. Y. Tanaka, C. Kojima, E.H. Morita, Y. Kasai, K. Yamasaki, A. Ono, M. Kainosho and K. Taira, J . Am. Chem. Soc., 2002,124,4595. H. Xia and G.D. Rayson, Adv. Enuiron. Res., 2002,7,157. K. Zangger, G. Shen, G. Oz, J.D. Otvos and I.M. Armitage, Biochem. J., 2001,359,353. J. Ejnik, J. Robinson, J.Y. Zhu, H. Forsterling, C.F. Shaw and D.H. Petering, J. Znorg. Biochem., 2002,88,144. W. Schuh, G. Hagele, R. Olschner, A. Lindner, P. Dvortsak, H. Kopacka, K. Wurst and P. Peringer, J. Chem. Soc., Dalton Trans., 2002,19. D.C. Haagenson, D.F. Moser, L. Stahl and R.J. Staples, Znorg. Chem., 2002,41,1245. I. Garcia, E. Bermejo, A.K. El Sawaf, A. Castineiras and D.X. West, Polyhedron, 2002,21,729. X.Y. Liang, J.A. Parkinson, S. Parsons, M. Weishaupl and P.J. Sadler, Znorg. Chem., 2002,41, 4539. R.A. Allred, L.H. McAlexander, A.M. Arif and L.M. Berreau, Znorg. Chem., 2002,41,6790. M. Matzapetakis, B.T. Farrer, T.C. Weng, L. Hemmingsen, J.E. Penner-Hahn and V.L. Pecoraro, J . Am. Chem. Soc., 2002,124,8042. D.L. Reger, T.D. Wright, M.D. Smith, A.L. Rheingold, S. Kassel, T. Concolino and B. Rhagitan, Polyhedron, 2002,21,1795. M.Z. Chalaca, J.D. Figueroa-Villar, J.A. Ellena and E.E. Castellano, Znorg. Chim. Acta, 2002, 328,45. L. Gasque, S. Bernes, R. Ferrari and G. Mendoza-Diaz, Polyhedron, 2002,21,935. A. Castineiras, I. Garcia and E. Bermejo, 2. Anorg. Allg. Chem.,2002,628,492. R. Carballo, A. Castineiras and T. Perez, Z. Naturforsch., B: Chem. Sci., 2001,56,881.
26
metal interactions with humic s~bstances,4~~ dynamics of aluminiumSlow citrate complexes studied by H and I3C NMR Mechanistic aspects of inorganic chemistry probed via the parahydrogen phenomenon,442 and NMR chromatography. DOSY, which contains its use to study the reaction between [(q5-C5H5)2ZrH(C1)] H2C0.443 and
3.1 Fluxional Molecules. - 3.1.1 Lithium. The variable temperature 31P NMR show exchange and 7Li coupspectra of [Li(CHMePPh2=NC02Me)]2(THF)2 ling at - 110 0C.444The lithium salts of chiral bicyclic allylic a-sulfonyl carbanions show fluxionality and activation energies have been determined.445 NMR self-diffusion measurements have been used to study the aggregation of lithium salts of 2,5,8,1 l-But4-cycloocta[1,2,3,4,def,5,6,7,8-deflbisbiphenylene. The barrier to racemisation has been determined as AGf200= 9.5 f 0.2 kcal mol- in the dimer compared to > 15 kcal mol- in the tetramer.446 6Li1H HOESY has been applied to (40). 6Li6LiEXSY shows Li exchange between the two different sites with AGI = 12.8 f 0.1 kcal m 0 1 - l . ~ ~ ~
Me
(40) 3.1.2 Sodium. Analysis of the H EXSY NMR spectrum of the Na+ complex of
5,11,17,23-But4-25,26,27,28-(Et2NCO)~methoxycalix[4]arene interconvershows sion of the methylene protons from the N(CH2CH3)2moiety. 23NaNMR data were also reported.448
3.1.3 Magnesium. The variable temperature H NMR spectra of [{ CH(CMeNC6H3-2,6-Pri2)2} Mg(OBu)(THF)] show Pr exchange due to re-
stricted rotation of the Aryl-Pr bond.449 Line shape analysis of variable temperature NMR experiments suggest dynamic behaviour of [Mg(3,5-But2-pyrazolato)~(3,5-But2-pyrazolate)2].450 Synchronised four Bailar twists and six atro440
441
442
443
444
44s
446
447
448
449
W.L. Klingery, A.J. Simpson, F. Han and B. Xing, Humic Substances and Chemical Contaminants, Proceedings o a Workshop and Symposium, Anaheim, C A , United States, Oct. 26-27,1997,2001, f 397. A. Bodor, I. Banyai, L. Zekany and I. Toth, Coord. Chem. Rev., 2002,228,163. S.B. Duckett, Rec. Adv. Hydride Chem., 2001,329. G, Schilling, GIT Labor-Fachzeitschri, 2002,46,1163. I. Fernandez, J.M.A. Gutitrrez, N. Kocher, D. Leusser, D. Stalke, J. Gonzalez and F.L. Ortiz, J. Am. Chem. SOC.,2002,124,15 184. H.-J. Gais, M. Van Gumpel, M. Schleusner, G. Raabe, J. Runsink and C. Vermeeren, Eur. J . Org. Chem., 2001,4275. R. Shenhar, H. Wang, R.E. Hoffman, L. Frish, L. Avram, I. Willner, A. Rajca and M. Rabinovitz, J. Am. Chem. Soc., 2002,124,4685. R. Sott, J. Granander and G. Hilmersson, Chem.-Eur. J., 2002,8,2081. A. Moser, G.P.A. Yap and C. Detellier, J. Chem. SOC., Dalton Trans., 2002,428. M.H. Chisholm, J. Gallucci and K. Phomphrai, Inorg. Chem., 2002,41,2785.
27
=
penantiomerisation processes have been monitored for [MhL6l4-, L
(41).451
3.1.4 Calcium. The dynamic processes in [(q5-CsH4CHButCHBu'C5H4q5)Ca(MeOCH2CH20Me)J have been in~estigated.~~' I5N NMR mobility A study on the dicalcium P43M calbindin D9k and its mono La3+substituted form has been reported.453 3.1.5 Barium. A variable temperature I3C{'H} NMR study of [Ba{ 1,4,7,10,13(HOCHZCH2)s-1,4,7,10,13-pentaaza~yclopentadecane}]~ shows racemisation with AH: = 45.4 2.2 kJ mol-I and AS: = 4.5 f 8.5 J K-' m 0 1 - I . ~ ~ ~
+
3.1 -6 Group 3. [(q5-C5Me5)2Y(q3-C3H4-2-Me)] shows two (q5-CsMe5) signals at low temperature and one at high and AGS = 12.8(2) kcal. m 0 1 - I . ~[Y{qs~~ C5H4CH(CH2CH2)2NMe}3] fluxional with coordinated and uncoordinated is nitrogens exchanging.456Variable temperature 'H and I3C NMR spectroscopy shows that [InL'] and [InL2] are fluxional at room temperature while [YL'] and [YL2] only become fluxional at elevated temperatures, L' = 1,4,7,10-N4-4,7,10(H02CCH2)3--cyclododecylacetylbenzylamine and L2 = 1,4,7,10-N4-4,7,101 (H02CCH2)31-cyclododecylacetyl-R-( + )-a-methylben~ylamine.~~ 3.1.7 Lanthanum and the Lanthanides. The 31P NMR spectrum of [La{N(PPh2)2}3J shows two signals at 173K and one at room temperature.458 Ar shows 'J(I3C'H) = 102 Hz. The I3C NMR spectrum of (a), = 2,6-Pr12C6H3, There is a fluxional process which exchanges methyl groups in [(ArO)Ln{(pArO)(p-R)A1R2}l2, = La, Sm.459 Ln 3.1.8 Titanium. Bridge-terminal OCH exchange has been observed in [(qIfluorenyl)Ti( - O P I ? ) ( O P ~ ' The]activation parameters for rac-meso isomer~ )~ ~.~~~
450 45 1
452
453 454
455 456
451 458 459
N.C. Mosch-Zanetti, M. Ferbinteanu and J. Magull, Eur. J. Znorg. Chem., 2002,950. R.W. Saalfrank, B. Demleitner, H. Glaser, H. Maid, D. Bathelt, F. Hampel, W. Bauer and M. Teichert, Chem.-Eur. J.,2002,8,2679. P.-J. Sinnema, B. Hohn, R.L. Hubbard, P.J. Shapiro, B. Twamley, A. Blumenfeld and A. Vij, Organometallics, 2002,21, 182. I. Bertini, C.J. Carrano, C. Luchinat, M. Piccioli and L. Poggi, Biochemistry, 2002,41,5104. K.M. Walters, M.A. Buntine, S.F. Lincoln and K. Wainwright, J. Chem. Soc., Dalton Trans., 2002,3571. C.P. Casey, J.A. Tunge and M.A. Fagan, J. Organomet. Chem., 2002,663,91. M.M. Corradi, M.A.D. McGowan, P.C. McGowan and M. Thornton-Pett, Eur. J. Znorg. Chem., 2002,2362. S . Liu, J. Pietryka, C.E. Ellars and D.S. Edwards, Bioconjugate Chemistry, 2002,13,902. P.W. Roesky, M.T. Gamer, M.Puchner and A. Greiner, Chem.-Eur. J., 2002,8,5265. G.R. Giesbrecht, J.C. Gordon, J.T. Brady, D.L. Clark, D.W. Keogh, R. Michalczyk, B.L. Scott and J.G. Watkin, Eur. J. Inorg. Chem., 2002,723.
28
Ar (42)
Ar
ism of [(q5-3,4-Me2-2-Ph-phospholyl)2TiC12] been determined.46 Dynamic have 'H NMR spectroscopy and spin saturation transfer experiments show a rotation of the fulvene ligand in [(q5-C5R5)Ti{q6-C5H4C(C6H4-4-Me)2}C1] = with hG'314 = 60.6 & 0.5 kJ mo1-'.462 Pr'exchange has been observed in [Ti(3,5-PrI2-1,2,4t r i a ~ o l e ) ~Ligand ~ ] . ~ ~ rotation and racemisation have been observed in (43).464 [(4-MeC6H4S02NPr')2Ti(NMe2)2] two Pr' methyl signals at -20 "C which shows exchange on warming.465The dynamic NMR spectrum of (44) shows 6-membered ring inversion.466 Exchange in [Ti2{p2-(OCH2CH2)2NMe}(p2OPri)(OPr')5]has been investigated.467
Me,"
(43)
0 TiOC6H,-2,6-Pr',
(44)
3.1.9 Zirconium. The variable temperature 'H NMR spectra of [Zr{ 2-(2,4,6Me3C6H2NCH2)2CHC5H4N} show exchange of the inequivalent ZrMe Me2] The 'H NMR spectrum of (45) shows inequivalent Pr' and CH = CH 'H NMR spectroscopy has been used to study the fluxionality of (46), R = SiMe2Ph.470 The fluxionality of [Zr(CH2Ph)2{ 2,2'-(Me3SiN)2-biphenyl}] has been studied using variable temperature NMR ~ p e c t r o s c o p y . ~ ~ ' rotaSlow tion about the But-Zr bond of (47) has been observed.472Restricted rotation
460
46 1 462
463 464 465
466 46 7 468 469
470 47 1 472
S.Y. Knjazhanski, G. Cadenas, M. Garcia, C.M. Perez, I.E. Nifant'ev, I.A. Kashulin, P.V. Ivchenko and K.A. Lyssenko, Organometallics,2002,21,3094. T.K. Hollis, Y.J. Ahn and F.S. Tham, Chem. Commun., 2002,2996. J. Stroot, A. Lutzen, M. Friedemann, W. Saak and R. Beckhaus, 2.Anorg. Allg. Chem., 2002,628, 797. N.C. Mosch-Zanetti, M. Hewitt, T.R. Schneider and J. Magull, Eur. J. Inorg. Chem., 2002,1181. S.M. Mullins, A.P. Duncan, R.G. Bergman and J. Arnold, Inorg. Chem., 2002,40,6952. S. Hamura, T. Oda, Y. Shimizu, K. Matsubara and H. Nagashima, J. Chem. SOC.,Dalton Trans., 2002,1521. Y. Kim and J.G. Verkade, Organometallics, 2002,21,2395. T. Kemmitt, N.I. Al-Salim and G.J. Gainsford, Aust. J. Chem., 2002,55, 513. P. Mehrkhodavandi, R.R. Schrock and P.J. Bonitatebus, Organometallics, 2002,21,5785. M. Niehues, G. Erker, G. Kehr, P. Schwab, R. Frohlich, 0. Blacque and H. Berke, Organometallics, 2002,21,2905. R.M. Gauvin, C. Mazet and J. Kress, J. Organomet. Chem., 2002,658,l. R.M. Gauvin and J. Kress, J. Mol. Catal. A: Chem., 2002,182-183,411. R.J. Keaton, L.A. Koterwas, J.C. Fettinger and L.R. Sita, J. Am. Chem. SOC.,2002,124, 5932.
29
about the Zr-O-Ar bond has been observed in [(q5-C5H5)(q2The carboxylates of (48) alternate between q1 Bu'N = CCH2Ph)2Zr(OAr)].473 and q2bonding with AG: = 37 1 kJ r n 0 1 - l . ~ ~ ~ Dynamic 'H NMR spectroscopy shows cyclopentadienyl fluxionality in (49)with AGT = 5.1 kcal mo1-1.475
-N'
(45)
CH2Ph
(46)
(47)
3.1.10 Vanadium. The NH2 protons of (50) show two signals at 233 K and one broad signal at 303 K.476
Br
(50)
3.1.1 1 Niobium. The variable temperature 'H NMR spectroscopy of (51) shows But exchange.47 The fluxionality of [(q5-C6H6Me)Nb{ N[(SiMe2CH2)2PH]2}] NMR spectroscopy.478AGI for alkyne rotation in has been investigated by 31P [(q5-C5H4SiMe3)(q2-Me3SiC=CSiMe3)Nb(CH2SiMe3)2] 12.6 kcal has AG' = rn01-l.~~~ 'H NMR spectroscopy has been used to investigate restricted rotation around the (q5-Bu'C5H4)-Nb bond in [(q5-B~tCsH4)6Nb4Te40=2Cr(CO)5].480
J.l
7.12 Tantalum. Variable temperature 'H NMR spectroscopy has been used to
M.G. Thorn, J. Lee, P.E. Fanwick and I.P. Rothwell, J. Chem. Soc., Dalton Trans., 2002,3398. B. Wenzel, P. Lonnecke and E. Hey-Hawkins, Organometallics, 2002,21,2070. D. Huerlander, N. Kleigrewe, G . Kehr, G. Erker and R. Frohlich, Eur. J. Znorg. Chem., 2002, 2633. C. Kimblin, X.H. Bu and A. Butler, Znorg. Chem., 2002,41,161. M. Brandl, H. Brunner, J. Wachter and M. Zabel, Organometallics, 2002,21,3069. M.D. Fryzuk, C.M. Kozak, M.R. Bowdridge and B.O. Patrick, Organornetallics, 2002,21,5047. A. Galindo, M. Gomez, P. Gomez-Sal, A. Martin, D. del Rio and F. Sanchez, Organornetallics, 2002,21, 293. H. Brunner, H. Cattey, D. Evrard, M.M. Kubicki, Y. Mugnier, E. Vigier, J. Wachter, R. Wanninger and M. Zabel, Eur. J . Znorg. Chem., 2002,1315.
473 474 475
476 47 7 478 479
480
30
investigate the nature of the fluxionality of [Ta(NMe2h{S02(NB~t)2}].48
(51)
3.1 .13 Chromium, Molybdenum, and Tungsten. The fluxionality of [(OC)5M(pH)BH(PMe3)BH2PMe3], = Cr, W, has been studied using "B NMR spectroM copy.^^^ The variable temperature 'H NMR spectrum of [(OC),W = CPhN = C(CH = CHPh)NMe(CH2Ph)] shows the NCH2 as two AB signals at -55 "C and one AB signal at 10 0C.483Role exchange between the indenyl groups has been observed for [(q'-C9H7)(q3-C9H7)M(NR2)2], = Mo, M w.484 The barrier to alkyne rotation in [Tp'(OC)IW(R'C=CCH2R2)]has been determined.485The variable-temperature 'H NMR spectra of paramagnetic [(q3-2MeC3H4)3Cr]show dynamic behaviour with AG:300 = 49 f 6 kJ m ~ l - ' . ~ ~ ~ Variable temperature 31P{ NMR investigations have revealed the trigonal 'H} twist fluxional process in [(q3-C,H,)MX(C0)2{Ph2P(CH2),PPh2}], m = 7 , n = 7; rn = 6, n = 9; m = 8, n = 13; M = Mo, W.487The fluxionality in Scheme 1 has been investigated by 31P NMR spectroscopy.488
Scheme 1
'H EXSY has been used to study the fluxionality of [W2(p-q5,q5-CsHs)(OR)4].489 The 31P NMR spectrum of [(q5-C5H5)Mo{ P(OMe)3}2(q4-1,3signals for the P2C2 ligand at - 60 "C and one at room P2C2But2)]+ shows two 31P
48 1
482
483
484
48 5
486
487
488
489
R.C. Mills, P. Doufou, K.A. Abboud and J.M. Boncella, Polyhedron, 2002,21, 1051. M. Shimoi, K. Katoh, Y.B. Kawano, G. Kodama and H. Ogino, J. Organomet. Chem., 2002,659, 102. R. Aumann, D. Vogt and R. Frohlich, Organometallics, 2002,21, 1819. U. Radius, J. Sundermeyer, K. Peters and H.G. von Schnering, Z . Anorg. Allg. Chem., 2002,628, 1226. M.B. Wells, J.E. McConothy, P.S. White and J.L. Templeton, OrganometaIlics, 2002,21, 5007. R. Blom and 0. Swang, Eur. J. Inorg. Chem., 2002,411. J . Friend, S.Y. Master, I. Preece, D.M. Spencer, K.J. Taylor, A. To, J. Waters and M.W. Whiteley, J . Organomet. Chem., 2002,645,218. M. Tamm, T. Bannenberg, B. Dressel, R. Frohlich and C. Holst, Znorg. Chem., 2002,41,47. B.E. Bursten, M.H. Chisholm, M.L. Drummond, J.C. Gallucci and C.B. Hollandsworth, J . Chem. SOC.,Dalton Trans., 2002,4077.
31
temperature. AGI = 48.0 kJ m ~ l - ' . ~Cyclopentadienylexchange occurs in (52) ~O with AG' = 71 f 1 kJ mol-'.491 NMR spectroscopy has been used to show the hopping of Cr(C0)3between arene rings in (53).492EXSY has been used to demonstrate the restricted rotation about the arene-carbene bond in [{(q5C5H5)(0C)2Fe CHC6H4-2-OMe-q6}Cr(C0)3].493 to rotation of the = The barrier SnMe3group in (54) has been determined.494
(52)
(53)
(W
The temperature dependent 'H NMR spectra of [WOS3Cu3(pyrazole)3Cl] have been reported.495 fluxionality of [ReH3{(Ph2PCH2CH2)3N}] and [ReH4{(Ph2PCH2CH2)3N}] has been investigated by variable temperature NMR spectroscopy.496 Variable temperature 'H and I3CNMR spectra as well as TI measurements have shown that [Re2H2(C0)9] a classical hydride. The two is carbonyls trans to hydrides exchange with E, = 44 & 1 kJ mol-I. Another much faster process equilises bridging and terminal hydrides at 172 K.497The variable show temperature 'H NMR spectra of [MeRe(NC6H3Pri2-2,6)2(SCH2CH2S)] exchange of the CH2 protons with AG: = 64 kJ m 0 1 - I . ~ ~ ~ Multisite magnetisation transfer studies of metal migration in [(q3-C7H7)Re(CO)4], [(q3C7H7)os(Co)3(snPh3)], [(r13-C7H7)Re(C0)3(PMe3)], [(q5-C7H7)Re(CO)3], [(q5C7H7)Fe(C0)2( SnPh3) 1, [(q5-C7H7)0s(C0)2(SnPh3)1 and Ch5C7H7)Ru(CO)2(SnPh3)] been have The 'tic-toc' mechanism has been observed for [Re(C0)3{ 3,5-Me2pz)(CH2)2S(CH2)2( K~-( 3,5-Me2pz)}(MeOH)] .5 0 0
+
3.1 .I 4 Rhenium. The
490
491
492
493
494
495
496
497
498
499
500
A.D. Burrows, N. Carr, M. Green, J.M. Lynam, M.F. Mahon, M. Murray, B. Kiran, M.T. Nguyen and C. Jones, Organometallics, 2002,21,3076. P. Schollhammer, B. Didier, N. Le Grand, F.Y. Petillon, J. Talarmin, K.W. Muir and S.J. Teat, Eur. J . Znorg. Chem., 2002,658. Y. Oprunenko, I. Gloriozov, K. Lyssenko, S. Malyugina, D. Mityuk, V. Mstislavsky, H. Gunther, G. von Firks and M. Ebener, J. Organomet. Chem., 2002,656,27. Q.W. Wang, F.H. Forsterling and M.M. Hossain, Organometallics, 2002,21,2596. A.E. Aliev, J.E. Anderson, D. Butler, J. Gonzalez-Outeirio, L. Lunazzi, A. Mazzanti, J.W. Steed and R. Wilhelm, Eur. J. Znorg. Chem.,2002,133. A. Beheshti, W. Clegg, R. Hyvadi and H.F. Hekmat, Polyhedron, 2002,21,1547. A. Albinati, V.I. Bakhmutov, N.V. Belkova, C. Bianchini,I. de 10s Rios, L. Epstein, E.I. Gutsul, L. Marvelli, M. Peruzzini, R. Rossi, E. Shubina, E.V. Vorontsov and F. Zanobini, Eur. J. Inorg. Chem., 2002,1530. M. Bergamo, T. Beringhelli, G. DAlfonso, P. Mercandelli and A. Sironi, J . Am. Chem. SOC.,2002, 124,5117. W.-D. Wang, A. Ellern, I.A. Guzei and J.H. Espenson, Organometallics, 2002,21,5576. D.R. Muhandiram, G.Y. Kiel, G.H.M. Aarts, I.M. Saez,J.G.A. Reuvers, D.M. Heinekey, W.A.G. Graham, J. Takats and R.E.D. McClung, Organometallics, 2002,21,2687. S. Alves, A. Paulo, J.D.G. Correia, A.Domingos and I. Santos, J. Chem. SOC., Dalton Trans., 2002, 4714.
32
Variable temperature 'H NMR spectra of [1,4C6H4{ CH20CH2Cpz3Re(C0)3Br}2] show dynamics with two sets of pyrazolyl signals at low temperature and one at room t e m p e r a t ~ r e . ~ ' ~ phosphorus The ligands exchange roles in (55)resulting in the 31P NMR spectrum being AB at low temperature and A2 at higher t e m p e r a t ~ r e . ~ ' ~
Ph
(55)
3.1 .I 5 Iron and Ruthenium. Carbonyl exchange in [(p-pdt){Fe(C0)2(PMe3)}2]

+ The and [(p-H)(p-pdt){Fe(C0)2(PMe3)}2] has been in~estigated.~'~ variable temperature 'H NMR spectra of [R~H(H2Bpin)(HBpin)(PCy~)~l and [ R u H ( H ~ B ~ ~ ~ ) ( H ~ have C ~ ~ ) ~ ] ) ( P been studied as a function of t e m p e r a t ~ r e . ~ ' ~ NMR studies of intramolecular isomerisation and fluxionality of [RU(CO)~H~L~], including the detection of minor isomers by parahydrogeninduced polarisation, have been reported.505 The 'H NMR spectrum of [RUH~(~~-HS~M~~)~(CH~)~(PC~~)~] two inequivalent shows exchange between The q2-HSiMe2groups with AG: = 68.4 kJ m ~ l - ' . ~ ' ~ 'H NMR spectra of (56) show two (q5-C5Me5) signals at 20 "C and one at 80 "C and AH$ and AS' were dete~rnined.~'~ The variable temperature 'H NMR spectra of [{(q5C5Me5)Ru}3(p-H)z(p3-q2-HC = CH)(p3-CMe) show hydride, cyclopentadienyl J and alkyne exchange.508
(56)
The fluxionality of (57) has been in~estigated.~" The NMe2 group in (58) shows restricted rotation of the C(sp3)-Nbond with AG: = 9.95 kcal m ~ l - ' . ~ ~ '
501 502
503
504
505
506
507
508 509
D.L. Reger, K.J. Brown and M.D. Smith, J. Urganomet. Chem., 2002,658,50. X. Couillens, M. Gressier, M. Dartiguenave, S. Fortin and A.L. Beauchamp, J. Chem. Soc., Dalton Trans., 2002,3032. X. Zhao, I.P. Georgakaki, M.L. Miller, R. Mejia-Rodriguez, C.Y. Chiang and M.Y. Darensbourg, Inorg. Chem., 2002,41,3917. V. Montiel-Palma, M. Lumbierres, B. Donnadieu, S. Sabo-Etienne and B. Chaudret, J. Am. Chem. SOC.,2002,124,5624. D. Schott, C.J. Sleigh, J.P. Lowe, S.B. Duckett, R.J. Mawby and M.G. Partridge, Inorg. Chem., 2002,41,2960. I. Atheaux, F. Delpech, B. Donnadieu, S. Sabo-Etienne, B. Chaudret, K. Hussein, J.C. Barthelat, T. Braun, S.B. Duckett and R.N. Perutz, Organometallics, 2002,21,5347. Y. Ohki and H. Suzuki, Angew. Chem., Int. Ed. Engl., 2002,41,2994. T. Takao. T. Takemori, M.Moriya and H. Suzuki, Organometallics, 2002,21,5190. T.A. Jenny, V. Huber, L.Q. Ma, J. Raemy, D. Zeller and H. Stoeckli-Evans, Organometallics, 2002,21,2504.
33
The variable temperature 'H NMR spectrum of (59) shows restricted rotation about the C-N bond. The I3CNMR spectra of (60)show M e 0 exchange. AGf = 44.1 kJ m 0 1 - l . ~ ' The variable temperature 'H NMR spectra of (61) show ~ restricted rotation of a phenyl group."
''
-iT
F6 Me2N-0 NMe,
Fe(C0)2PPh3
The 'H NMR spectrum of the C6H4of (62) goes from ABXY to [AX12 on warming. Independent CO migration and twisting of the CH2CH2group was also observed.' l4 The I3CNMR spectra of (63)show CO and CNR exchange.' Berry pseudorotation in [(q5-C5H5)(OC)2M{ P(OC7H60)2}],M = Fe, Ru, has been investigated and the activation parameters determined.' l6 AGj for the hindered rotations in [(r15-C5H5)Fe(q6-C6H5)NHN = CMe(q5-C5H4)Fe(q5-C5H5)] has been determir~ed.''~ shows two cyclopentadienyl 'H NMR signals at (64) room temperature and four at - 90 OC.' * Similarly, [Ru{(q5-C5H4)C(0)(q5C5H4)}2R~] shows two cyclopentadienyl 'H NMR signals at 333 K and four at 223 K.'19 The dynamic NMR spectra of (q6-C6Et6) complexes of Ruo and Ru"
5 10
511
512
513
514
515 516 517
518
A.C. Filippou and T. Rosenauer, Angew. Chem.,Int. Ed. Engl., 2002,41,2393. R.D.A. Hudson, A.R. Manning, J.F. Gallagher, M.H. Garcia, N. Lopes, I. Asselberghs, R. Van Boxel, A. Persoons and A.J. Lough, J. Organornet. Chem., 2002,655,70. K.G. de Cadenet, R. Rumin, F.Y. Pktillon, D.S. Yufit and K.W. Muir, Eur. J . Inorg. Chem., 2002, 639. M.V. Ovchinnikov, D.P. Klein, I.A. Guzei, M.G. Choi and R.J. Angelici, Organometallics, 2002, 21,617. G. Sanchez-Cabrera, F.J. Zuno-Cruz, M.J. Rosales-Hoz and V.I. Bakhmutov, J. Organomet. Chem., 2002,660, 153. K. Matsubara, S. Mima, T. Oda and H. Nagashima, J . Organomet. Chem., 2002,650,96. H.Nakazawa, K. Kawamura, T. Ogawa and K. Miyoshi, J. Organornet. Chem., 2002,646,204. C. Manzur, M. Fuentealba, L. Millan, F. Gajardo, D. Carrillo, J.A. Mata, S. Sinbandhit, P. Hamon, J.-R. Hamon, S. Kahlal and J.-Y. Saillard, New J. Chem., 2002,26,213. M. Enders, G. Kohl and H. Pritzkow, Organometallics, 2002,21, 1 1 11.
34
have been reported.520EXSY has been used to look at restricted rotation of the pyridine in a trans,cis,~is-[RuCl~(CO)~{ 5, 10-(4-C5H4N)2Zn[ 15,20-Ph2-por= = phyrinate]}2].521Carbonyl fluxionality in [Fe(C0)2(PR13)(R2N CR2CR3 O)] has been in~estigated.~ 22
A
Fe-Cu
Iu(CO),
The variable temperature 'H NMR spectra of [ H B P Z ~ R U ( N H P ~ ) ( P M ~ ~ ) ~ ] show restricted rotation about the Ru-NHPh bond.523 The 'H variable temperature NMR spectra of [(bipy)2Ru(NC5H4-4-Me)2]2+ restricted rotation of show the p i ~ o l i n eEXSY shows sulfur inversion in (65).525 variable tempera.~~~ The ture 31P NMR spectrum of [(Ph2PNMeCHRCHRNMePPh2)Ru(02CMe)2] shows exchange between isomers.526 Ligand migration within the tetracarboxylate di-iron core of [Fez{ ~~-02CCsH3-2,6-(CsH4-4-F)2)2( 02CC&-2,6(C6H4-4-F)2}2(THF)2] been probed by solution variable temperature 19F has NMR spectroscopy.527
3.1 .I 6 Osmium. Variable temperature 'H NMR spectra of [OSH{K-N,K-O(ON = CMe2)}(= C = CHBU')(PP~'~)~] two hydride signals at 203 K and show one at 293 K due to restricted rotation of the 0 s = C = CHBu' 3.1.17 Cobalt. The fluxional behaviour of the dppm ligands in [(p-
dpprn)C0~(C0)~(pPh~PC=CPPh~)] and
'I9
520
[(p-dppm)C~~(CO)~(p-Ph~PC=
521
522
523
524
525 526
527
s28
M. Sato, M. Suzuki, M. Okoshi, M. Kurasina and M. Watanabe, J. Organomet. Chem., 2002,648, 72. R. Baldwin, M.A. Bennett, D.C.R. Hockness, P. Pertici, A. Verrazzani, G.U. Barretta, F. Marchetti and P. Salvadori, J. Chem. Soc., Dalton Trans., 2002,4488. E. Iengo, E. Zangrando, S. Geremia, R. Graff, B. Kieffer and E. Alessio, Chem.-Eur. J., 2002,8, 4670. R. Siebenlist, H.-W. Fruhauf, K. Vrieze, W.J.J. Smeets and A.L. Spek, Organometallics, 2002,21, 5628. D. Conner, K.N. Jayaprakash, T.B. Gunnoe and P.D. Boyle, Znorg. Chem., 2002,41,3042. A.H. Velders, C. Massera, F. Ugozzoli, M. Biagini-Cingi, A.M. Manotti-Lanfredi, J.G. Haasnoot and J. Reedijk, Eur. J. Znorg. Chem., 2002, 193. G. Tresoldi, S. Lo Schiavo, S.Lanza and P. Cardiano, Eur. J. Znorg. Chem., 2002,181. V.F. Kuznetsov, G.R. Jefferson, G.P.A. Yap and H. Alper, Organometallics, 2002,21,4241. D. Lee and S.J. Lippard, Znorg. Chem., 2002,41,2704. P. Barrio, M.A. Esteruelas and E. Oiiate, Organometallics, 2002,21,2491.
1: N M R Spectroscopy in the L q i and Gas Phase iud

2-
35
CPPh2)Mo(COb] has been examined by variable temperature 'H NMR spectro~copy.~~~

3.1 .I 8 Rhodium and Iridium. The formulation of [(qS-C5Me5)(Me3P)RhH(H2)] is based on T,(min) = 23 ms at 150 K, J(2H'H) = 10 Hz and J(3H'H) = 70 Hz. [{(q5-C5Me5)(Me3P)RhH}2(y-H)] shows hydride exchange with AG: = 9.1 kcal mol- 1.530 Restricted rotation in [p-C1Rh(H)(RSCH2)2C6H3-2,6] been obhas
+
served.531The 31P NMR spectrum of (66)is AB at low temperature and a singlet at room temperature.532
Intramolecular PMe3 exchange has been observed in [(Ph2PCH2CH2SiMe2)Rh(PMe3)2]. Intermolecular exchange is observed when PMe3 is added.533 [Ir(C6H2-2,4,6-Me3)3(PPh3)z] dynamic due to restricted is rotation, P-C bond rotation and PPh3 dissociation.' 34 Variable temperature NMR studies indicate that [Ir(q2-C2H4)2(CO)(dppe)] undergoes three dynamic processes corresponding to ethene rotation, Berry pseudorotation and intermolecular ethene exchange.535Dynamic 'H and I3C NMR spectra of [Rh(q3C3Hs)3]have provided evidence for three different fluxional processes.536The EXSY NMR spectra of [(q3-C3H4Ph)(q4-C8H12)IrC12]rotation.53 'H show ally1
+
529
530
531
532
533
s34
535
536
F.-E. Hong, Y.-C. Chang, R.-E. Chang, S.-C. Chen and B.-T. KO,Organometallics, 2002,21,961. F.L. Taw, H. Mellows, P.S. White, F.J. Hollander, R.G. Bergman, M.Brookhart and D.M. Heinekey, J . Am. Chem. Soc., 2002,124,5100. D.R. Evans, M. Huang, W.M. Seganish, E.W. Chege, Y.-F. Lam, J.C. Fettinger and T.L. Williams, Znorg. Chem., 2002,41,2633. K. Fujita, H. Nakaguma, F. Hanasaka and R. Yamaguchi, Organometallics, 2002,21,3749. M.Okazaki, S. Ohshitanai, H. Tobita and H. Ogino, J . Chem. Soc., Dalton Trans., 2002,2061. B.G. Jacobi, D.S. Laitar, L.H. Pu, M.F. Wargocki, A.G. DiPasquale, K.G. Fortner, S.M. Schuck and S.N. Brown, Znorg. Chem., 2002,41,4815. P.J. Albietz, B.P. Cleary, W. Paw and R. Eisenberg, Znorg. Chem., 2002,41,2095. K.D. John, R. Michalczyk, G. Hernandez, J.C. Green, R.L. Martin, R.T. Baker and A.P. Sattelberger, Organometallics, 2002,21, 5757.
(66)
36
NMR spectroscopy shows restricted rotation of the tolyl rings in syn-[{Rh(p-4HNC6H4Me)(q4-C8H12)}2].The fluxionality of [(2-C5H3N-6-CH2NMe),M(q438 CgH12)] +, = Rh, Ir, is due to nitrogen exchange.539The interconversion of dM and 1-forms of the six-membered chelate cycles in [{ K-R~PCH~CH(OH)CH~-KPR22}Rh(q4-C8H12)] has been in~estigated.~ The fluxionality of [($C 5 M e 5 ) 2 R h 2 ( p - q 5 , q5 - { X C 6 H 4 C H ( C H 2 ) C C ( C H 2 ) CHC6H4X))l2+ been shown to involve q5-q3-q5 has migration of the allylbenzene fragment.541 Restricted naphthyl rotation in (67), Ar = 2-naphthyl, has been observed.542Exchange of the indenyl rings with AG: = 12.4 0.3 kcal mol- 543 has been observed for [Ir2(CO)3(qS-C9H7)3]. The intramolecular dynamics of [Rh4(C0)6(p-PPh2)4] have been investigated using 13C, 31Pand lo3Rh NMR spectro~copy.~~ exchange in [Rh5(CO)13(en)]- been observed.545Re13C0 has stricted rotation of the pyrrole rings in [Rh6(C0)14{ p-P(NC4H4)3}3] been has observed and AH: and AS: determined.546
3.1.19 Nickel, Palladium and Platinum. The H and 31P variable temperature
NMR spectra of (68) show exchange above 283K and temperature dependent shifts at higher t e r n p e r a t ~ r e sA~detailed analysis of the 19F NMR spectra of . ~~ [Pd2(p-pz)2(C6C12F3-3,5)4]2- a dynamic behaviour due to boat invershow ~ i o n . ~ ~ studies have revealed an intramolecular exchange between the NMR pendant and coordinated pyridyl groups in (69).549 Exchange of the inequivalent
537 538
539
540 541
542
543 544 545
546
547
548
549
B. Bartels, C. Garcia-Yebra, F. Rominger and G. Helmchen, Eur. J. Inorg. Chem., 2002,2569. C. Tejel, M.A. Ciriano, M. Bordonaba, J.A. Lopez, F.J. Lahoz and L.A. Oro, Chem.-Eur. J.,2002, 8,3128. T. Sciarone, J. Hoogboom, P.P.J. Schlebos, P.H.M. Budzelaar, R. de Gelder, J.M.M. Smits and A.W. Gal, Eur. J. Inorg. Chem., 2002,457. A. Frick, V. Schulz and G. Huttner, Eur. J. Inorg. Chem., 2002,3129. A. Castro, P.M. Maitlis, M.L. Turner, B.E. Mann and H. Adams, J. Organomet. Chem., 2002,663, 145. L.E. Harrington, J.F. Britten, D.W. Hughes, A.D. Bain, J.Y. Thepot and M.J. McGlinchey, J. Organomet. Chem.,2002,656,243. M.C. Comstock and J.R. Shapley, Organometallics, 2002,21, 5983. E. Gullo, S. Detti, G. Laurenczy and R. Roulet, J. Chem. SOC.,Dalton Trans., 2002,4577. A. Fumagalli, M.C. Malatesta, A. Tentori, D. Monti, P. Macchi and A. Sironi, Inorg. Chem., 2002,41,76. C. Babij, C.S. Browning, D.H. Farrar, 1.0. Koshevoy, I.S. Podkorytov, A.J. Poe and S.P. Tunik, J. Am. Chem. SOC.,2002,124,8922. W. Clegg, G.R. Eastham, M.R.J. Elsegood, B.T. Heaton, J.A. Iggo, R.P. Tooze, R. Whyman and S. Zacchini, Organometallics, 2002,21, 1832. R. de la Cruz, P. Espinet, A.M. Gallego, J.M. Martin-Alvarez and J.M. Martinez-Ilarduya, J . Organomet. Chem., 2002,663,108. M. Sauthier, F. Leca, L. Toupet and R. Reau, Organometallics, 2002,21, 1591.
37
PPh2 groups is observed in (70).550There is a low barrier to phosphorus inversion in [M(dppe){ CH2C6H2Me2P(C6H2-2,4,6-Me3)}], Pd, M = Variable temperature NMR experiments for (71) show restricted rotation of the aryl The 'H and '95PtNMR spectra of (72),553and (73),554 show sulfur inversion. The fluxionality of (74) has been investigated. Nitrogen exchange has been observed in [PtMe(q4-CeH12)(C5H4N-2-CH =NC6H4-4-OMe)].5 The 'HNMR spectra of [{q'-HB(3,5-Me2p~)~}PtMe(CHO)lshow N exchange.557 Addition of external weak nucleophiles to CPtMe(2.9-Me2-1, 10-phen)(PPh3)] accelerates exchange of the nitrogens of the ligand.' 5 8 Restricted rotation about the Pt-P and P-C bonds in complexes such as [Pt{ P(C6H2-2,4,6-Me3)2H}2Et2] has been studied by variable temperature NMR spectro~copy.~Variable tem59 Ph2P-2perature 'H NMR spectroscopy of [(C6F5)2Pd(Ph2PC5H4-q5){ (Me2NCH2)C5H3-q5}Fe] shows two isomers at low t e m p e r a t ~ r e . ~ ~ ' variable The have been retemperature NMR spectra of [ ~ z ~ B ( ~ z ) ~ P ~ ( C ~ F ~ ) ( N C B U ~ ) ] ported.561One C6F5signal is seen in the room temperature 19FNMR spectra of (75) and three in the ratio 1:1:2 at low temperature.562Variable temperature NMR studies have been reported for [Pt2(pdppm)2(p-C=CR)(C=CR)2]5 6 3 . Dynamic NMR spectroscopy has been used to show sulfur inversion and alkene rotation in (76) and AH' and AS: were determined.564 The variable temperature 'H NMR spectra of (77)show 6 different butadiene hydrogen signals at -90 "C and three different ones at room temperature due to S in~ersion?~ P(C7H7)3 fluxional in [M{(q2-C7H7)P(C7H7)2}X2], = Pd, Pt, X is M = C1, Br, I, NCO, NCS, NCSe, N3. 77Se and 195Pt NMR data were reported.566 The barrier for platinum migration around the p-xylene ring in [{1c~-HB(3,5+
550
551
552
553
554
555
556
557
558
559
560
561
562
563
564
565 566
M.A. Zuideveld, B.H.G. Swennenhuis, M.D.K. Boele, Y. Guari, G.P.F. van Strijdonck, J.N.H. Reek, P.C.J. Kamer, K. Goubitz, J. Fraanje, M. Lutz, A.L. Spek and P. van Leeuwen, J. Chem. SOC.,Dalton Trans., 2002,2308. M.A. Zhuravel, D.S. Glueck, L.N. Zakharov and A.L. Rheingold, Organometallics, 2002, 21, 3208. M. Catellani, C. Mealli, E. Motti, P. Paoli, E. Perez-Carreno and P.S. Pregosin, J . Am. Chem. SOC.,2002, 124,4336. A. Knodler, W. Kaim, V.K. Jain and S. Zali, J. Organomet. Chem.,2002,655,218. P.V. Bernhardt, C. Gallego, M. Martinez and T. Parella, Inorg. Chem., 2002,41, 1747. A.N. Vedernikov, J.C. Huffman and K.G. Caulton, Inorg. Chem., 2002,41,6867. F. Di Bianca, G. Bandoli, A. Dolmella, S. Antonaroli and B. Crociani, J. Chem. SOC., Dalton Trans., 2002,212. S. Reinartz, M. Brookhart and J.L. Templeton, Organometallics, 2002,21,247. R. Romeo, L. Fenech, S. Carnabuci, M.R. Plutino and A. Romeo, Inorg. Chem., 2002,41,2839. E.M. Pelczar, E.A. Nytko, M.A. Zhurzvel, J.M. Smith, D.S. Glueck, R. Sommer,C.D. Incarvito and A.L. Rheingold, Polyhedron, 2002,21,2409. B.R. Manzano, F.A. Jalon, F. Gomez-de la Torre, A.M. Lopez-Agenjo, A.M. Rodriguez, K. Mereiter, W. Weissensteiner and T. Strum, Organometailics,2002,21,789. J. Ruiz, F. Florenciano, V. Rodriguez, C. de Haro, G. Lopez and J. Perez, Eur. J. Inorg. Chem., 2002,2736. I. Ara, J. Fornies, A. Garcia, J. Gomez, E. Lalinde and M.T. Moreno, Chem.-Eur.J.,2002,8,3698. K.M.-C. Wong, C.-K. Hui, K.-L. Yu and V.W.-W. Yam, Coord. Chem. Rev., 2002,229,123. L. Canovese, V. Lucchini, C. Santo, F. Visentin and A. Zambon, J. Organomet. Chem.,2002,642, 58. MA. Jalil, T. Nagai, T. Murahashi and H. Kurosawa, Organometallics, 2002,21,3317. M. Herberhold, T. Schmalz, W. Milius and B. Wrackmeyer, Z. Anorg. Allg. Chem., 2002,628, 437.
38
Pt Me I Me Me
(74)
+
(75)
Me2pz)3}Pt(q2-p-Me2C6H4)H] been determined.567 31P has The NMR spectrum of [LPd(q3-C3H4Me)]+, = a calixC4) arene bearing Ph2P groups, is A2at room L Phase sensitive NOESY and ROESY show temperature and AB at - 50 0C.568 that [Pd(q3-RC3H4){~2-Ph2PNR2PPh(N2C3HMe2-3,5)}]+ undergoes syn-anti isomerism.569AGI has been determined for allyl rotation in [CHR(3,5-RR2pz),Pd(q3-2-MeC3H4)] 70 Saturation transfer has shown syn-anti exchange in + [Pd(q3-Me2CCHCH2)(dppb)]+.571 the dynamic NMR spectrum of (78) Effects in appear to be allyl rotation.572[Sn9Pt2(PPh3)I2- highly fluxional in solution is and gives rise to a single time-averaged 19SnNMR Restricted rotation of the PPh3 has been observed in [{HB(3,5Me2C3HN2)3}Pd(PPh3)Cl].574 The temperature dependent H NMR spectra of (79)have been reported. The 195Pt NMR spectrum was also recorded.575 The free
567 568
569
570
571 572
573 574
C.M. Norris, S. Reinartz, P.S. White and J.L. Templeton, Organometallics, 2002,21, 5649. M. Lejeune, C. Jeunesse, D. Matt, N. Kyritsakas, R. Welter and J.P. Kintzinger, J. Chem. Soc., Dalton Trans., 2002,1642. S.K. Mandal, G.A.N. Gowda, S.S. Krishnamurthy, C. Zheng, S.J. Li and N.S. Hosmane, Eur. J . Inorg. Chem., 2002,2047. M.C. Carrion, A. Diaz, A. Guerrero, F.A. Jalon, B.R. Manzano, A. Rodriguez, R.L. Paul and J.C. Jeffery, J. Organomet. Chem., 2002,650,210. M. Ogasawara, K. Takizawa and T. Hayashi, Organometallics, 2002,21,4853. M.A. Pericas, C. Puigjaner, A. Riera, A. Vidal-Ferran, M. Gomez, F. Jimenez, G. Muller and M. Rocamora, Chem.-Eur. J., 2002,8,4164. B. Kesanli, J. Fettinger, D.R. Gardner and B. Eichhorn, J. Am. Chem. SOC.,2002,124,4779. H.O.Do, J.H. Lee, H Kim and S. Park, J. Coord. Chem., 2002,53,143.
39
'" -,
Me
(76)
--a-
Ph
(77)
and coordinated ends of Me2phen in [PtX2( L)(2,9-Me2phen)]exchange rapidly at room temperature but the exchange slows at 213K.576ROESY is used to look at exchange in (80)due to different conformation^.^^^ Inversion of E is observed in [RBu'Si(p-EHhM(dppe)], E = P, As; M = Ni, Pd, Pt.578 The variable 19F and 31P NMR spectra of [PdAg(ptemperature 'H, 02CCF2CF3)2(02CCF2C3)(dppf)] show exchange between p- and o - O ~ C R . ' ~ ~ 10S3, has been invesThe fluxional behaviour of the 174,7-trithiacyclodecane, tigated in [Pt( 10S3)(PPh3)Cl]+and the 195Pt NMR spectrum reported.580 The variable temperature 31PNMR spectra show fast H transfer between sulfur at atoms in [Pt2(dppe)z(p-S)(p-SH)J+ room temperature which is slow.581The NMR spectrum of (81)is AB at room temperature and variable temperature 31P broadens on The 'H NMR spectra of (82) show phenyl exchange due to restricted rotation of the p h e n y l ~ . ~ ~ ~
3.1.20 Copper. AGI = 13.6 kcal mol-' for helical isomerism of (83).584 Exchange
of the methylene protons in [Cu2L2I2+, = (U), been ~bserved.'~' L has Movement of c u ' around the ligand, (pz-1)6c6, has been investigated.586
3.1.21 Silver. The fluxional behaviour of [Ag{ N(CH2CH2SCH2CH2)3-1,3,5-
C6H3}] has been investigated.587The variable temperature 31P + NMR spectrum of [(P4)AgAl{ OCMe(CF3)2}4]2 been reported and the 27AlNMR spectrum has measured.
575
576
577
"'
579
''O
'"
'*
583
584
585
'"
'"
'"
K.S. Schmidt, J. Reedijk, K.Weisz, E.M.B. Janke, J.E. Sponer, J. Sponer and B. Lippert, Inorg. Chem., 2002,41,2855. N. Margiotta, F.P. Fanizzi, R.Cini, G. Tamasi and G. Natile, Inorg. Chim. Acta, 2002,339,503. A.J. Baer, B.D. Koivisto, A.P. Cote, N.J. Taylor, G.S. Hanan, H. Nierengarten and A. Van Dorsselaer, Inorg. Chem., 2002,41,4987. M. Driess, F. Franke and H. Pritzkow, J. Organomet. Chem., 2002,643,468. Y.C. Neo, J.J. Vittal and T.S.A. Hor, J. Chem. SOC.,Dalton Trans., 2002,337. G.J. Grant, D.F. Galas and D.G. VanDerveer, Polyhedron, 2002,21,879. G. Aullon, M. Capdevila, W. Clegg, P. Gonzalez-Duarte, A. Lled6s and R. Mas-Balleste, Angew. Chem., Int. Ed. Engl., 2002,41,2776. J.S.L. Yeo, J.J. Vittal, W. Henderson and T.S.A. Hor, Organometallics, 2002,21,2944. S. Doherty, E.G. Robins, M. Nieuwenhuyzen, J.G. Knight, P.A. Champkin and W. Clegg, Organometallics, 2002,21, 1383. M.A. Heuft and A.G. Fallis, Angew. Chem., Int. Ed. Engl., 2002,41,4520. J. Mathieu, A. Marsura, N. Bouhmaida and N. Ghermani, Eur. J. Inorg. Chem., 2002,2433. A.M. Guerrero, F.A. Jalon, B.R. Manzano, R.M. Claramunt, M.D. Santa Maria, C. Escolastico, J. Elguero, A.M. Rodriguez, M.A. Maestro and J. Mahia, Eur. J . Inorg. Chem., 2002,3178. J.M. Baumeister, R. Alberto, K.Ortner, B. Spingler, P.A. Schubiger and T.A. Kaden, J. Chem. SOC.,Dalton Trans., 2002,4143. I. Krossing and L. van Wullen, Chem.-Eur. J.,2002,8,700.
40
CH; C6Hl 1
(79)
i8Se LPhJP)pPt/\
se
Pt(PPh3)?
3.1.22 Gold. AG: has been determined for (85).589

P h 3 P A u G C C 3 d
41
Ph3PAUC&C H,
PhCH,CH,
(85)
Zinc. Exchange of the aromatic protons in [Zn(H2L)(HNCH2CH2)3],H4L a calix[4]arene, has been observed.590The variable temperature 'H NMR spectrum of (86)shows that the zinc commutes around the ligand.591[ZnC12{(2C5H4NCH2)2NCH2-2-CsH3N-6-C6H3-2,5-(0Me)2}] shows inversion about the ligand amine group with AGt = 5 & 0 5 kJ m 0 1 - l . ~Carboxylate shift in 6 . ~~ [ZQ{ (Me2NCH2)2CHOH}2(02CR)6] been observed and activation parhas ameters determined. J9
3.1.23
=
(86) 3.1.24 Cadmium. The dynamics of interdomain and intermolecular interactions
in mammalian metallothioneins have been investigated by 'I3Cd NMR spectroscopy.5%

3.1.25 Boron. The variable temperature 'H and "B NMR spectra of [(I$-
C5HJ2Rh2B3H7] show fluxionality.5 9 5 The fluxional behaviour of [ClCuB3Hg] has been studied the~retically.'~~ variable temperature 'H NMR spectra of The [{(q5-C5H5)ZrCl}B5H8] show that the B-H-B protons exchange between - 60 "C
589
590
591
592
593
594
595
596
D. Eisler, W. Hong, M.C. Jennings and R.J. Puddephatt, Organometallics, 2002,21,3955. T. Kajiwara, S. Yokozawa, T. Ito, N. Iki, N. Morohashi and S. Miyano, Angew. Chem., Znt. Ed. Engl., 2002,41,2076. C. Seward, J. Pang and S. Wang, Eur. J. Znorg. Chem., 2002,1390. Z.C. He, D.C. Craig and S.B. Colbran, J. Chem. Soc., Dalton Trans.,2002,4224. A. DemSar, J. KoSmrlj and S. Petrikk, J . Am. Chem. Soc., 2002,124,3951. K. Zangger and I.M. Armitage, J. Znorg. Biochem., 2002,88,135. H. Yan, A.M. Beatty and T.P. Fehlner, Organometallics, 2002,21,5029. C. Serrar, A. Es-Sofi, A. Boutalib, A. Ouassas, A. Jarid, I. Nebot-Gil and T. Tomas, J. Phys. Chem. A, 2002,105,9776.
42
and room temperature.597 The fluxionality of the BH3 has been observed in [8,8-{q2-(H3B)dppm}-nido-8,7-RhS&Hlo].s98 adducts of PhCR = MCH2Ph, In ButMeC = NCH2Ph and PhHC = NPh with B(C6F5)3, steric crowding and nstacking results in restricted rotation about the B-N and B-C bonds.599The variable temperature 'H NMR spectra of [B(NC5H6-2,2,6,6-Me4)(4,5-Me2imida~olyl)~] show methyl exchange and the "B NMR spectrum was reported.600
3.1.26 Aluminium and Gallium. The barriers to inversion of the [Me2MCH2-
SMe12six-membered rings are 39 kJ mol-' for M = A1 and 36 kJ mol-' for M = Ga.601 AG: has been determined for nitrogen inversion in [(Me2Ga)4(N2H2)(NHNH2)2] 'Li and 29SiNMR spectra have been reported and for (87).602 Diffusion of methylaluminoxane in toluene has been probed by 'H NMR spin-lattice relaxation time
(87)
3.1.27 Carbon. The reorientation kinetics of cyanogen bromide have been investigated using 13Cand 15NNMR spectroscopy.604
3.1.28 Silicon. Inversion barriers and 29Si chemical shifts of silyl anions have been calculated.605 AG: has been determined for ring inversion in 1-Me-l-silacyclohexane.606The 'H NMR spectra of (88)show two But signals in the ratio 1:2 at 245 K and one at 298 K due to Br migration.607Changes in the NMR spectra of [(2,6-Pri2C6H3)P(SiMe2But)2] due to restricted rotation about the P-C bond are with AG: = 40 kJ mol-' and phosphorus inversion with AG' = 72 kJ mol-1.608 The variable temperature 'H and 29Si NMR spectra of trans[ClBu'Si(CPh = CPh)2SiButC1]show restricted rotation of the phenyl Methyl exchange in (89) has been studied and the 29SiNMR spectrum recorded.610 The variable temperature 'H NMR spectra of (90) show methyl
597 598 599
600
60 1
602
603
604
605 606
607
608
609
610
R.L. Thomas, N.P. Rath and L. Barton, Inorg. Chem., 2002,41,67. 0.Volkov, R. Macias, N.P. Rath and L. Barton, Inorg. Chem., 2002,41,5837. J.M. Blackwell, W.E. Piers, M. Parvez and R. McDonald, Organometallics, 2002,21, 1400. A. Weiss, H. Pritzkow and W. Siebert, Eur. J . Inorg. Chem., 2002, 1607. C . Lustig and N.W. Mitzel, Organometallics, 2002,21, 3471. H. Noth and T. Seifert, Eur. J . Inorg. Chem., 2002,602. E.W. Hansen, R. Blom and P.O. Kvernberg, Macromol. Chem. Phys., 2001,202,2880. S . Molchanov and A. Gryff-Keller,Mol. Phys., 3002,100, 3349. M. Flock and C. Marschner, Chem.-Eur. J . , 2002,8, 1024. I. Arnason, A. Kvaran, S. Jonsdottir, P.I. Gudnason and H. Oberhammer, J . Org. Chem., 2002, 67,3827. A. Sekiguchi, Y. Ishida, N. Fukaya, M. Ichinohe, N. Takagi and S. Nagase, J . Am. Chem. Soc., 2002,124,1158. R.T. Boere and J.D. Masuda, Can. J . Chem., 2002,80,1607. J.C. Yang, I. Guzei and J.G. Verkade, J . Organomet. Chem., 2002,649,276. A.R. Bassindale, Y.I. Baukov, P.G. Taylor and V.V. Negrebetsky, J . Organomet. Chem., 2002, 655, 1.
43
exchange between inside and outside.61 The 'H NMR spectrum of (91) changes from AB to A2 and the 29SiNMR spectrum was recorded.612
3.1.29 Lead. The variable temperature 'H NMR spectra of [PbLI2+, L = 2-H2NC6H4CH2N{(CH2CH20),CHzCHz)2NCH2C6H4-2-NH2, show changes due to conformational exchange.61
3.1.30 Phosphorus. The fluxionality of [RP{(CH2)4}2] been investigated.6l 4 has Dynamic NMR spectroscopy has been applied to racemisation of spiro-2,2'dioxybiphenyl-cyclotriphosphazenes.6l 5 31P NMR spectroscopy has been used to study exchange in (92) due to inversion at phosphorus.616 Variable temperature 'H and 3'P NMR spectra of (93) show exchange.617Variable temperature I3C NMR spectroscopy has been used to look at exchange in (94).618The variable temperature 'H NMR spectra of [Ph3PAsMePh]+ shows P-As bond
61 612
613
614 615
616
617
618
P. Sood, H.M. Zhang and M. Lattman, Organometallics, 2002,21,4442. E. Gomez, Z. Hernandez, C. Alvarez-Toledano, R.A. Toscano, V. Santes and P. Sharma, J. Orgunomet. Chem., 2002,648,280. D. Esteban, F. Avecilla, C. Platas-Iglesias, J. Mahia, A. de Blas and T. Rodriguez-Blas, Inorg. Chem., 2002,41,4337. U. Monkowius, N.W. Mitzel, A. Schier and H. Schmidbaur, J . Am. Chem. SOC.,2002,124,6126. M.E. Amato, G.A. Carriedo, F.J.G. Alonso, J.L. Garcia-Alvarez, G.M. Lombard0 and G.C. Pappalardo J. Chem. SOC.,Dalton Trans.,2002,3047. S. Matsukawa, S. Kojima, K. Kajiyama, Y. Yamamoto, K. Akiba, S.Re and S. Nagase, J. Am. Chem. SOC.,2002,124,13 154. P. Kommana, S. Kumaraswamy, J.J. Vittal and K.C.K. Swamy, Inorg. Chem., 2002,41,2356. S.L. Renard, J. Fisher,C.A. Kilner, M. Thornton-Pett andT.P. Kee, J. Chem. SOC.,Dalton Trans., 2002,292 1.
44
breaking.61931P NMR spectroscopy has been used to show exchange in [P316]+ with the spectrum being AX2 at 183 K and a broad A3at room temperature. The 27A1 NMR spectrum of [Al(OR),]- was also reported.620
(92)
(93)
But
But
3.1.31 Bismuth. The variable temperature 'H NMR ((Me3Si)2CH}2BiBi(CH(SiMe3)2}2] been examined.621 have
spectra
of
3.1.32 Selenium and Tellurium. Conformational inversion of 9-(9'H-fluoren-9'ylidene)-9H-selenoxantheneand 9-(9'H-fluoren-9'-ylidene)-9H-telluroxanthene has been investigated by 'H, "Se and '25TeNMR spectroscopy.622
3.2 Ionic Equilibria. - A self-consistent microscopic theory of ionic self diffusion in concentrated aqueous solution has been developed and explains recent NMR data.623The critical behaviour of NMR shifts and relaxation times in ionic solutions has been reported.624NMR relaxation data have been used to study the influence of hydration numbers in aqueous solutions of electrolytes on the activation energies of molecular The effect of common ions such as Na+, K+, Ca2+,Mg2+, C1-, [SO,]'- and [C03]'- on water concentration has
619
620 621 622
623
624 625
K.A. Porter, A.C. Willis, J. Zank and S.B. Wild, Inorg. Chem., 2002,41,6380. I. Krossing, J . Chem. Soc., Dalton Trans., 2002, 500. G. Balazs, H.J. Breunig and E. Lork, Organometallics, 2002,21,2584. A. Levy, P.U. Biedermann, S. Cohen and I. Agranat, J . Chem. Soc., Perkin Trans. 2,2001,2329. J.F. Dufreche, 0. Bernard, P. Turq, A. Mukherjee and B. Bagchi, Phys. Rev. Lett., 2002, 88, 095902/1. V. Balevicius and R. Blinc, Lithuanian J . Phys., 2001,41,495. N.A. Mel'nichenko, A.V. Bazhanov and A.S. Kupriyanov, Zh. Fiz. Khim., 2002,76,858.
45
been studied by measuring the 170 NMR chemical shift and line width of water.626'Hand I3CNMR studies on thiosemicarbazides and their interaction with Ca2+,Co2+,Ni2+,Zn2+ and Pb2+have been reported.627The solvation structures and solvent exchange reactions of metal ions in various coordinating solvents have been investigated using high-pressure NMR spectroscopy.62 'H NMR titrations of poly[(R)-3-{4-(4-Et-2-oxazolin-2-yl)-phenyl} thiophene] with Fe", Cu', Cu", Ag' and Zn" have been reported.629Solvent extraction of Fe" from Nit', Cu" and Zn" using N,N'-substituted malonamides has been studied using NMR spectroscopy.630 The interaction of 4,7,10,13-tetra-azahexadecane1,16-diamine and 4,7,1O-triazatridecane-l,13-diamine H+,Co2+, with Cu2+and Zn2+has been followed by NMR spectroscopy.631 NMR relaxation method The has been used for determining the coordination numbers of oxygen containing polyatomic anions in diamagnetic aqueous solutions.63 3.2.1 Group 1. Variable temperature 13C{ 'H} NMR spectroscopy shows interchange between diastereomeric isomers of 1,4,7-tris{(S)-2-HO-3PhCHzCH2CH2}-1,4,7-triazacyclon~naneand Na+. 6 3 3 The exchange kinLi+ etics of Li+ C221 cryptate have been studied by 7LiNMR lineshape analysis and the activation parameters were determined.634 The interaction of Co"' complexes of macrocyclic amines tethered to benzo-crown ethers with alkali metal ions has been studied by 7Liand 23NaNMR spectroscopy.635 transport and Ion dynamics have been studied by 'H, 7Li and 19Fpulsed field gradient spin-echo NMR spectroscopy.636 The ability of tris(macrocyc1ic)compounds with sidearms to transport Na has been assayed by 23NaNMR spectroscopy.637 23NaNMR spectroscopy has been used to study Na+ exchange in (95).638 Complex formation equilibria of phosphocreatine with Na+, K + and Mg2+have been investigated by 31P NMR 23Naand '39La NMR studies have been applied to cation binding to aqualysin I.640 Cation-induced complex formation between poly+
626
627
628
629
630
631
632
633
634
635
636
637 638
639
640
R. Li, Z. Jiang, S. Shi, H. Yang and S. Yuan, Huanjing Kexue, 2002,23,44. B. Sireesha, G.S. Reddy, G.G. Kumari, C.S. Devi and M.G.R. Reddy, Proc. Nut. Acad. Sci., India, A: Phys. Sci,, 2002,70,381. S. Funahashi and Y. Inada, Bull. Chem. SOC.Jpn., 2002,75,1901. H. Goto, Y. Okamoto and E. Yashima, Chem.-Eur.J., 2002,8,4027. M.C. Costa, C.E. Fernandes, M.J. Hudson and P.B. Iveson, Solvent Extraction for the 21st Century, Proceedings o ISEC '99, Barcelona, Spain, July 11-16,1999,2001,1,271. f J. Aguilar, P. Diaz, F. Escart, E. Garcia-Espana, L. Gil, C. Soriano and B. Verdejo, Inorg. Chim. Acta, 2002,339,307. V.I. Chizhik, A.V. Egorov, A.V. Komolkin and A.A. Vorontsova, J . Mol. Liq., 2002,98-99, 173. J.M. Weeks, M.A. Buntine, S.F. Lincoln and K.P. Wainwright, Inorg. Chim. Acta, 2002,331,340. M. Shamsipur, T. Madrakian and E. Karkhaneei, Main Group Met. Chem., 2002,25,271. P.V. Bernhardt and E.J. Hayes, Inorg. Chem., 2002,41,2892. P. Gavelin, P. Jannasch, I. Furo, E. Pettersson, P. Stilbs, D. Topgaard and 0. Soederman, Macromolecules, 2002,35,5097. S.L. De Wall, E.S. Meadows, C.L. Murray, H. Shabany and G.W. Gokel, Supramol. Chem.,2000, 12,13;C.L. Murray and G.W. Gokel, J . Supramol. Chem., 2001,1,23. M. Botta, U. Casellato, C. Scalco, S. Tamburini, P. Tomasin, P.A. Vigato, S. Aime and A. Barge, Chem.-Eur.J., 2002,8, 3917. F. Cecconi, C. Frassineti, P. Gans, S. Iotti, S. Midollii, A. Sabatini and A. Vacca, Polyhedron, 2002,21, 1481. K. Suefuji, S.-J. Lin, T. Wakagi, H. Matsuzawa and E. Yoshimura, Biosci. Biotechnol. Biochem., 2002,66,1281.
46
uridylic acid and schizophyllan has been investigated by 23NaNMR spectroscoDv.641

2+
(95)
7Li and I9F pulsed field gradient spin echo has been used to study Li+ self-diffusion and transport number in non-aqueous electrolyte solutions.6427Li, 23Na, and '33Cs 39K NMR spectroscopy has been used to carry out a comparative equilibrium study of alkali cation hydroxide complexes in aqueous solutions.643 Spin-lattice relaxation times have been used to study aqueous solutions of electrolytes at high temperatures and pressures.644Temperature and pressure I effects on the T of 2H of DzO in alkali bromide solutions have been Using pulsed field gradient 'H, 7Li and I9F NMR spectroscopy, liquid electrolytes composed of glymes and polyetheneglycol dimethyl ethers doped with [LiN(S02CF3)2]were investigated.646 'H and 7Li lineshape and TI measurements have been used to study the polymer electrolyte formed by ethylene glycol, citric acid and LiC104.647 and Na+ complexation by silicon podant solvents Li+ has been studied using 'H, 7Li, 13Cand 23NaNMR spectroscopy.648The complexation of Li+ and Na+ cations by three bis(oxaalky1)sulfites has been studied by 'H, 7Li,I3Cand 23NaNMR spectroscopy.6497LiNMR spectroscopy has been used to study the ability of crown ethers attached to carbon tubes to bind Li+.650 Electrostatic coupling between various sodium arylsulfonates and homopolymers of [(C3H5)2NMe2]Cl been studied using 'H and 35ClNMR has spectroscopy, including pulsed field gradient^.^ NMR pulsed field gradient
641
642 643
644
645
646
647
648
649
650
651
K. Sakurai, R. Iguchi, K. Koumoto, T. Kimura, M. Mizu, Y. Hisaeda and S. Shinkai, Biopolymers, 2002,65, 1. M. Videa, W. Xu,B. Geil, R. Marzke and C.A. Angell, J. Electrochem. Soc., 2001,148, A1352. K. Popov, L.H.J. Lajunen, A. Popov, H. Ronkkomaki, M. Hannu-Kuure and A. Vendilo, Inorg. Chem. Commun., 2002,5,223. N. Matubayashi, N. Nakao, M. Kubo, H. Tsunashima and M. Nakahara, Koatsuryoku no Kagaku to Gijutsu, 2001,11, 132. K. Fumino, A. Shimizu and Y. Taniguchi, J. Mol. Liq., 2002,95,193. K. Hayamizu, E. Akiba, T. Bando and Y. Aihara, J. Chem. Phys., 2002,117,5929. C.E. Tambelli, J.P. Donoso, C.J. Magon, J. Schneider, E.C. Pereira and A.V. Rosario, Mol. Cryst. Liq. Cryst. Sci. Technol., Sect. A, 2002,374,141. M. Beltowska-Brzezinska, T. Luczak, B. Gierczyk, K. Eitner, B. Brzezinski, R. Pankiewicz and G. Schroeder, J. Mol. Struct., 2002,607,77. G. Schroeder, B. Gierczyk, B. Leska, G. Wojciechowski, R. Pankiewicz, B. Brzezinski and F. Bartl, J . Mol. Struct., 2002,607,9. M.G.C. Kahn, S. Banerjee and S.S. Wong, Nano Lett., 2002,2, 1215. J. Kriz, J. Dybal and D. Kurkova, J. Phys. Chem. B, 2002,106,2175.
1 :N M R Spectroscopy in the Liquid and Gas Phase
47
NMR spectroscopy has been used to study aqueous solutions of NaC1, NaN3, 18-crown-6crown ether and f b c y ~ l o d e x t r i nThe fractions and concentrations .~~~ of H 2 0and NaCl in a sub-eutectic quasi-liquid phase have been measured by 'H and 23Na NMR spectroscopy.653 23NaNMR spectroscopy has been used to study the interaction between hyaluronan and Ca2+,Mg2+ and Cu2+.654 A non-peptide, cation conducting channel has been studied using dynamic 23Na NMR spectroscopy in phospholipid vesicles.65 Extremely slow counterion dynamics in xanthan liquid crystal have been investigated using I4N and 23Na NMR spectroscopy.656 A 'H, I7O, 23Na and 3'P NMR investigation of the NaDNA/ethidium bromide anisotropic system has been r e p ~ r t e d . ~Ordering of alkali halide salts dissolved in bacteriophage Pfl solutions has been studied using 23Na,3'C1, 3yKand 79BrNMR An NMR study of 'H and 'H in the mesomeric phases of the micellar lyotropic mixture, K laurate/ldecanol/D20has been published.659The slow orientational dynamics of water molecules at a micellar surface of C7F1SC02Cshave been investigated using NM R spectroscopy.660 3.2.2 Magnesium, Calcium, Strontium and Barium. Complex formation of Ca2 with (96)has been studied by 'H and I3CNMR spectroscopy.661Conformational changes in Ca2+ bound S-100 proteins caused by Mg2+ binding have been investigated using I9F NMR spectroscopy.662 Ionic solvation of alkali earth cations with HMPA has been studied using ' H NMR spectroscopy and solvation numbers were determined.663 Bifunctional binding and recognition of biotin and related ligands by [Mg( 15-crown-5)I2+has been investigated using NMR spectroscopy.664The interaction of lower rim calix(4)arene derivatives with Mg2+,Ca2+,Sr2+, Ba2+,Hg2+,Pb2+and Cd2+has been studied using 'H NMR spectroscopy.665Calcium binding to inositols linked through 0 or N has been investigated using 'H NMR spectroscopy.66613CNMR spectroscopy has been used to characterise the effect of pH on the formation of barium titanium citrate gel.66713NaNMR spectroscopy has been used to study the interaction
+
6s2
6s3
6s4
6ss
6s6
6s7
6s8
'''
660 661
663
664
66s
666
667
F. Hallwass, M. Engelsberg and A.M. Simas, Chem. Commun., 2002,2530. H. Cho, P.B. Shepson, L.A. Barrie, J.P. Cowin and R . Zaveri, J . Phys. Chem. B, 2002,106,11226. M. Adrian-Scotto, M. Guibbolini, G. Mallet, M. Gaysinski and D. Vasilescu, J . Biomol. Struct. Dyn., 2002, 19,7 15. G.W. Gokel, Cell Biochem. Biophys., 2001,35,211. J.R.C.van der Maarel, D.E. Woessner and M.E. Merritt, J . Phys. Chem. B, 2002,106,3864. A. Catte, F.C. Marincola, M. Casu, G. Saba and A. Lai, J . Biomol. Struct. Dyn., 2002,20,99. S . Vyas, C.J. Hernandez and M.P. Augustine, J . Chem. Phys., 2002,116,7109. C.R. Rodriguez, D.J. Pusiol, A.M. Figueiredo Net0 and R.O. Seitter, Phys. Rev. E: Stat., Nonlinear, Soft Matter Phys., 2002,65,031703/1. S. Balasubramanian and B. Bagchi, J . Phys. Chem. B, 2002,106, 3668. C.D. Hall and N . Djedovic, J . Organomet. Chem., 2002,648,8. S. Matsuda, Bull. Chem. SOC.Jpn., 2002,75,2503. N. Alizadeh and M.K. Amini, Iranian J . Chem. Chem. Eng., 200420, 12. E.R. Sanchez, M.C. Gessel, T.L. Groy and M.T. Caudle, J . Am. Chem. Soc., 2002,124,1933. A.F.D. de Namor, S. Chahine, D. Kowalska, E.E. Castellano and O.E. Piro, J . Am. Chem. Soc., 2002,124,12 824. B.J. Paul, J . Willis, T.A.Martinot, I. Ghiviriga, K.A. Abboud and T. Hudlicky, J . Am. Chem. Soc., 2002,124, 10 416. T.-T. Fang and J.-D. Tsay, J . Am. Ceram. Soc., 2001,84,2475.
48
between hyaluronan and Mg2+,Ca2+ and The interaction between ciprofloxacin and DNA mediated by Mg2+has been investigated using 'HNMR spectroscopy.669
3.2.3 Yttrium. The solution speciation of YX3 complexes of R3E0,E = As, P, has been investigated using "Y NMR spectroscopy.670 3.2.4 Lanthanum and the Lanthanides. The temperature dependence of the 'H NMR spectrum of [(r15:r5'-C24H16)L~I(THF)] H F is indicative of the dyin T namic exchange of solvent molecules.671 13'La NMR spectroscopy has been applied to kinetic and equilibium studies of the substitution of coordinated water by acetohydroxamic 'H NMR spectroscopy has been used to study water exchange and relaxometric properties of Gd"' complexes with DTPAbis(amide) l i g a n d ~ . ~ Gd"' induced NMR relaxation rate measurements have shown that an EDTA-linked P-cyclodextrin dimer forms a 1:2 complex 4B u ~ C ~ H ~The solution.structures of Ln"' complexes of DTPA-BIN have C ~ ~ - ~ ~ ~ been investigated using 'H and 13CNMR 2H I7Orelaxation and measurements have been carried out on (4S)-4-PhCH2-3,6,10-(H02CCH2)33,6,10-triazadodecanedioic complexes of Gd3 .6 7 6 The formation constants acid of Gd3+ with some bis(amino acid) ligands have been determined from NMR relaxation measurement^.^^ The hydration number of [Dy{ TETA-(POh}13The contributions of diffusion has been measured by 1 7 0 NMR spectroscopy.678 and exchange in relaxation by MRI contrast agents have been evaluated.679'H,
668
669 670 671
672 673
674 675 676
677
678 679
M. Adrian-Scotto, M. Guibbolini, G. Mallet, M. Gaysinski and D. Vasilescu, J . Biomol. Struct. Dyn., 2002,19, 715. T . Skauge, I. Turel and E. Sletten, Znorg. Chim. Acta, 2002,339,239. N.J. Hill, W. Levason, M.C. Popham, G. Reid and M. Webster, Polyhedron, 2002,21,445. I.L. Fedushkin, Y.A. Kurskii, V.I. Nevodchikov, M.N. Bochkarev, S. Muechle and H . Schumann, Russ. Chem. Bull., 2002,51, 160. M. BiruS, R. van Eldik, M. GabriEeviE and A. Zahl, Eur. J . Znorg. Chem., 2002,819. T.-H. Cheng, K.-T. Lin, M.-H. Ou, H.-L. Shih, G.-C. Liu and Y.-M. Wang, J. Chin. Chem. SOC. (Taipei, Taiwan), 2001,48, 1099. J.J. Michels, J. Huskens and D.N. Reinhoudt, J . Am. Chem. SOC.,2002,124,2056. J.-h. Feng, X.-j. Li, X.-y. Li and F.-k. Pei, Gaodeng Xuexiao Huaxue Xuebao, 2001,22,1615. T . H . Cheng, T.M. Lee, M.H. Ou, C.R. Li, G.C. Liu and Y.M. Wang, Helu. Chim. Acta, 2002,85, 1033. H . Miyake, M. Watanabe, M. Takemura, T. Hasegawa, Y. Kojima, M.B. Inoue, M. Inoue and Q. Fernando, J. Chem. Soc., Dalton Trans., 2002,1119. B. Song, T. Storr, S. Liu and C . Orvig, Znorg. Chem., 2002,41,685. Y. Gossuin, A. Roch, R.N. Miller and P. Gillis, J . Magn. Reson., 2002, 158, 36.
49
I3C and I5N NMR spectroscopy has been used to study complex formation between La3+,Tm3+ and Yb3+ and [NO3]- and [NCS]-.680 The fuc-mer isomerism and exchange of free and coordinated HMPA on [LnC13(HMPA)3] have been investigated using 'H NMR spectroscopy.68 The stability constants of inner- and outer-sphere complexes of [La{ 2-thienyl-C(0)CHC(O)CF3}3] with [C~(acac)~] have been determined by 59C0NMR spectroscopy.682 13C NMR spectroscopy has been used to study the complexation of Th'" with various lanthanides(II1) by glycolic The nature of equilibrium shifts in racemic [Pr(2,2'-0xydiacetate)~]~induced by L-proline and its derivatives has been 13CNMR spectroscopic studies on investigated using 'H NMR the complexing ability of D-erythro-L-manno-D-gluco-dodecitol with La3+and Pr3+in water have been reported.685'39LaNMR spectroscopy has been used to study the complexation of La3+with p-sulfonatocalix[4]arene.686 The change in and interconversion of conformers of two cavitands on binding to La3+has been in~estigated.~'~ Molecular factors that determine the Curie spin relaxation in dysprosium complexes have been investigated using I7ONMR spectroscopy.688 EXSY has been used to study exchange in the Yb3+ complex of 1,4,7,10(H02CCHJ4-2-Me-1,4,7,1 O-tetraazacyclododecane.6 Lanthanide complexes 89 10-(H02CC0)4-1,4,7,10-tetraa~acyclododecane been shown to be have of 1,4,7, pH reported MRI contrast agents.690
'
3.2.5 Uranium.The selective complexation of U"' over Ce"' and Nd"' by terThe pyridine has been shown by 'H NMR spectro~copy.~~' rates and mechanhave been ism of F- and H 2 0 exchange in [UO2F5I3-and [UO2F4(0H2)I2studied by NMR 'H, I7O,19Fand 31P NMR spectroscopy has been used to study equilibrium and ligand exchange dynamics in binary and ternary dioxouranium(V1)-glyphosate-F- systems.693 3.2.6 Titanium. 'H NMR spectroscopy has been used to investigate self-recognition of [{ 2,3-02C6H3(-1,4-C6H4)n'C6H302-2,3}3Ti2]4- of Li+, in the presence Na+, K' or [NH4]+.694
A. Fratiello, V. Kubo-Anderson, R. Lee, M. Patrick, R. Perrigan, T. Porras, S. Sharma and S. Stoll, J. Solution Chem., 2002,31,681. "' S. Petricek and A. Demsar, Zbornik Referatov s Posvetovanja Slovenski Kemijski Dnevi, Maribor, Slovenia, Sept. 20-21,2001,2001,911. 6 8 2 N. Kameta, H. Imura, K. Ohashi and T. Aoyama, Polyhedron, 2002,21,805. 6 8 3 T. Toraishi, I. Farkas, Z. Szabo and I. Grenthe, J . Chem. SOC.,Dalton Trans., 2002,3805. 684 T.N. Parac-Vogt, K. Binnemans and C. Gorller-Walrand, J. Chem. SOC.,Dalton Trans., 2002, 1602. M. Mach, E. Utzig and S. Jarosz, Pol. J. Chem., 2002,76, 565. "' Y. Israeli, C. Bonal, C. Detellier, J.P. Morel and N. Morel-Desrosiers, Can. J. Chem., 2002, 80, 163. 6 8 7 P. Amrhein, A. Shivanyuk, D.W. Johnson and J. Rebek, J . Am. Chem. SOC.,2002,124,lO 349. P. Caravan, M.T. Greenfield and J.W.M. Bulte, Magn. Res. Med., 2001,46,917. 6 8 9 R.S. Ranganathan, N. Raju, H. Fan, X. Zhang, M.F. Twedle, J.F. Desreux and V. Jacques, Inorg. Chem., 2002,41,6856. 690 S. Aime, D. Delli Castelli and E. Terreno, Angew. Chem., Int. Ed. Engl., 2002,41,4334. 6 9 1 J.-C. Berthet, C. Riviere, Y . Miquel, M. Nierlich, C. Madic and M. Ephritikhine, Eur. J. Inorg. Chem., 2002,1439. 6 9 2 V. Vallet, U. Wahlgren, Z. Szabo and 1. Grenthe, Inorg. Chem., 2002,41,5626. 6 9 3 Z. Szabo, J. Chem. SOC.,Dalton Trans., 2002,4242.
50
3.2.7 Zirconium. The displacement of [MeB(C6F5)3] from seven different zirconocene methyl cations by neutral Lewis bases has been investigated by NMR spectro~copy.~~ 3.2.8 Vanadium. Aqueous solutions of 4-hydroxypyridine-2,6-dicarboxylatodioxovanadate(V) complexes have been investigated using 'H, I3C, 1 0 7 and "V NMR spectroscopy.696Coordination between [V(04C2)(0)(02)2]and histidine has been monitored by 51VNMR spectroscopy.697"V NMR spectroscopy has been used to investigate complexation of [V0413- with 2HOC6H4CH2NHCH2C(0)NHCH2C(O)NHCH2C02H.698 Isomerism between a-cis and P-cis-[( 1,2-propylenediarninetetraa~etate)Va]~- has been studied quantitatively by "V NMR spectroscopy.699 3.2.9 Tantalum. The effect of [Bun4N]Cl on the equilibrium between [Ta{ 02C20Hlo(SiMe3)2-3,3'}2C12] - and [Ta{ 02C20H10(SiMe3)2-3,3'}2Cl]has been investigated by 'H NMR spectroscopy.700
3.2.10 Molybdenum. 'H NMR spectroscopy has been used to follow MeCN Molybdate exchange in [ ( T ~ ~ - C ~ H ~ ) M ~ ( P ~ ~ P C H M ~ C H ~ P P ~ ~ ) ( N C M ~ ) ] equilibria have been investigated in LiC104 and NaCl media using 9 5 MNMR ~ NMR spectroscopy shows the equilibria in Scheme 2.703 spectroscopy.70231P The equilibrium speciation in aqueous H '/[MOO~]'-/[HVO~]~-/[HPO~]~-/~has been carried out using in part "V NMR spectroscopy.704Equilibria and dynamics in the H+/[MOO~]'-/H~O/[SO~]~- been studied using I7O and have 95M~ NMR including I7ONMR EXSY The pH dependence of phosphomolybdate species has been studied using 31P NMR spectroscopy. O7
'
Scheme 2
694 695
696
697
698
699 700
701
702
703
704 705
706
707
M. Albrecht and M. Schneider, Eur. J. Inorg. Chem., 2002,1301. F. Schaper, A. Geyer and H.H. Brintzinger, Organometallics, 2002,21,473. L.Q. Yang, A. La Cour, O.P. Anderson and D.C. Crans, Inorg. Chem., 2002,41,6322. J.L. Ye, X.W. Zhou, Z. Chen, Z.W. Chen and P.Q. Huang, Chin. Chem. Lett., 2001,12,987. J.C. Pessoa, I. Correia, T. Kiss, T. Jakusch, M. Castro and C. Geraldes, J. Chem. Soc., Dalton Trans., 2002,4440. M.-H. Lee, Anal. Sci., 2001, 17, a235 C.S. Weinert, P.E. Fanwick and I.P. Rothwell, Organometallics, 2002,21,484. H. Brunner, J. Klankermayer and M. Zabel, Eur. J. Inorg. Chem., 202,2494. J.J. Cruywagen, A.G. Draaijer, J.B.B. Heyns and E.A. Rohwer, Inorg. Chim. Acta, 2002,331,322. P. Mialane, A. Dolbecq, L. Lisnard, A. Mallard, J. Marrot and F. Secheresse, Angew. Chem., Int. Ed. Engl., 2002,41,2398. A. Selling, I. Anderson, J.H. Grate and L. Pettersson, Eur. J. Inorg. Chem., 2002,743. F. Taube, M. Hashimoto, 1. Anderson and L. Petterson, J. Chem. Soc., Dalton Trans., 2002, 1002. F. Taube, 1. Anderson, I. Tbth, A. Bodor, 0.Howarth and L. Pettersson, J. Chem. Soc., Dalton Trans., 2002,4451. C.E. Easterly, D.M. Hercules and M. Houalla, Appl. Spectrosc., 2001,55, 1671.
I : N M R Spectroscopy in the L q i and Gas Phase iud
51
3.2.11 Tungsten. The formation of 1:l and 2:2 complexes of Ce"' with [P2w17061]10and their interaction with proline have been studied using 'H and 183W NMR The system NaH2P04-Na2W04-NaV03 during acidification has been studied by 31Pand 51V NMR NMR spectroscopy has been used to study the complexation of D-quinic acid with molybdate and t~ngstate.~" Li+/Na+ exchange in the cavity of N l [ N O 2 2 o ( z l 0 6 2 and N l [ N O 2 C 3 P W 5 5 ) ]has been a8(aH)C2PW55)] a7(aH)o(21062 demonstrated by 31P dynamic NMR spectro~copy.~'~ 51Vand 183W I7O, NMR spectroscopy has been applied to the quantitative determination of sodium dodecatungstosilicate ~peciation.~ Tungstate-phosphate aqueous solutions have been studied by 3'PNMR spectroscopy at various pH from 8.4 to 0.25.713 Protonation and solvation measured by electrospray-ionization time-of-flight mass spectrometry for phosphotungstate species differ from those observed by 31P NMR spectro~copy.~'~ formation of lanthanide complexes with [a-2The PZw17061]10-has been studied using '83W NMR titrati~n.~''
'
3.2.12 Manganese. The displacement of Mn2+from RNA by K + and Mg2+has been studied using 'H detected '*PNMR spectro~copy.~' 3.2.13 Rhenium. Variable temperature 'H EXSY NMR experiments have shown exchange between [Re3(p-H)4(CO)9(PPh3)] and [Re3{p-M(PPh3)}(p3-H)(p2H)3(CO),(PPh3)], M = Cu, Ag, A u . ~ 'Exchange as in Scheme 3 has been ~ demonstrated by variable temperature NMR spectro~copy.~' pH dependThe ence of ReVOcomplexes of N-mercaptoacet yl-glycylgly~ine,~' and S-trityl-Dpenicillamine-acetamide-(2-Me-2-propanethiol) ethyl has been studied by 'H NMR spectroscopy. 3.2.1 4 Iron. The equilibrium constant for phosphine exchange between [(q5C5H5)Fe(CO),(PPh3)] and P(2-f~ranyl)~ been determined by 31P has NMR
+
708
709
710
71
712 713
714 715
'16
717
718
719
720
M. Sadakane, A. Ostuni and M.T. Pope, J. Chem. SOC.,Dalton Trans., 2002,63. A.K. Akhmetova, K.T. Arynov, Z. Zhubatov and A.I. Raivich, Izv. Minist. Obraz. Nauki Resp. Kaz., Nuts. Akad. Nauk Resp. Kaz., Ser. Khim., 2001, 8. M.L. Ramos, M.M. Pereira, A.M. Beja, M.R. Silva, J.A. Paixao and V.M.S. Gil, J. Chem. SOC., Dalton Trans., 2002,2126. L. Ruhlmann, J. Canny, R. Contant and R. Thouvenot, Inorg. Chem., 2002,41,3811. B.J. Smith and V.A. Patrick, Aust. J . Chem., 2002,55,281. A.K. Akhmetova, Z. Zhubatov, K.T. Arynov, G.O. Nurgalieva and A.I. Raivich, Izv. Minist. Obraz. Nauki Resp. Kaz., Nuts. Akad. Nauk Resp. Kaz., Ser. Khim., 2001,74. C.E. Easterly, D.M. Hercules and M. Holuala, Appl. Spectrosc., 2001,55, 1665. Q.H. Luo, R.C. Howell, J. Bartis, M. Dankova, W.D. Horrocks, A.L. Rheingold and L.C. Francesconi, Inorg. Chem., 2002,41,6112. J.S. Summers, J. Shimko, F.L. Freedman, C.T. Badger and M. Sturgess, J. Am. Chem. SOC., 2002, 124,14 934. T. Beringhelli, G. D'Alfonso, M.G. Garavaglia, M. Panigati, P. Mercandelli and A. Sironi, Urganornetallics, 2002,21,2705. C.P. Casey, T.M. Boller, S.Kraft and LA. Guzei, J. Am. Chem. SOC.,2002,124,13 215. M. Lipowska, L. Hansen, X.L. Xu, P.A. Marzilli, A. Taylor, jun. and L.G. Marzilli, Inarg. Chem., 2002,41, 3032. M. Lipowska, L. Hansen, R. Cini, X.L. Xu, H. Choi, A.T. Taylor and L.G. Marzilli, Inorg. Chim. Acta, 2002,339, 327.
52
Ph
i
Scheme 3
Ph
s p e c t r o ~ c o p y .Anion binding to ferrocene-appended amido-pyrrole ~~ and calixC4larenes containing ferrocene a m i d e ~has been studied using 'H ,~~~ NMR titration. The cation dependence of electron transfer between [Fe(CN)6]3and [Fe(CN)6I4- has been investigated using 'H NMR spectroscopy.724 Ion pairing between the alkali metals and [Fe(CN)5(NO)]2- has been studied using I3C NMR spectroscopy.725'H and 13CNMR studies of the interaction between lauryl maltoside and cytochrome c oxidase have been reported.726The temperature dependence for water exchange in [Fe(nta)(OH2),]- has been investigated Ligand exchange kinetics for nitriles on a Fe"' using 1 0 7 TI nitrile hydratase model complex have been determined using I3C line-broadening analysis.728The interaction between Fe"' sidophores and membranes has been studied using NMR line broadening.729
3.2.1 5 Ruthenium and Osmium. The thermodynamic parameters for the equilibrium between [RuH(q4-1,5-CsHlz)(q6-anthracene)] [Ru(q ',q3-CsHI3)(q6and 9.10-dihydroanthracene)]+ have been determined.730A 'H NMR study of the interaction of the 5-HO-3-indolyl acetic acid and N-acetyltryptophan complexes of [(q6-p-cymene)Ru(acetone)3] with [Pd(dien)(0H2)l2+ has been The 7Li and I9FNMR spectra of LiFHF in the presence of (97), LM = ($-pcymene)Ru, (q5-C5H5)Rh, (q5-C5H5)Ir, show exchange in and out of the cavity. 'J(19F7Li)= 91 to 103 Hz.732Concentration dependent 'H NMR studies show aggregation of di- and tetra-nuclear Ru" and 0s" complexes of polypyridyl ligands by n-n The binding of A,A-[ { R~(4,4-Me~-bpy)~},(p-2,2'bipyrimidine)14+ ,734 and A-[ R~(2,9-Me~-phen)~(dipyrido-[3,2-a:2',3'-~] p h e n a ~ i n e ) ] ' + ,to~DNA bulge sites has been studied by 'H NMR spectro~ ~
721 722 723 724 725 726 727 728 729 730 731 732 733 734
O.G. Adeyemi and L.K. Liu, Bull. Chem. SOC.Ethiopia, 2001,15,23. G . Denuault, P.A. Gale, M.B. Hursthouse, M.E. Light and C.N. Warriner, New J. Chem., 2002, 26,811. B. Tomapatanaget and T. Tuntulani, Tetrahedron Lett., 2001,42,8105. A. Zahl, R. van Eldik and T.W. Swaddle, Inorg. Chem., 2002,41,757. G.A. Lawrance, M. Maeder, Y.M. Neuhold, K. Szacilowski,A. Barbieri and Z. Stasicka, J. Chem. SOC.,Dalton Trans., 2002, 3649. K. Chattopadhyay, T.K. Das, A. Majumdar and S. Mazumdar, J. Inorg. Biochem., 2002,91,116. T. Schneppensieper, A. Wanat, G. Stochel and R. van Eldik, Inorg. Chem., 2002,41,2565. J. Shearer, H.L. Jackson, D. Schweitzer, D.K. Rittenberg, T.M. Leavy, W. Kaminsky, R.C. Scarrow and J.A. Kovacs, J. Am. Chem. SOC.,2002,124,11417. G.F. Xu, J.S. Martinez, J.T. Groves and A. Butler, J . Am. Chem. SOC.,2002,124,13 408. M. Hirano, T. Shibasaki, S. Komiya and M.A. Bennett, Organometallics, 2002,21, 5738. A. Schluter, K. Bieber and W.S. Sheldrick, Inorg. Chim. Acta, 2002,340, 35. M.-L. Lehaire, R. Scopelliti and K. Severin, Inorg. Chem.,2002,41,5466. A.K. Bilakhiya, B. Tyagi, P. Paul and P. Natarajan, Inorg. Chem., 2002,41,3830. B.T. Patterson, J.G. Collins, F.M. Foley and F.R. Keene, J. Chem. SOC.,Dalton Trans., 2002,4343.
53
scopy, including NOE measurements. The equilibrium constant for the aquation of [Ru(bpy)2{ PPh2(C6H4-2-OMe))l2+ been determined by NMR spectrohas s c ~ p yThe dimerisation of [M(bpy)2(eilatin)]2+, = Ru, Os, by n-nstacking . ~ ~ ~ M Extensive use has been made of has been studied by 'H NMR 'H NMR spectroscopy to study the coordination of 9-Me-adenine to cis[Ru(bpy)Kl2: and a-[R~(azpy)z(N03)2].~ [HB(pz)3{ P(OMe)3}2NHC6H4-]? exists as two isomers which interconvert at high temperature.739 'H NMR spectroscopy has been used to study the binding of Ru" to b l e ~ m y c i n . ~ ~ ' Pyridine exchange reactions on [ R U ~ ( ~ - O ) ( ~ - O ~ C M ~ ) ~ ( N Cbeen ~ ) ~ ] ~ have ~ H investigated using 'H NMR
+
3.2.16 Cobalt. 'H NMR spectroscopy has been used to study the equilibrium in 'H Scheme 4.742 NMR spectroscopy has been used to examine the equilibrium between (98) and [02P(OMe)2]-.743EXSY has been used to study ligand ex.744 +, change on [Co(dipic~linate)~]~- The binding of [C~(his)~] [Co(en),(C20,)l + and [K( 18-crown-6)][SCN] with the tetrasodium salt of tetrakis(su1fonatomethyl)calix[4]resorcinarene has been studied in neutral and alkaline aqueous media by NMR
[HCo(dppe)2(NCMe)12+ MeOC6H4NH2~[Co(dppe)2]+ [MeOC6H4NH3] + MeCN +

Scheme 4
735
736
737
738
739
740
741
742
743
744
745
A. Greguric, I.D. Greguric, T.W. Hambley, J.R. Aldrich-Wright and J.G. Collins, J. Chem. SOC., Dalton Trans., 2002,849. C.W. Rogers, Y. Zhang, B.O. Patrick, W.E. Jones and M.O. Wolf, Inorg. Chem., 2002,41, 1162. D. Gut, A. Rudi, J. Kopilov, 1. Goldberg and M. Kol, J. Am. Chem. SOC.,2002,124,5449. A.C.G. Hotze, M.E.T. Broekhuisen, A.H. Velders, K. van der Schilden, J.G. Haasnoot and J. Reedijk, Eur. J. Inorg. Chem., 2002,369. D. Conner, K.N. Jayaprakash, T.B. Gunnoe and P.D. Boyle, Organometallics, 2002,21,5265. B. Mouzopoulou, H. Kozlowski, N. Katsaros and A. Garnier-Suillerot, Inorg. Chem., 2002,40, 6923. M. Abe, A. Mitani, A. Ohsawa, M. Herai, M. Tanaka and Y. Sasaki, Inorg. Chim. Acta, 2002,331, 158. R. Ciancanelli, B.C. Noll, D.L. DuBois and M.R. DuBois, J . Am. Chem. SOC.,2002,124,2984. J. Chin, S. Chung and D.H. Kim, J. Am. Chem. SOC., 2002,124,lO 948. L.Q. Yang, D.C. Crans, S.M. Miller, A. la Cour, O.P. Anderson, P.M. Kaszynski, M.E. Godzala, L.D. Austin and G.R. Willsky, Inorg. Chem., 2002,41,4859. A.R. Mustafina, V.V. Skripacheva, E.K. Kazakova, N.A. Markarova, V.E. Kataev, L.V. Ermolaeva and W.D. Habicher, J. Inclusion Phenom. Macrocyclic Chem., 2002,42,77.
54
(98)
3.2.17 Rhodium and Iridium. 'H and 31PNMR spectroscopy has been used to determine ApK, values between [IrH5(PPri3)2] [IrHs(PCy3)2].746 NMR and 'H spectroscopy has been used to study the titration of [(q5-CsMe5)Ir(p.-H)31r(q5C5Me5)] with water.747Variable temperature NMR spectroscopy has been used to study the equilibrium in Scheme 5.748 The 'H NMR spectra of cis[M(CO)fCl(pyrazine)] show fast and reversible dissociation of the p y r a ~ i n e . ~ ~ ~ 'H and 31PNMR spectroscopy has been used to study oxidised carbon nanotubes reacting with Wilkinson's catalyst.750Exchange between isomers of phosphinooxazoline complexes of Rh"' and Ir"' has been investigated using 'H and 31P NMR s p e c t r o s ~ o p yThe forms of Rh"' in nitric acid solutions have .~~~ NMR spectroscopy.752 been studied by I4N,15N,''0 and lo3Rh
+
(q4-cod)Rh
< CI PPh,
I
MePbP, I-
Scheme 5
3.2.18 Nickel. NMR titration has been used to study the binding of dicarboxylic acids to a 15-membered Ni" macrocyclic cyclidene with two cyclen recognition sites.753The binding of Ni2+ to terminally blocked hexapeptides has been investigated by NMR spectroscopy.754 3.2.1 9 Palladium and Platinum. The equilibrium in Scheme 6 has been studied by NMR spectro~copy.~~ dynamic equilibrium between isomers of [Pd(q3A
746
747 748
749
7s0
7s1 7s2
7s3
7s4
S.E. Landau, K.E. Groh, A.J. Lough and R.H. Morris, Inorg. Chem., 2002,41,2995. S. Ogo, H. Nakai and Y. Watanabe, J. Am. Chem. Soc., 2002,124,597. L. Viau and R. Chauvin, J. Organomet. Chem., 2002,654,180. C. Dragonetti, M. Pizzotti, D. Roberto and S. Galli, Inorg. Chim. Acta, 2002,330, 128. S. Banerjee and S.S. Wong, J. Am. Chem. Soc., 2002,124,8940. D. Carmona, F.J. Lahoz, S. Elipe, L.A. Oro, P. Lamata, F. Viguri, F. Sanchez, S. Martinez, C. Caliviela and M.P. Lopez-Ramde Viu, Organometallics, 2002,21,5100. A.V. Belyaev, M.A. Fedotov, S.P. Khranenko and V.A. Emel'yanov, Russ. J. Coord. Chem., 2001, 27,855; M.A. Fedotov, Russ. J. Coord. Chem., 2002,28,573. O.P. Kryatova, A.G. Kolchinski and E.V. Rybak-Akimova, J. Inclusion Phenom. Macrocyclic Chem., 2002,42,25 1. M. Mylonas, A. Krezel, J.C. Plakatouras, N. Hadjiliadis and W. Bal, J. Chem. SOC.,Dalton Trans., 2002,4296.
I: N M R Spectroscopy in the Liquid and Gus Phuse
55
PhCHCHCHPh)(phosphino-oxazoline)]+ has been investigated by 'H and I3C NMR Kinetic studies of [CNl- exchange on [M(CN)4]2-, M = Pd, Pt, have been performed as a function of pH by I3C NMR spectroscopy.
R'
R'
l4
Scheme 6
'H NMR spectroscopy has been used to study the addition of [(en)Pd(ON02)2] a facial amphiphile to give a 2:2 complex.7s8The interaction to of amine complexes of Pd and Pt with purine nucleosides has been studied by NMR s p e c t r o s c ~ p y . ' Cis-trans isomerism of [CSH3N-2,6-(CH2NHC6H4-4~~ R),PdCl] + has been investigated using line-shape analysis.760Anion binding to [{ Pd(B~~-bpy))~(p-pyrimidone)]~ been studied by ' H NMR t i t r a t i ~ n . ~ ~ ' has The temperature dependence of the 'H NMR spectra of [Pd(ONMe = NNC6H32,5-Me2)?] show cis-trans isomerism.762' H NMR spectroscopy has been used to study the trimer/tetramer equilibrium of [M(dppp)12 with NCsH4-4-N= N-4+ C5H4N. 6 7 The hydrolysis profile of [{ tran~-PtCl(NH~)~}~{ p-transPt(NH3)2[NHl(CH2)6NH2]2}]4+ been examined using 'H,15N HSQC NMR has s p e c t r o ~ c o p y . ''H~NMR spectroscopy has been used to study the pH stability ~ of [Pt2(NH~)~(C4H~,N0)2(Cl~H1~N504)(S0~)J2 . 7 6 s '95PtNMR spectroscopy has been used to study the reactions of [Pt(dien)Cl]+ with sulfur donors.766Linkage isomerism of cytosine with [Pt(NH2Me)lL2]' has been investigated by 'H and Ig5Pt NMR The binding behaviour of (aminoethano1)dichloroplatinum complexes to 5'-GMP and DNA has been investigated by 'H
+
75s
'" P. Dotta, P.G.A. Kumar and P.S. Pregosin. M a g n . Rrson. Chem., 2002,40,653.
757 7s8
7'9
L. Canovese. F. Visentin, G. Chessa, C. Santo. P. Uguagliati, L. Maini and M. Polito, J . Chem. Soc., Dalton Trans., 2002, 3696.
F.J. Monlien, L. Helm, A. Abou-Hamdan and A.E. Merbach, Inorg. Chern., 2002,41, 1717. L. Isaacs and D. Witt, Angew. Chem., Int. Ed. Engl., 2002,41, 1905. W. Wirth. J. Blotevogel-Baltronat, U. Kleinkes and W.S. Sheldrick, Inorg. Chim. Acta, 2002,339,
14.
760
7h'
762
763
764
A. Arniiz, J.V. C'uevas. G. Garcia-Herbosa, A. C'arbayo. J.A. Casares and E. Gutierrez-Puebla,J. Chem. Sot.., Dalton Trans., 2002,2581. Z.Q. Qin, M.C. Jennings and R.J. Puddephatt, Inorg. Chem., 2002.41, 3967. Z. Ciunik, J.A. Wolny. M.F. Rudolf and S. Wolowiec, J . Chem. Soc., Dalton Trans., 2002, 885. C.A. Schalley, T. Muller, P. Linnartz, M. Witt, M. Schafer and A. Lutzen, Chem.-Eur. J.,2002,8, 3538. M.S. Davies, D.S. Thomas, A. Hegmans, S.J. Berners-Price and N. Farrell, Inorg. Chem., 2002,
41, 1101.
76s
766 767
K. Ito, R. Somazawa, J. Matsunami and K. Matsumoto, Inorg. Chim. Acta, 2002,339,292. K. Lemma, S.K.C.Elmroth and L.I. Elding, J . Chem. Soc., Dalton Trans., 2002, 1281. W. Bruning, E. Freisinger, M . Sabat, R.K.O. Sigel and B. Lippert, Chem.-Eur. J., 2002,8,4681.
56
NMR The hydrolysis reactions of [Pt(NC5H4R)2(N03)2] have been studied using 'H, I3Cand '95PtNMR spectroscopy.769The binding of Na+ to Pt" terpyridyl complexes containing crown ether pendants has been probed by 'H NMR spectroscopy.770 The pK, value for a platinum complex of 9ethylguanine has been investigated by 'H, I3C and 195Pt NMR The hydrolysis and redox processes of a hydrosoluble Pd"-diphosphine system has been studied by 31PNMR spectroscopy.772Halogen scrambling reaction of [PtC13{P(C6H4-4-Me)3}]-on addition of Br- has been studied by 31PNMR spectroscopy. The liquid-liquid extraction of Pt"/Pt'" from hydrochloric acid by N-acyl-N',N'-dialkylthioureas has been studied by 'H, I3C and 195Pt NMR spectroscopy.774 3.2.20 Copper. 'H NMR spectroscopy has been used to study Cu2+coordination to a pentade~apeptide.~~' binding to a monomeric prion has been invesCu2+ tigated by 'H and 13CNMR spectroscopy.776The effects of temperature and pressure on the water exchange of [CU{(NC~H~-~-CH~)~N)(OH~)]~+ have been 19F studied using 1 7 0 NMR spectroscopy.777 NMR spectroscopy has been used to monitor the titration of (99) with acid or base.778The structure and dynamics of the lincomycin-copper(I1)complex in water have been studied by 'H and 13C NMR spectroscopy.779'H NMR spectroscopy has been used to study the pH dependent Cu+ and Cu2+release from p s e u d o a z ~ r i nI7O~ ~ , ~ NMR spectroscopy has been used to determine the rate of water exchange on [Cu(terpy)(OH2)2]2+.781 binding of Cu2+ to (100) has been investigated by NMR The spectroscopy.782 The kinetics of electron self-exchange reactions in the [ C U ( S ~ C N E ~ ~system have been determined by NMR l i n e - b r ~ a d e n i n g . ~ ~ ~ )~]/I~
768 769
I10
771 772 773 774 775 716 771 778 719 180 781 182
M.S. Robillard, M. Galanski, W. Zimmermann, B.K. Keppler and J. Reedijk, J. Inorg. Biochem., 2002,88,254. F.D. Rochon and C. Tessier, Can. J. Chem., 2002,80, 379. V.W.-W. Yam, R.P.-L. Tang, K.M.-C. Wong, X.-X. Lu, K.-K. Cheung and N.-Y. Zhu, Chem.Eur. J.,2002,8,4066. X. Riera, V. Moreno, E. Freisinger and B. Lippert, Inorg. Chim. Acta, 2002,339,253. F. Janin, E.G. Kuntz, J.B. Tommasino and O.M. Vittori, J. Mol. Catal. A: Chem., 2002,188,71. S.J. Sabounchei and V. Jodaien, J. Chem. Res., Synop., 2002, 112. K.R. Koch, J. Miller and A.N. Westra, International Solvent Extraction Conference, Cape Town, South Africa, Mar. 17-21,2002,2002,327. C . Conato, W. Kamysz, H. Kozlowski, M. Luczkowski, 2. Mackiewicz, P. Mlynarz, M. Remelli, Dalton Trans., 2002, 3939. D. Valensin and G. Valensin, J. Chem. SOC., M. Luczkowski, H. Kozlowski, M. Stawikowski, K. Rolka, E. Gaggelli, D. Valensin and G. Valensin, J. Chem. SOC.,Dalton Trans., 2002,2269. A. Neubrand, F. Thaler, M. Korner, A. Zahl, C.D. Hubbard and R. van Eldik, J. Chem. SOC., Dalton Trans., 2002,957. C . Belle, C. Beguin, I. Gautier-Luneau, S. Hamman, C. Philouze, J.L. Pierre, F. Thomas and S. Torelli, Znorg. Chem., 2002,41,479. E. Gaggelli, N. Gaggelli, D. Valensin, G. Valensin, M. Jeiowska-Bojczuk and H. Kozowski, Znorg. Chem., 2002,41,1518. K. Sato, S. Nagatomo, C. Dennison, T. Niizeki, T. Kitagawa and T. Kohzuma, Inorg. Chim. Acta, 2002,339,383. G.U. Priimov, P. Moore, L. Helm and A.E. Merbach, Znorg. React. Mech. (Amsterdam, Neth.), 2001,3, 1. R. Tanaka, T. Yano, T. Nishioka, K. Nakajo, B.K. Breedlove, K. Kimura, I. Kinoshita and K. Isobe, Chem. Commun., 2002,1686.
57
13+
3.2.21 Silver. NMR titration results indicate that there are Ag+-n interactions in Ag+ complexes of N-ally1 and N-butenyl lariat ethers.784'H NMR spectroscopy has been used to investigate the titration of Ag+ with (101).785 NMR titration 'H has been used to follow the formation of triangular and tetrahedral array of Ag+ by (102).786The tumbling volume of some [Ag{ 1,8-(CN)2-p-menthane}2]flfl+ The interaccomplexes has been estimated from 13CNMR T I tion of Ag+ with trilinked N2S2-donormacrocycles has been investigated by 'H NMR t i t r a t i ~ nThe ~ ~ . ~ coordination of Ag+ with Ph2PNRPPh2has been invesNMR spectroscopy.789 The variable coordination modes of tigated by 31P [NO2]- in a series of Ag' complexes of ER3,E = P, As, Sb, have been studied by 'H and 31P NMR The coordination of P(2-f~ryl)~ Ag+ has to been studied by 31PNMR spectroscopy.791 A 31PNMR titration of 1,3(PhCH20)2-5-( -03SOCH2)C6H3 with AgSbF6-triphosphine has been reported.792 The affinity of p-But-dihomooxacalix[4]arene and p-But-calix[4] arene for Ag+ has been investigated by 'H NMR spectroscopy.79331P NMR spectroscopy has been used to investigate the addition of a thiophosphorylated cavitand with Ag p i ~ r a t e . ~ ~ ~ 3.2.22 Gold. The self-assembly of Au' rings from [ ( A u C = C C H ~ O C ~ H ~ ) ~ C M ~ ~ ] with diphosphane ligands has been studied by NMR spectroscopy.795The
783
784 785
786
787
788
789
790
791
792
793
794
V.G. Shtyrlin, A.V. Zakharov, A.M. Kuznetsov, O.V. Kukushkina and P.P. Chernov, Eur. J. Inorg. Chem., 2002,2947. P. Arya, A. Channa, P.J. Cragg, P.D. Prince and J.W. Steed, New J . Chem., 2002,26,440. A. Marquis, J.P. Kintzinger, R. Graff, P.N.W. Baxter and J.M. Lehn, Angew. Chem., Int. Ed. Engl., 2002,41,2760. S. Hiraoka, T. Yi, M. Shiro and M. Shionoya, J. Am. Chem. SOC.,2002,124,14 510. M. Turcotte and P.D. Harvey, Inorg. Chem., 2002,41,2971. J.D. Chartres, A.M. Groth, L.F. Lindoy and G.V. Meehan, J. Chem. SOC.,Dalton Trans., 2002, 371. E.J. Sekabunga, M.L. Smith, T.R. Webb and W.E. Hill, Inorg. Chem., 2002,41,1205. A. Cingolani, Effendy, M. Pellei, C. Pettinari, C. Santini, B.W. Skelton and A.H. White, Inorg. Chem., 2002,41,6633. F. Bachechi, A. Burini, R. Galassi, B.R. Pietroni and D. Tesei, Eur. J. Inorg. Chem., 2002,2086. X.L. Xu, E.J. MacLean, S.J. Teat, M. Nieuwenhuyzen, M. Chambers and S.L. James, Chem. Commun., 2002, 78. P.M. Marcos, J.R. Ascenso, M.A.P. Segurado and J.L.C. Pereira, J. Inclusion Phenom. Macrocyclic Chem., 2002,42,281. B. Bibal, B. Tinant, J.P. Declercq and J.P. Dutasta, Chem. Commun., 2002,432.
58
(101)
(102)
kinetics of [CN]- exchange on [Au(CN)J have been investigated using I3C NMR spectroscopy.796Scrambling reactions of cyano(se1enone)Au' complexes have been investigated using I3Cand "N NMR spectroscopy.797The interaction of thiurea with aurofin and [Et3PAuCl] has been studied using I3C, 15Nand 31P NMR spectroscopy.798 3.2.23 Zinc. The encapsulation of lipophilic organic molecules in a cubo-octahdral supramolecular capsule by a 4:4 self-assembly of tris(Zn"-cyclen) and trianionic trithiocyanurate has been followed by 'H NMR spectroscopy.799'H and I3CNMR spectroscopy has been used to study the binding of Zn2+and Pb2+to four edta-derived macrocycles containing an ether moiety.800 Zn2+coordination to a tripodal imidazole has been investigated by 'H NMR spectroscopy.801'H NMR spectroscopy has been used to study a titration of Zn2+with (103).802 I3C NMR spectroscopy has been used to show that I3CO2exchanges with carbamate in some tetrazine carbamato complexes.803
3.2.24 Cadmium. Temperature dependent '13Cd NMR studies have established that there is little difference in the binding abilities of epoxide adducts of cadmium p h e n ~ x i d e s . ~ ' ~ binding constants for the inclusion of some aroThe matic anions in [Cd{ (S)-1,4,7,10-[(S)-PhOCH2CH(OH)CH2]41,4,7,10-tetraazacyclododecane}]2+have been measured by 'H NMR titrati~n.~" "N and 'H,
795 796 797 798 799 800
801
802
803
8 04
805
C.P. McArdle, M.J. Irwin, M.C. Jennings, J.J. Vittal and R.J. Puddephatt, Chem.-Eur.J., 2002,8, 723. F.J. Monlien, L. Helm, A. Abou-Hamdan and A.E. Merbach, Inorg. Chim. Acta, 2002,331,257. S . Ahmad, A.A. Isab, A.R. Al-Arfaj and A.P. Arnold, Polyhedron, 2002,21,2099. S. Ahmad and A.A. Isab, J. Inorg. Biochem., 2002,88,44. S . Aoki, M. Shiro and E. Kimura, Chem.-Eur.J.,2002,8,929. R. Delgado, M.D. Cabral, R. Castanheira, A.J. Zhang and R. Herrmann, Polyhedron, 2002,21, 2265. A. Jansco, I. Torok, L. Korecz, A. Rockenbauer and T. Gajda, J . Chem.SOC.,Dalton Trans., 2002, 2601. R. Dobrawa and F. Wurthner, Chem. Commun., 2002,1878. C.S. McCowan, T.L. Groy and M.T. Caudle, Inorg. Chem., 2002,41,1120. D.J. Darensbourg, J.R. Wildeson, S.J. Lewis and J.C. Yarbrough, J . Am. Chem. Soc., 2002,124, 7075. C.B. Smith, A.K.W. Stephens, K.S. Wailwork, S.F. Lincoln, M.R. Taylor and K.P. Wainwright, Znorg. Chem., 2002,41,1093.
59
P 4
Ar Ar
Bn*0 uN o
0 0 Ar Ar
"P NMR spectroscopy has been used to study Cd2+binding to ATP.806The coordination of Cd2+to the phosphoryl cleavage site of a hammerhead ribozyme has been reappraised, based on 31P NMR data.807
3.2.25 Mercury. A 'H NMR titration of Hg2+with (6-MeC5H3-2-CH2)3N has been reported. Extensive 'H-'99Hgcoupling was observed.808Variable temperature 13C{ NMR measurements have been carried out on the Hg2+complex of 'H} 1,4,7-trithiacyclodecaneand suggests rapid ligand exchange. The 13Cd NMR spectrum of the cadmium analogue was reported.809
'
3.2.26 Boron. The equilibrium between cations inside and outside the [M12H12I2- has been investigated.810The influence of the solvent on the 19F chemical shift of the [BF4]- ion has been reported.811 3.2.27 Aluminium.Monomer-trimer equilibrium constants for [BuizA1(N3)] have NMR spectroscopy has been determined using 27AlNMR spectroscopy.8 27Al been used to study Al"' chelates of triazacyclononane polycarboxylate NMR spectroscopy has been used to investigate complex l i g a n d ~ . ~ ' ~ 31P 'H and formation between A13 with iminodiacetic acid.8l4 The interaction of 3,4-hydroxypyridinecarboxylic acids with A13+ has been investigated by 'H NMR spectroscopy.81 The composition distribution of different kinds of aluminium salt aqueous solutions at different pH values has been investigated by 27AlNMR
+
806
807
808
809
810
811
812
813
814
815
L. Jiang and X.-A. Mao, Gaodeng Xuexiao Huaxue Xuebao, 2002,23,763. K. Suzumura, K. Yoshinari, Y. Tanaka, Y. Takagi, Y. Kasai, M. Warashina, T. Kuwabara, M. Orita and K. Taira, J. Am. Chem. Soc., 2002,124,8230. D.C. Bebout, J.F. Bush, K.K. Crahan and E.V. Bowers, Inorg. Chem., 2002,41,2529. M.L. Helm, C.M. Combs, D.G. VanDerveer and G.J. Grant, Inorg. Chim. Acta, 2002,338,182. O.P. Charkin, N.M. Klimenko, D. Moran, A.M. Mebel, D.O. Charkin and P.v.R. Schleyer, J . Phys. Chem., A, 2002,106,ll 594. V.N. Plakhotnyk, R.Schmutzler, L. Ernst, Y.V. Kovtun and A.V. Plakhotnyk, J . Fluorine Chem., 2002,116,41. 2.-h. Zhang and 2.-X- Gao, Wuji Huaxue Xuebao, 2001,17,819. J.P. Andre, H. Macke, A. Kaspar, B. Kunnecke, M. Zehnder and L. Macko, J. Inorg. Biochem., 2002,88, 1. M . Kilyen, A. Lakatos, R.Latajka, A. Labadi, A. Salifoglou, C.P. Raptopoulou, H. Kozlowski and T. Kiss, J. Chem. SOC.,Dalton Trans., 2002,3578. V.B. Di Marco, R.A. Yokel, M.G. Ferlin, A. Tapparo and G.G. Bornbi, Eur. J . Inorg. Chem., 2002,2648.
60
spectroscopy.816 and I3CNMR spectroscopy has been used to study alumin'H ium coordination in aqueous A13+-citratecomplexes.817The rates of solvent exchange in aqueous All1'-maltolatecomplexes have been determined by I7Oand 27AlNMR spectroscopy.818The influence of All1' on the mechanism of watersilicate melt interaction has been studied by 'H NMR spectroscopy.819The distribution of Na+ coordination in sodium silicate glass at water dissolution has been determined by NMR spectroscopy.820The kinetics of oxygen exchange between [Ge04A112(0H)24(OH2)12]8+ aqueous solutions have been studied and NMR spectroscopy has using I7ONMR spectroscopy.82 I7O,I9F,23Naand 27Al been used to study the structure of high-temperature NaF-A1F3-Al2O3 melts.822
3.2.28 Gallium. 71Ga NMR spectroscopy has been used to study Gall' hydration in aqueous solution.823 3.2.29 Silicon and Germanium. Ionic dissociation of hexacoordinate silicon complexes to pentacoordinate siliconium salts has been investigated by 29SiNMR spectroscopy, see Scheme 7.824 Host-guest chemistry between silicon-bridged calix[6]pyrrole and anions such as halides, [H2P04]-, [HS04]-, [NO,]- and [CN]- has been investigated by 'H NMR t i t r a t i ~ n .The ~ ~ ~ stability of [M(O4C2),l2-,M = Si, Ge, in solution has been investigated by 'H, I3Cand 29Si NMR spectroscopy.
Ap,.r:
Scheme 7
,Si-Ph
Me*
+CI-
3.2.30 Tin. A 'H NMR titration has been used to study the complex formation between [Me2Sn12+ and malic 1 0 7 and '19Sn NMR spectroscopy has
'16
817
818
'9 1
820
821 822
823
824
825
826
K. Ding, J. Liu, L. Zhao and T. Zhang, Zhongguo Pige, 2002,31, 6; J.W. Phair and J.S.J. van Deventer, Ind. Eng. Chem. Res., 2002,41,4242. A. Bodor, I. Banyai and I. Toth, Coord. Chem. Rev., 2002,228,175. P. Yu, B.L. Phillips, M.M. Olmstead and W.H. Casey, J. Chem. SOC.,Dalton Trans., 2002,2119. V.O. Zavel'skii and T.P. Salova, Geokhimiya, 2002,781. A.G. Simakin, T.P. Salova, M. Romero and J.M. Rincon, Materiales de Construccion (Madrid, Spain), 2001,51,209. A.P. Lee, B.L. Phillips and W.H. Casey, Geochim. Cosmochim. Acta, 2002,66,577. V. Lacassagne, C. Bessada, P. Florian, S. Bouvet, B. Ollivier, J.P. Coutures and D. Massiot, J. Phys. Chem. B, 2002,106,1862. W.W. Rudolph and C.C. Pye, Phys. Chem. Chem. Phys., 2002,4,4319. D. Kost, V. Kingston, B. Gostevskii, A. Ellern, D. Stalke, B. Walfort and I. Kalikhman, Organometallics, 2002, 21, 2293; I. Kalikhman, V. Kingston, B. Gostevskii, V. Pestunovich, D. Stalke, B. Walfort and A. Kost, Organometallics, 2002,21,4468. G. Cafeo, F.H. Kohnke, G.L. La Torre, M.F. Parisi, R.P. Nascone, A.J.P. White and D.J. Williams, Chem.-Eur. J., 2002,8, 3148. 0.Seiler, C. Burschka, M. Penka and R. Tacke, Z. Anorg. Allg. Chem., 2002,628,2427.
61
been used to study the Rb2Sn(OH)6-H20-H202-Rb2Sn(OOH)6 system.82' The interaction of Sn"and Sb"' fluorides with phosphorus chlorides has been studied by 19F,31P II9Sn NMR spectro~copy.'~~ and 3.2.31 Lead. The structural features of complexes of Pb" with a tetraiminodiphenol macrocyclic ligand have been investigated by 'H NMR spectroscopy.' 30 Two-dimensional 207Pb NMR spectroscopy has been used to study ligand exchange between Pb2 and l-Pri-3-Me-benzylaldimino-5-selenopyrazolate.
+
3.2.32 Nitrogen. The 1yot ropic system, cetyl trimet hylammonium bromide-H20, The has been studied by 2H, 14N and 1 7 0 NMR spectro~copy.'~~ molecular dynamics of poly(N-diallyldimethylammonium chloride) have been studied using 'H and 35Cl NMR ~pectroscopy.'~~ effect of the anion on the chemical The shifts of the aromatic hydrogen atoms of liquid l-Bun-3-Me-imidazolium salts has been reported. 34
'
3.2.33 Antimony. 19FNMR studies of the conjugate Br-nsted-Lewis superacid HS03F-SbF5,'35 and Sb"' fluoride complexes in solution,'36 have been reported. 3.2.34 Bismuth. The interactions of Bi"' with human lactoferrin have been investigated by 13CNMR spectroscopy.837 3.2.35 Selenium and Tellurium. NMR investigations of the reaction equilibrium ~~ involving CCl3CC1= CC12 and E2C12, E = Se, Te, have been r e p ~ r t e d . ' 77Se NMR spectroscopy has been used to show the equilibrium in Scheme 8 and 31P NMR spectroscopy for the equilibrium in Scheme 9.839 3.2.36 Xenon. A I9F-I9F EXSY NMR study of F- exchange with [XeF2] has been published.840
827
828
829
830 831
832
833
834
83s
836
837
838
839
K. Gajda-Schrantz, L. Nagy, T. Fiore, L. Pellerito and T. Gajda, J. Chem. SOC.,Dalton Trans., 2002, 152. P.V. Prikhodchenko, V.I. Privalov, T.A. Tripol'skaya and E.G. Ippolitov, Doklady Akademii Nauk, 2001,381,351; P.V. Prikhodchenko, V.I. Privalov, T.A. Tripol'skaya and E.G. Ippolitov, Zh. Neorg. Khim., 2001,46,2060. Y.V. Kokunov, M.M. Ershova and G.A. Razgonyaeva, Russ. J. Coord. Chem., 2002,28,461. B. Dutta, B. Adhikary, P. Bag, U. Florke and K. Nag, J. Chem. SOC.,Dalton Trans., 2002,2760. Y.E. Chernysh, G.S. Borodkin, M.S. Korobov, B.S. Luk'yanov, N.V. Stankevich, I.G. Borodkina, V.Y. Vdovichenko and Y.M. Korobov, Russ. J. Coord. Chem., 2002,28, 170. F. Asaro, L. Liguori and G. Pellizer, Croat. Chem. Acta, 2001,74,877. J. Kriz, J. Dybal and D. Kurkova, J . Phys. Chem. A , 2002,106,7971. A.D. Headley and N.M. Jackson, J. Phys. Org. Chem.,2002,15,52. J. Kuhn-Velten, M. Bodenbinder, R. Brochler, G. Hagele and F. Aubke, Can. J. Chem., 2002,80, 1265. E.V. Kovaleva, L.A. Zemnukhova and V.V. Kon'shin, Russ. J. Coord. Chem., 2002,28,758. L. Zhang, K.Y. Szeto, W.B. Wong, T.T. Loh, P.J. Sadler and H. Sun, Biochemistry, 200440, 13 281. J. Beck, A. Hormel and M. Koch, Eur. J. Inorg. Chem.,2002,2271. H.J. Reich, M.J. Bevan, B.0. Gudmundsson and C.L. Puckett, Angew. Chem., Int. Ed. Engl., 2002,41, 3436.
62
Scheme 9
3.3 Equilibria among Uncharged Species. - 3.3.1 Lithium. 'H and 6Li NMR spectroscopy has been used to study the formation of aggregates between alkyllithium and chiral lithium amide~.'~' EXSY has been used to study LiI interaction as in Scheme Mixtures of [Mg(OCH2CH20Et)2] and of [LiOCH2CH20Et] with [Bu2Mg] have been studied by 'H, I3C and 7Li NMR spectroscopy and 'H6Li HOESY.843The role of 'ate' complexes in the lithiumsulfur, lithium-selenium and lithium-tellurium exchange reactions has been investigated using 13CNMR ~pectroscopy.'~~
+ Lil
Scheme 10
3.3.2 Strontium and Barium. Variable temperature 31P NMR spectra of [(THF),Sr{PR(C6H4-2-CH2NMe2)}2] show a monomer-dimer e q u i l i b r i ~ m . ' ~ ~ Variable temperature 19F NMR studies of [M{ OC(CF3)2CH*(OCH2CH2)20Me}2]and [M{ OC(CF3)2CH20CH2CH2N(CH2CH20Me)2}], = Sr, M Ba, show the presence of two isomers.846 3.3.3 Scandium and Yttrium. The dissociation constant and dissociation rate of [(q5-C5Me5)2YH]2 been measured by NMR line-broadening technique^.'^^ have
840
841
842
843
844
845
846
847
N. Vasdev, B.E. Pointner, R. Chirakal and G.J. Schrobilgen, J. Am. Chem. Soc., 2002,124,12 863. A. Corruble, D. Davoust, S. Desjardins, C. Fressigne, C. Giessner-Prettre, A. Harrison-Marchand, H. Houte, M.-C. Lasne, J. Maddaluno, H. Oulyadi and J.-Y. Valnot, J. Am. Chem. Soc., 2002,124,15 267. S.H. Bertz, C.M. Carlin, D.A. Deadwyler, M.D. Murphy, C.A. Ogle and P.H. Seagle, J. Am. Chem. Soc., 2002,124,13 650. M. Micha-Screttas, C.G. Screttas, B.R. Steele and G.A. Heropoulos, Tetrahedron Lett., 2002,43, 4871. H.J. Reich, B.O. Gudmundsson, D.P. Green, M.J. Bevan and I.L. Reich, Helv. Chim. Acta, 2002, 85, 3748. S. Blair, K. Izod and W. Clegg, Znorg. Chem., 2002,41,3886. Y. Chi, S. Ranjan, P.W. Chung, H.Y. Hsieh, S.M. Peng and G.H. Lee, Znorg. Chirn. Acta, 2002, 334,172. C.P. Casey, J.A. Tunge, T.Y. Lee and D.W. Carpenetti, Organornetallics, 2002,21,389.
63
The variable temperature 13C NMR spectra of (104), M = Sc, Y, show exundergoes change.848'H NMR spectroscopy indicates that [ ( v ~ - C ~ M ~ ~ ) ~ Y C ~ ( L ) ] ligand exchange.849
/
But
=N
,Pi
3.3.4 Ytterbium. Variable temperature 19F NMR spectroscopy shows that [Yb{ 2,6-(CsH4NCH2)2CsH3N)(p-O2SOCFJJ2 exchanges between two
3.3.5 Lutetium. Solvent exchange on [(q5:q5-C24H16)LuI(THF)] been inveshas tigated by 'H NMR spectroscopy.851
3.3.6 Titanium. The activation parameters for ligand exchange dynamics in lineshape analysis.852 cis-[TiF4L2] have been determined from 19F 3.3.7 Zirconium. The interaction of [ZrCh] with [Et6A12]has been studied by 'H and 27AlNMR spectroscopy.853The variable temperature 'H NMR spectroscopy of (105) shows exchange between two isomers.854
848 849
D.J.H. Emslie, W.E. Piers, M. Parvez and R. McDonald, Organornetallics, 2002,21,4226. W.J. Evans, C.H. Fujimoto, M.A. Johnston and J.W. Ziller, Organometallics, 2002,21, 1825. G. Paolucci, J. Zanon, V. Lucchini, W.-E. Damrau, E. Siebel and R.D. Fischer, Organornetallics,
2002,21, 1088.
851
852
853
854
I.L. Fedushkin, Y.A. Kurskii, V.I. Nevodchikov, M.N. Bochkarev, S. Muechle and H. Schumann, Russ. Chern. Bull., 2002,51, 160. G.B. Nikiforov, S.G. Sakharov, E.G. Il'in and Y.A. Buslaev, Zh. Neorg. Khim., 2001,46,1164. Y . Shiraki, Y. Nakamoto and Y.Souma, J . Mol. Catal. A: Chem., 2002,187,283. T. Toupance, S.R. Dubberley, N.H. Rees, B.R. Tyrrell and P. Mountford, Organornetallics,2002,
21, 1367.
64
3.3.8 Molybdenum. The variable temperature NMR spectra of (106) show a coordination equilibrium with DMF as a function of temperature.' The activation barriers to the interconversion of isomers of [Mo(q3C3H5)(S2CNC4H8)(CO)(dppm)] been determined.' 5 6 have
3.3.9 Tungsten. Variable temperature NMR spectra show the equilibrium in Scheme 11.857
ONW ;, OC, ON-W-CO Ph,P-AuE!-Bu'
, = AP
PPh3
Bu'
7 -
Scheme 11
3.3.10 Rhenium. Temperature dependent EXSY NMR experiments on [Re2@H)(p-S-naph)(CO),(NCMe)]have shown that there are two isomers in equilibr i ~ m . ' ~ The equilibrium for Scheme 12 has been determined by 31P ' NMR spectro~copy.'~~
[Pt(dm~e)~H] [(q'-C5H5)Re(PMe3)(NO)(CO)]+ [Pt(dmpe)2] + =$
[(r15-C,H5)Re(PMe3)(NO)(CHO)I
Scheme 12
3.3.1 1 Iron. NMR studies of [Zn{ (q5-C5H5)Fe[(q'-CsH4)CH N(CH2)3= NMe2]}C12] suggest that two species coexist in solution.860The variable temperature 'H NMR spectra of cis-[Fe[{ HO(CH2)4}2PCH2CH2P{(CH2)40H}2]
855
856 857
858
859
R.R. Schrock, J.Y. Jamieson, S.J. Dolman, S.A. Miller, P.J. Bonitatebus and A.H. Hoveyda, Organometallics, 2002,21,409. K.-H. Yih, G.-H. Lee, S.-L. Huang and Y. Wang, Organometallics, 2002,21,5767. J. Ipaktschi and F. Munz, Organometallics, 2002,21,977. H. Egold, D. Schwarze and U. Florke, J. Chem. SOC., Dalton Trans., 2002,1078. W.W. Ellis, A. Miedaner, C.J. Curtis, D.H. Gibson and D.L. DuBois, J. Am. Chem. SOC.,2002, 124,1926. C. Lopez, A. Caubet, S. Perez, R. Bosque, X. Solans and M. Font-Bardia, Polyhedron, 2002,21, 2361.
I: N M R Spectroscopy in the Liquid and Gas Phase (SO,)] shows ligand exchange.861
65
3.3.1 2 Ruthenium. The equilibrium constant for the binding of pyridine to (107)
has been determined.862 31P NMR spectroscopy shows exchange in [ B U ' ~ P P ~ R U ~ ( Cbetween two isomers.863Temperature dependent 'H and O)~~] 31P NMR spectra of (108) show two different rotamers which i n t e r ~ o n v e r t . ' ~ ~
+/
3.3.13 Rhodium. Variable temperature 'H NMR spectroscopy has been used to
study the encapsulation of C120 (109).865 NMR spectroscopy has been into 31P used to study exchange between isomers of (110).866Exchange of 3-Ph-selenenyl-l-Ph-propene on [Rh2(MTPA)J has been investigated by 'H, I3C and "Se NMR spectro~copy.'~~
3.3.14 Iridium. Variable temperature 19F NMR spectroscopy has been used to
study the equilibrium in Scheme 13.868

3.3.15 Nickel. The coordination of a fifth ligand to (111)has been investigated by
a temperature dependent NMR titration NMR titration experiments have been used to demonstrate molecular tweezers based on a 15-memberedNi" macrocyclic cyclidene bind dicarboxylic acids.' 70
3.3.1 6 Palladium. The solvation of [PdRX(AsPh,),] has been investigated by 'H
NMR
861 862 863 864
~pectroscopy.~ Equilibria 71
between
conformers
of
[{ 1,2-
865 866 867 868 869

8 70
871
W.K. Miller, J.D. Gilbertson, C. Leiva-Paredes, P.R. Bernatis, T.J.R. Weakley, D.K. Lyon and D.R. Tyler, Znorg. Chem., 2002,41,5453. D.G. Gusev and A.J. Lough, Organometallics, 2002,21,5091. R.D. Adams, B. Captain, W. Fu, P.J. Pellechia and M.D. Smith, Angew. Chem., Znt. Ed. Engl., 2002,41, 1951. R.C. van der Drift, E. Bouwman, E. Drent, H. Kooijman, A.L. Spek, A.B. van Oort and W.P. Mul, Organometallics, 2002,21,3401. K. Tashiro, Y. Hirabayashi, T. Aida, K. Saigo, K. Fujiwara, K. Komatsu, S. Sakamoto and K. Yamaguchi, J . Am. Chem. SOC., 2002,124,12 086. A. Suarez, M.A. Mendez-Rojas and A. Pizzano, Organometallics, 2002,21,4611. H. Duddeck, S. Malik, T. Gati, G. Toth and M.I. Choudhary, Magn. Reson. Chem., 2002,40,153. J.H. Berenguer, M. Bernechea, J. Fornies, J. Gomez and E. Lalinde, Organometallics, 2002,21, 23 14. M. Broring, S. Prikhodovski and C.D. Brandt, J. Chem. SOC.,Dalton Trans., 2002,4213. O.P. Kryatova, A.G. Kolchinski and E.V. Rybak-Akimova, J . Inclusion Phenom. Macrocyclic Chem., 2002,42,251. J.A. Casares, P. Espinet and G. Salas, Chem.-Eur. J., 2002,8,4843.
66
Spectroscopic Properties of Inorganic and Organometailic Compounds

Hex
Hex
Hex
\ Hex
4
Ph
Scheme 13
Et Et
( B U ~ ~ P C H ~ ) ~ C ~ H ~ } P ~ ( ~ * - ~ ~ ~ ) ] by H, I3C and 3PNMR have been investigated ~pectroscopy.~~EXSY has been used to study exchange between isomers of 31P (l12).873 NMR investigation has shown that fumaronitrile complexes containing
*S.J. Sabounchei and K. Karamei, Asian J. Chem., 2002, 13, 1581.
67
(113)exist in solution as two isomers.874Low temperature NMR measurements suggest that [(q3-C3H5)Pd{ bis(diphenylphosphino)calix[4]arene tetrabenzyl ether}] is fluxional due to the interconversion of isomers.875[(q3-CloHI5)PdCl]2 exists in solution as two interconverting e p i m e r ~A ~ ~ ~ . molecular receptor consisting of a spacer bearing two cofacially disposed terpyridyl-Pd-ligand units has been studied using variable temperature 'H NMR spectroscopy for molecular recognition of planar aromatic molecules.877 binding of CW [(5,10,15-Ph3The to 20-CsH4N-porphyrin)2PdC12] has been investigated by 'H NMR spectroscopy.878
3.3.1 7 Platinum.'H NMR spectroscopy shows exchange between two isomers of [(q2-fumaronitrile)Pt(NC5H4CH2SBut)].879 The interactions of cis- and trans[PtC12(NH2Pr')(amine)] with 5'-GMP have been investigated by 'H NMR spectroscopy.880 EXSY of four isomers of [{(S,R, R, S)MeNHCHMeCHMeNHMe}Pt( l-Me-5'-GMP)J shows four isomers which exchange.881Equilibria between complexes of [PtC12(5,5,7-Me31,4-diazacycloheptane)]and di- and oligonucleotides have been investigated.882The binding of (aminoethanol)PtCl2 complexes to 5'-GMP has been studied by 'H NMR spectroscopy.883 The relative stability of [PtCllL], L = dppe, dppp, dppb and the sulfonated anaNMR spectra.884 The equilibrium belogues, has been determined from 195Pt tween [(dppe)Pt(OTf)z] and (114) has been investigated by NMR spectroscopy.
873 8 74 875 876 877
878 879
880
881 882
883
884
P. Dotta, A. Magistrato, U. Rothlisberger, P.S. Pregosin and A. Albinati, Organometallics, 2002, 21,3033. M. Zehnder, M. Neuburger, S. Schaffner,M. Jufer and D.A. Plattner, Eur. J. Znorg. Chem., 2002, 1511. K. Takenaka, Y. Obora, L.H. Jiang and Y. Tsuji, Organometallics, 2002,21, 1158. S.G. Sakharov, I.F. Golovaneva, E.P. Sizova, L.A. Pol yakova, A.P. Klyagina and S.P. Gubin, Zh. Neorg. Khim., 2002,47,92. A.J. Goshe, I.M. Steele, C. Ceccarelli, A.L. Rheingold and B. Bosnich, Proc. Natl. Acad. Sci. U.S.A.,2002,99,4823. D.Y. Sun, F.S. Tham, C.A. Reed, L. Chaker and P.D.W. Boyd, J. Am. Chem. Soc., 2002,124,6604. L. Canovese, F. Visentin, G. Chessa, C. Santo, P. Uguagliati, L. Maini and M. Polito, J. Chem. SOC.,Dalton Trans., 2002,3696. E. Pantoja, A. Alvarez-Valdes, J.M. Perez, C. Navarro-Ranninger and J. Reedijk, Znorg. Chim. Acta, 2002,339,525. J.S.Saad, T. Scarcia, K. Shinozuka, G. Natile and L.G. Marzilli, Znorg. Chem., 2002,41,546. V.P. Munk, C.I. Diakos, B.A. Messerle, R.R. Fenton and T.W. Hambley, Chem.-Eur. J.,2002,8, 5486. M.S. Robillard, M. Galanski, W. Zimmermann, B.K. Keppler and J. Reedijk, J. Znorg. Biochem., 2002,88,254. D.W. Lucey and J.D. Atwood, Organometallics, 2002,21,2481.
68
0
0
U N
K KR
3.3.18 Copper. The mechanism of MeCN exchange at CU' in calixC6larene complexes has been studied by 'H NMR spectroscopy.886 3.3.1 9 Gold. Ligand scrambling in [Cy3PSAuCN] complexes in solution has been studied by 13C and "N NMR spectroscopy.88713C, '*N and 31PNMR spectroscopy has been applied to ligand exchange reactions of [(Ph3P)AuCl] with SC(NH2)2.888 Ligand exchange reactions of [(Et3P)AuSATg] with ergothionine, imidazolidine-2-thioneand diazinane-2-thione have been studied by 13C and 31PNMR spectroscopy.889'H NMR spectroscopy has been used to study the fate of sulfur-bound hydrogen on the formation of self-assembledthiol monolayers on 3.3.20 Z n . Variable concentration 'H NMR spectroscopic studies of ic [{(PhCH2)2N}2Zn],89f [{(2,6-Et2C6H3)2N}zZn(p-OP+)],892 and show a monomer-dimer equilibrium. The association constant for CHB(3-cumenyl-5-Mep~)~Zn-thyminate]-9-Et-adenine has been determined by NMR spectrocopy.^^^ Complexation induced shifts in 'H NMR chemical shifts of zinc porphyrins with amines correlate well with differences in association cons t a n t ~'H ~ ~ ~ spectroscopy has been used to study complexation of two . NMR aromatic diimide guest molecules with a zinc b i ~ p o r p h y r i n 'H ~ ~ . ~ NMR titrations have confirmed the formation of a 1:l complex between a phenanthroline strapped zinc porphyrin and an N-unsubstituted i m i d a ~ o l e'H NMR spec.~~~ troscopy has been used to follow host-guest equilibria between ethane-bridged bis(zinc porphyrin) and chiral monoamine and monoalcohol guests.897 Rotaxane type complexation behaviour of cyclodextrins with Zn" tetraporphyrin-viologen linked compounds has been studied by 'H NMR spectro885 886 887
888 889 890 891
892 893 894
895 896 897
N.M. Brunkan, P.S. White and M.R. GagnC, Organometallics, 2002,21, 1565. Y. Rondelez, M.-N. Rager, A. Duprat and 0.Reinaud, J. Am. Chem. SOC., 2002,124,1334. S . Ahmad, A.A. Isab, H.P. Perzanowski, M.S. Hussain and M.N. Akhtar, Transition Met. Chem. (Dordrecht, Neth.), 2002,27, 177; S . Ahmad, A.A. Isab and H.P. Perzanowski, Can. J. Chem., 2002,80, 1279. S . Ahmad and A.A. Isab, J. Inorg. Biochem., 2002,88,44. A.A. Isab and S. Ahmad, J. Inorg. Biochem., 2002,88,53. M. Hasan, D. Bethell and M. Brust, J. Am. Chem. SOC.,2002,124,1132. D.R. Armstrong, G.C. Forbes, R.E. Mulvey, W. Clegg and D.M. Tooke, J. Chem. SOC.,Dalton Trans., 2002, 1656. L.R.Rieth, D.R. Moore, E.B. Lobkovsky and G.W. Coates, J. Am. Chem. SOC.,2002,124,15 239. D. Badura and H. Vahrenkamp, Inorg. Chem., 2002,41,6020. R.M. Gomila, D. Quinonero, C. Rotger, C. Garau, A. Frontera, P. Ballester, A. Costa and P.M. Deya, Org. Lett., 2002,4,399. L.Flamigni, M.R. Johnston and L.Giribabu, Chem.-Eur. J.,2002,8,3938. D. Paul, J.A. Wytko, M. Koepf and J. Weiss, Inorg. Chem., 2002,41,3699. V.V. Borovkov, J.M. Lintuluoto, H. Sugeta, M. Fujiki, R. Arakawa and Y.Inoue, J . Am. Chem. 2002,124,2993. SOC.,
69
s c ~ p y . ~The equilibrium between [trans,cis,cis-RuC12(C0)2{5,lO-(4* ~ NC5H4)215,20-Ph2-porphyrinato-Zn}]~ a nitrogen ligand has been shown to and be slow by NMR spectroscopy.899
3.3.21 Cadmium. Variable temperature NMR and ROESY studies of [{ MeSi(SiMeNC6H4-4-Me)3Sn}2Cd] have shown dynamic exchange between two isomers.900 3.3.22 Boron. Variable temperature I9F NMR spectroscopy has been used to study the equilibrium between MeCN and [B(CSF5)3] (115).901 or The variable show temperature 'Hand IIB NMR spectra of [(C4H4N)2BB(C4H4N)2] an equilibrium with a polymer.902
3.3.23 Aluminium. Donor-acceptor interactions of compounds such as [Et3A1E(SiMe3)3] [Bu'~AIEP~'~],= P, As, Sb, show temperature-dependand E ent NMR spectroscopy.903A trimer-monomer equilibrium for [Et2AlN3] has been studied using 'H and 27AlNMR spectroscopy.904 3.3.24 Silicon. Competitions between pairs of [(Me3Si)2(ZMe2Si)CSiMe2Br] a for deficiency of AgBF4 in E t 2 0have been studied using 19FNMR spectroscopy. The 29SiNMR spectrum of [(Me3Si)2(PhOMe2Si)CSiMe2Br] reported.905 was
3.3.25 Tin. 'H NMR spectroscopy has been used to study the equilibrium in Scheme 14. The '19Sn NMR spectrum was also reported.906The interaction of
898 899
900
90 1
902
903
904
905
906
T. Ujiie, T. Morozumi, T. Kimura, T. Ito and H. Nakamura, J . Inclusion Phenom. Macrocyclic Chem., 2002,42,301. E. Iengo, E. Zangrando, R. Minatel and E. Alessio, J. Am. Chem. Soc., 2002,124,1003. M . Lutz, B. Findeis, M. Haukka, R. Graff, T.A. Pakkanen and L.H. Gade, Chem.-Eur.J.,2002,8, 3269. M.V. Metz, D.J. Schwartz, C.L. Stern, T.J. Marks and P.N. Nickias, Organometallics, 2002, 21, 41 59. H. Abu Ali, I. Goldberg and M. Srebnik, Eur. J . Inorg. Chem., 2002,73. A. Kuczkowski, S. Schulz, M. Nieger and P.R. Schreiner, Organornetallics, 2002,21,1408. Z.-X. Gao, X.-H. Zhang and L.-C. Feng, Wuji Huaxue Xuebao, 2002, 18, 654; Z.-X. Gao and X.-H. Zhang, Wuji Huaxue Xuebao, 2002,18,683. C. Eaborn, A. KowaIewska, J.D. Smith and W.A. Stanczyk, J . Organomet. Chem., 2002,640,29. R. Jambor, L. Dostal, A. RliiiEka, I. Cisaiova, J. Brus, M. HolEapek and J. HoleEek, Oraanometallics. 2002.21.3996.
70
[SnF2] and [SbF3] with [POC13] and [PC15] has been studied by 19F,31P and 'I9Sn NMR spectroscopy.907'19Sn NMR spectroscopy has been used to study diffusion-controlledexchange of halogens in mixtures of Sn'" tetrahalidese9O8
Scheme 14
3.3.26 Arsenic. 31P NMR spectroscopy has been used to study the exchange in the equilibrium in Scheme 15.909 Variable temperature 'H and 31P NMR spectroscopy of [ C H ~ ( ~ - B U ' - ~ - M ~ - C ~1,2-02c6cl-4)]shows exchange beH~~)~PC~( tween two isomers.910
Scheme 15
3.4 Course of Reactions. - I3C PHIP NMR spectra and polarisation transfer during hydrogenation of alkynes have been r e p ~ r t e d . ~ '
3.4.1 Lithium. 6Li and 7Li NMR spectroscopy has been used to study the
31P NMR spectroscopyhas been used to lithiation of l-meth~xynaphthalene.~~~ E = monitor the reaction of [Li{ Bu'N(E)P(~-NBu')~P(E)NHBu')~, S, Se, with [TeCb].913 'H and 31PNMR spectroscopy has been used to follow the isomerisation of [Li{ CH2P(C6H4-2-CH2NMe2)2}] to [RP{C6H4-2-CH(C6H4-2CH2NMe2)NMe2} Li].9
3.4.2 Potassium. Potassium efflux from plant cells has been measured using 87Rb NMR spectros~opy.~'
907
909
''
910
'12 '13
914
Y.V. Kokunov, M.M. Ershova and G.A. Razgonyaeva, Russ.J. Coord. Chem., 2002,28,461. Y.-h. Zhang and X.-a. Mao, Bopuxue Zazhi, 2001,18,322. N.V.Timosheva, A. Chandrasekaran,R.O. and R.R. Day Holmes, J. Am. Chem. SOC.,2002,124, 7035. S. Kumaraswamy and K.C.K. Swamy, Polyhedron, 2002,21,1155. M . Stephan, 0.Kohlmann, H.G. Niessen, A. Eichhorn and J. Bargon, Magn. Reson. Chem., 2002, 40,157. J. Betz and W. Bauer, J. Am. Chem. SOC.,2002,124,8699. G.G. Briand, T. Chivers and G. Schatte, Inorg. Chem., 2002,41,1958. K. Izod, P. O'Shaughnessy and W. Clegg, Urganometallics, 2002,21,641.
71
3.4.3 Calcium. The hydrolysis of [Ca(OEt)*]and [P(OEt)3] has been followed by 31P NMR spectroscopy.916 3.4.4 Yttrium. 'H NMR spectroscopy has been used to follow the reaction of (116), R = menthyl, with Pr"NH2.9'7
3.4.5 Uranium. The reaction of Co, Ni, and Cu Schiff base complexes with [UC14] has been followed by 'H NMR spectro~copy.~'~ 3.4.6 Titanium. The thermolysis of [qS-C5H4CMe2Ph)Ti(CH2Ph)3] been folhas lowed by 'H NMR spectros~opy.~'~ reaction of [A12Me6] with The [ ( B U ' ~ P N ) ~ T ~has~been followed by 31PNMR spectroscopy.920Transfer M ~] hydrogenation processes to the p3-alkylidyneon [{ Ti(q5-C5Me5)(p-O)}3(p3-CR)] have been detected by 'H NMR spectroscopy.921 3.4.7 Zirconium. The mechanism of vinylic and allylic C-F bond activation of non-perfluorinated alkenes using [(qS-C5Me5)2ZrH2] been studied using 'H has and 19FNMR spectroscopy.922 and I9FNMR spectroscopy has been used to 'H follow the reaction of C6FsHwith [(q5-CsMe5)2ZrH2].923 DOSY has been used to study the reaction of I3CO2with [(qs-C5H5)2ZrCl(H)].924 reaction of [(qsThe C5Me5)2ZrMe2] [Ph3C]+ has been followed by 'H NMR spectroscopy.925 with and The polymerisation of ethene over [(qS-C5H5)2ZrMe2] a silsesquioxane which has been modified with [(C6F5)2BX]has been studied by "B, 19Fand 29Si NMR spectroscopy to model catalysis on a silica surface.926"B NMR spectro91 5 916
917
M.L.H. Gruwel, Mol. Membrane B i d , 2001,18,291. D.D. Green, G.S.K. Kannangara, A. Milev and B. Ben-Nissan, Key Eng. Mater., 2002,218-220, 75. M.R. Douglass, M. Ogasawara, S. Hong, M.V. Metz and T.J. Marks, Otganometallics, 2002,21,
283.
918
T. Le Borgne, E. Riviere, J. Marrot, P. Thuery, J.-J. Girerd and M. Ephritikhine, Chem.-Eur. J.,
2002,8,774.
919 920 921
922 923 924 925
P.J.W. Deckers and B. Hessen, Organometallics, 2002,21,5564. J.E. Kickham, F. Gubrin and D.W. Stephan, J. Am. Chem. SOC.,2002,124,11486. R. AndrQ, M.V. Galakhov, M.P. Gomez-Sal, A. Martin, M. Mena, M.D. Morales-Varela and C. Santamaria, Chem.-Eur. J., 2002,8,805. B.M. Kraft and W.D. Jones, J . Am. Chem. SOC.,2002,124,8681. B.M. Kraft and W.D. Jones, J. Organornet. Chem., 2002,658,132. N.E. Schlorer, E.J. Cabrita and S. Berger, Angew. Chem., Int. Ed. Engl., 2002,41,107. C.P. Casey and D.W. Carpenetti, J. Organornet. Chem., 2002,642,120.
72
scopy has been used to analyse catalyst solutions obtained from [(q6C5H5BR)2ZrC12] and [MeA10],.92 The reaction of [(q5-C5H5)2ZrC12] or [{ Ph2C(q5-fluorenyl)2}ZrC12] with [AlBui3] and [PhNMe2H] has been investigated using 'H NMR The reaction of [Zr(OR),] with methacrylic acid has been monitored by 'H and 13C NMR spectroscopy.929 The preparation of Na3Zr2Si2PO12 been followed using "P NMR spectrohas scopy.930
+
3.4.8 Vanadium. The photoinduced reduction of [LVO2]-, where L is a tridentate ONS ligand, has been investigated by 'H NMR spectroscopy.93151VNMR spectroscopy has been used to follow the formation of d e ~ a v a n a d a t eAlco.~~~ holysis and hydrolysis reactions of [VOC12(OCH2CH20Ph)] have been monitored by 5'V NMR spectroscopy.933
3.4.9 Niobium. 19F,93Nband '19SnNMR spectroscopy has been used to study the reactions of [SnF2] and [SbF3] with [NbC15].934
3.4.10 Tantalum. The mechanism of the addition of dihydrogen to [(q5C5MeJ2Ta(CH2)H) has been examined by parahydrogen-induced polariza t i ~ n . The addition of parahydrogen to [{(q5-C5H5)2TaCl}2(p-N2)] been '~~ has investigated.' 36 3.4.1 1 Chromium. The reaction of [HCr(CO)5]- with methyl acrylate has been monitored by 'H NMR spectro~copy.~~' 3.4.12 Molybdenum. The reaction between [(q5-C5H5)Mo(PMe3)3H]and HC02H has been studied by 'H NMR spectroscopy.938'H NMR spectroscopy has been used to follow the reaction of [(q5-C5H5)M~(C0)2(PCy3)H] with [Ph3C]+.93931P NMR spectroscopy has been used to follow the reaction of (117) with [ B U ~ S ~ C = C P ~ ] . ' reaction of [(q7-C7H7)Mo(q6-C6H5Me)] The ~ ~ with op+
926
927
928
929
930
931 932
933
934
935
936
937
938 939
R.A. Metcalfe, D.I. Kreller, J. Tian, H. Kim, N.J. Taylor, J.F. Corrigan and S. Collins, Organometallics, 2002,21, 1719. Z.J.A. Komon, J.S. Rogers and G.C. Bazan, Organometallics,2002,21, 3189. C. Gotz, A. Rau and G. Luft, J. Mol. Catal. A: Chem., 2002,184,95. G. Kickelbick, M.P. Feth, H. Bertagnolli, M. Puchberger, D. Holzinger and S. Gross, J. Chem. Soc., Dalton Trans., 2002, 3892. A. Martucci, S. Sartori, M. Guglielmi, M.L. Di Vona, S. Licoccia and E. Traversa, J. Eur. Ceram. SOC.,2002,22, 1995. S.K. Dutta, S. Samanta, S. Mukhopadhyay, P. Burckel, A.A. Pinkerton and M. Chaudhury, Inorg. Chem., 2002,41,2946. L. Bouhedja, N. Steunou, J. Maquet and J. Livage, J. Solid State Chem., 2001,162,315. E.C.E. Rosenthal and F. Girgsdies, 2. Anorg. Allg. Chem., 2002,628,1917. Y.V. Kokunov, M.M. Ershova, G.A. Razgonyaeva and Y.A. Buslaev, Russ. J. Coord. Chern., 2001,27,644. D.C. Bregel, S.M. Oldham and R. Eisenberg, J. Am. Chem. SOC.,2002,124,13 827. D.C. Bregel, S.M. Oldham, R.J. Lachicotte and R. Eisenberg, Znorg. Chem., 2002,41,4371. B. Andrieu, J.-J. Brunet, 0.Diallo, B. Donnadieu, J. Lienafa and E. Roblou, J. Organornet. Chem., 2002,643,27. J.H. Shin, D.G. Churchill and G. Parkin, J. Organomet. Chem., 2002,642,9. M.H. Voges and R.M. Bullock, J . Chem. SOC.,Dalton Trans., 2002,759.
I : N M R Spectroscopy in the L q i and Gas Phase iud
73
tically active Schiff bases has been investigated using 'H NMR spectroscopy.941 The oxidation of PhSMe by H202catalysed by Na2Mo04has been followed by 'H NMR spectroscopy.942 The ability of [Mo02Br2L2]to oxidise Bu'SH to Bu'SSBu' has been examined by 'HNMR spectroscopy.943
3.4.23 Tungsten. 'H NMR spectroscopy has been used to follow the isomerisaThe conversion of [P2W15056]'2into tion of [W2(~2-02CBu')4(p-EtC=CEt)2].944 [P2W15M3062]9-, = V, Nb, has been followed by 31P M NMR spectroscopy and the '83W NMR spectra were reported.94s The isomerisation of fJ-[P2W18062]6to a'[P2W18062]6- has been followed by 31P NMR spectroscopy.946
3.4.14 Rhenium. The kinetic and thermodynamic parameters for the 0x0 and imido exchange reactions among [MeReOJ, [MeRe02(NR)], [MeReO(NRh] and [MeRe(NR)J have been reported.947NMR spectroscopy has been used to show that (SReRC)-[(q5-C5H5)Re(CN)( PPh3)(CHPhPPh2H)]+ epimerises to (SReSC)-[(q5-C5H5)Re(CN)(PPh3)(CHPhPPh2H)] NMR spectroscopy + .948 'H has been used to follow the reaction of [Re(OMe)(C0)3(bipy)] with MeI, EtBr and MeCOC1.949 3.4.25 Iron, Ruthenium and Osmium. 'H NMR spectroscopy has been used to follow the irreversible transformation of [(q5-C5MeS)Fe(dppe)(H2)] [(q5to C5Me5)Fe(dppe)(H)2]. 9 s 0 Vinyl C-F cleavage by [OS(H~)CC(PP~'~)~] + has been followed by 'H NMR s p e c t r o s c ~ p y . The reaction of [(q5-C5Me5)Os(CO)2H] ~~ with [(q5-C5Mes)Fe(C0)2FBF3] been followed by 'H NMR spectroscopy.9s2 has 31PNMR spectroscopy has been used to follow the reaction of [RuH(q5-indenyl)(dppm)] and PhCaCCrCPh.9s Reactions of PrC=CH and Bu'CsCH
+
940
941 942
943
944 945
946
947
948
949
950 951
952
A. Ricci, F. Angelucci, M. Bassetti and C. Lo Sterzo, J . Am. Chem. Soc., 2002, 124, 1060; F. Angelucci, A. Ricci, C. Lo Sterzo, D. Masi, C. Bianchini and G. Bocelli, Organometallics, 2002,21, 3001; A. Ricci and C. Lo Sterzo, J. Organomet. Chem., 2002,653,177. H. Brunner, J. Klankermayer and M. Zabel, Organometallics, 2002,21,5746. C.A. Bunton and N.D. Gillitt, J. Phys. Org. Chem., 2002,15,29. F.J. Arnaiz, R. Aguado, M.R. Pedrosa, J. Mahia and M.A. Maestro, Polyhedron, 2002,21,1635. M.J. Byrnes, M.H. Chisholm, J. Gallucci and P.J. Wilson, Organometallics, 2002,21,2240. B.J. Hornstein and R.G. Finke, Znorg. Chem., 2002,41,2720. T.M. Anderson and C.L. Hill, Znorg. Chem., 2002,41,4252. W.-D. Wang and J.H. Espenson, Znorg. Chem., 2002,41,1782. K. Kromm, F. Hampel and J.A. Gladysz, Organometallics, 2002,21,4264. E. Hevia, J. Perez, L. Riera, V.Riera, I. del Rio, S. Garcia-Granda and D. Miguel, Chem.-Eur.J., 2002,8,4510. J.-R. Hamon, P.Hamon, L. Toupet, K. Costuas and J.-Y. Saillard, C . R. Chim., 2002,5,89. G. Ferrando-Miguel, H. Gerard, 0.Eisenstein and K.G. Caulton, Znorg. Chem., 2002,41,6440. T.-Y. Cheng and R.M. Bullock, Organometallics, 2002,21,2325.
74
with [RuHCI{ ~ , ~ - ( B u ' ~ P C H ~ ) ~ C ~ H ~ } ] and [OsH2Cl{~ , ~ - ( B u ' ~ P C H ~ ) ~ C ~ H ~ } ] have been studied by NMR spectroscopy.954 A mechanistic study of [Ru(H)2(CO)(PPh3)3]catalysed addition of C-H bonds in aromatic esters to alkenes has been reported.95 The high-pressure hydrogenation of indole [Rh(q2-Me02CC=CC02Me)(Ph2PCH2)3CMe] and catalysed by [ R u ( N C M ~ ) ~ ( P ~ ~ P C H ~has C M ~ ]followed by NMR spectroscopy.956 ) ~ been Enantiomeric hydrogenations of R 3,3-Me2-oxaloacetate ketone substrates, 2 catalysed by [Ru{(R)-BINAP}(H)(NCMe),(THF),_,I+, have been followed by NMR spectro~copy.~~' mechanism of asymmetric hydrogenation of aThe (acy1amino)acrylicesters catalysed by [(BINAP)Ru(O~CM~)~] been studied has by NMR spectroscopy.958 In situ formation of ruthenium catalysts for the homogeneous hydrogenation of C o 2 from [(q6-C6H6)R~C12]2,9 and 59 [ R u C ~ ( O ~ C M ~ ) ( P M ~ ~ ) ~ ] , ~investigated using 31P has been ~ ' NMR spectroscopy. 29Si NMR spectroscopy has been used to detect intermediates during the catalytic hydrosilation of acetophenone using (118).961Mechanistic studies of the using parahydrogen as a probe hydrogenation of alkynes with [OS~(CO),&-H)~] have been reported.962The reactions of [OS,(CO)~{ p3-q3-C9H7(4-Me)N}(p-H)] and related compounds with parahydrogen have been studied.963
+
OC-yG& Si Me,Ph
'H NMR spectroscopy has been used to follow the reaction of R13SiCH= CH2 with CH2= CHCH20R2 to give R',SiCH = CHCH20R2 and CH2= CH2 = RU( catalysed by [ C ~ ~ ( C Y ~ P ) ~CHPh)].964 The polymerisation of [Fe(q5C5H5)2Si(C=CPh)2] been followed by 'H NMR spectroscopy and the product has
953 954
955 956 957 958
959
960
96 1 962
963 964
M. Bassetti, S. Marini, J. Diaz, M.P. Gamasa, J. Gimeno, Y. Rodriguez-Alvarez and S. GarciaGranda, Organometallics, 2002,21,4815. D.G. Gusev, T. Maxwell, F.N. Dolgushin, M. Lyssenko and A.J. Lough, Organometallics, 2002, 21, 1095. F. Kakiuchi, H. Ohtaki, M. Sonoda, N. Chatani and S. Murai, Chem. Lett., 2001,918. P. Barbaro, C. Bianchini, A. Meli, M. Moreno and F. Vizza, Organornetallics,2002,21, 1430. C.J.A. Daley and S.H. Bergens, J. Am. Chem. SOC.,2002,124,3680. M. Kitamura, M. Tsukamoto, Y. Bessho, M. Yoshimura, U. Kobs, M. Widhalm and R. Noyori, J. Am. Chem. SOC.,2002,124,6649. C.C. Tai, J. Pitts, J.C. Linehan, A.D. Main, P. Munshi and P.G. Jessop, Inorg. Chem., 2002,41, 1606. P. Munshi, A.D. Main, J.C. Linehan, C.C. Tai and P.G. Jessop, J. Am. Chem. SOC., 2002, 124, 7963. K. Matsubara, K. Ryu, T. Maki, T. Iura and H. Nagashima, Organometallics, 2002,21,3023. R. Gobetto, L. Milone, F. Reineri, L. Salassa, A. Viale and E. Rosenberg, Organometallics, 2002, 21, 1919. B. Bergman and E. Rosenberg, Organometallics, 2002,21,1508. M. Kujawa-Welten, C. Pietraszuk and B. Marciniec, Organometallics, 2002,21,840.
75
characterised by 29SiNMR spectroscopy.965 NMR spectroscopy has been 31P used to follow meso to racemic isomerism of [(qs-l-Ph2P-indenyl)2Fe].966 The has photolysis of [{ (qs-CsH5)Fe(C0)2CH2SiMe2}2CH2] been followed by 13Cand 29Si NMR spectroscopy.967 NMR spectroscopy has been used to monitor the 31P reaction of [(q5-indenyl)Ru(PPh3)2Cl] and HPPh2.968 Reactions of [($PhPh)RuCl(en)][PF6] with cysteine and methionine have been followed by 'H and I5NNMR spectroscopy.969 The oxidation of heme to p- and 6-biliverdin by Pseudomonas aeruginosa heme oxygenase has been studied using 'H and I3C NMR spectroscopy.970 NMR spectroscopy has been used to study the reduction of [Cr04]'- to Cr"' by ~ 7 . ~ Ligand ~ ' substitution reactions of cis,ciscytochrome [(bpy)2L'RuORuL2(bpy)2]"have been studied using 'H NMR spectroscopy.972 31PNMR spectroscopy has been used to follow the reaction of [RuCl(BINAP)(phen)(MeOH)] with air.973 The coordination process of a chiral diiminodiphosphine with ruthenium has been studied by 31PNMR spectroscopy.974
+
3.4.1 6 Cobalt. The mechanism of the reaction between 5'-deoxyadenosylcobinamide and cyanide has been studied using 'H NMR spectroscopy.975'H NMR spectroscopy has been used to determine the isomerisation kinetics of cisand tran~-[Co(S2CNR2)2(PHPh2)2]+.~~~ 3.4.1 7 Rhodium. The reaction of bis(a1kene)rhodium complexes with parahydrogen has been monitored by 'H NMR spectroscopy. The Io3RhNMR spectrum of [($-C5H5)Rh(C2H3SiMe3)(H)2]was also reported.977 The reactions of [Rh(Hh(PPh3),(Et0H),] with nitrogen ligands have been monitored by 'H NMR spectroscopy.978 The thermal decomposition of complexes of the type [RhX(H)(SiR'R2R3)(PPh3)2] followed by NMR spectroscopy. The 29Si{ was 'H} NMR spectra show that 'J('03Rh29Si) values increases in the number of alkoxy substituents of silicon.979 and 31P 'H NMR spectroscopy has been used to study
+
965
966
967
968
969
970
971
972
973
974 975
976
977
978
A. Berenbaum, A.J. Lough and I. Manners, Organometallics, 2002,21,4415. O.J. Curnow and G.M. Fern, Organometallics, 2002,21,2827. Y.Q. Mang, F. Cervantes-Lee and K.H. Pannell, Organometallics, 2002,21,5859. J.B. Westmore, L. Rosenberg, T.S. Hooper, G.D. Willett and K.J. Fisher, Organometallics, 2002, 21, 5688. F.Y. Wang, H.M. Chen, J.A. Parkinson, P.D. Murdoch and P.J. Sadler, Znorg. Chem., 2002,41, 4509. G.A. Caignan, R.Deshmukh, A. Wilks, Y.H. Zeng, H.-w. Hiang, P. Moenne-Loccoz, R.A. Bunce, M.A. Eastman and M. Rivera, J. Am. Chem. SOC.,2002,124,14 879. M. Assfalg, I. Bertini, C. Michel and P. Turano, Proc. Nat. Acad. Sci. U.S.A.,2002,99,9750. R. Arakawa, N. Kubota, T. Fukuo, 0.Ishitani and E. Ando, Znorg. Chem., 2002,41,3749. P.W. Cyr, S.J. Rettig, B.O. Patrick and B.R. James, Organometallics, 2002,21,4672. D.-D. Zhou, C. Li, X.-M. Liu, X.-W. Han and X.-H. Bao, Wuji Huaxue Xuebao, 2002,18,238. N.E. Brasch, A.G. Cregan and M.E. Vanselow, J. Chem. SOC.,Dalton Trans., 2002,1287. S . Iwatsuki, T. Suzuki, A. Hasegawa, S. Funahashi, K. Kashiwabara and H.D. Takagi, J. Chem. SOC., Dalton Trans., 2002,3593. C. Godard, P. Callaghan, J.L. Cunningham, S.B. Duckett, J.A.B. Lohman and R.N. Perutz, Chem. Commun., 2002,2836. X.Y. Yu, M. Maekawa, T. Morita, H.C. Chang, S. Kitagawa and G.X. Jin, Polyhedron, 2002,21, 1613.
76
the dissolution of [RhCl(PPh,),] in [l-Et-3-Me-imidazolium][A12C17] give to cis-[RhCl(( 181)-ClAlC13)(PPh3)] trans-[RhH(( 181)-ClA1C13)(PPh3)].980 and The enantiomeric hydrogenation of 30 acetamidobutenoates with Rh' complexes has been investigated by NMR s p e c t r o ~ c o p y .The hydroformylation of ethene in ~~ liquid C 0 2using [Rh(CO)2(acac)]as the catalyst precursor has been monitored by high pressure NMR spectroscopy.982High pressure "P NMR spectroscopy has been used to follow highly regioselective rhodium catalysed hydroformylaThe tion of alkenes using phosphine containing d e n d r i m e r ~ . ~ ' ~ asymmetric hydroformylation of styrene catalysed by carbohydrate diphosphite-Rh' complexes has been studied by high pressure NMR spectroscopy.984A kinetic study of the hydrosilation of acetophenone by [Rh(cod)C1I2/(R)-BINAPhas been carried out using 'H NMR spectroscopy.98531P NMR spectroscopy has been used to investigate the reaction of [ R h ( a ~ a c ) ( q ~ - C ~and )(119).986 intraH~ ~] The molecular dehydrofluorinative coupling of (q5-C5Me5) and C6F5Pligands in [(q5-C5Me5)Rh{ (C6Fs)2PCH2CH2P(C6F5)2}] been followed by NMR spechas tro~copy.~" NMR spectroscopy has been used to follow the dissociation of 'H [Rh{q6-C6H4-1,3-(OCH2CH2PPh2)2}]2.988 31P NMR spectroscopy has been used to follow the epimerisation of (120).989 The reaction of [(4,4'-Me2bpy)RhCl(DMSO)] with CH2C12 has been followed by 'H NMR spectroscopy.990
But
A 0
(119)
(120)
+
3.4.18 Iridium. 'H, ' B and 31P ' NMR spectroscopy has been used to follow the photolysis of [PhB(CH2PPh2)31rH2(PMePh2)],991 The kinetics of the isomerisation of [(qs-C5Me5)(Me3P)(H)Ir{ ~ - S ~ H ( ~ ~ S ) ( ~ - C H ~ - ~ , ~ - to ~ & H ~ ) } ] K M [(q5979 980 98 1
982 983
984 985 986
987 988
989 990 99 1
Y. Nishihara, M. Takemura and K. Osakada, Organometallics, 2002,21,825. B.E. Mann and M.H. Guzman, Inorg. Chim. Acta, 2002,330,143. D. Heller, H.-J. Drexler, J.-s. You, W. Baumann, K. Drauz, H.-P Krimmer and A. Borner, Chem.-Eur. J.,2002,8, 5196. C.R. Yonker and J.C. Linehan, J . Organomet. Chem., 2002,650,249. L. Ropartz, K.J. Haxton, D.F. Foster, R.E. Morris, A.M.Z. Slawin and D.J. Cole-Hamilton, J . Chem. SOC.,Dalton Trans., 2002,4323. M. Dieguez, 0. Pamies, A. Ruiz and C. Claver, New J. Chem., 2002,26,827. C. Reyes, A. Prock and W.P. Giering, Organornetallics, 2002,21,546. M. Kuriyama, K. Nagai, K. Yamada, Y. Miwa, T. Taga and K. Tomioka, J. Am. Chem. SOC., 2002,124,8932. R.M. Bellabarba, M. Nieuwenhuyzen and G.C. Saunders, Organometallics, 2002,21, 5726. B.J. Holliday, Y.-M. Jeon, C.A. Mirkin, C.L. Stern, C.D. Incarvito, L.N. Zakharov, R.D. Sommer and A.L. Rheingold, Organometallics, 2002,21,5713. J. Andrieu, P. Richard, J.M. Camus and R. Poli, Inorg. Chem., 2002,41,3876. R. Dorta, L.J.W. Shimon, H. Rozenberg and D. Milstein, Eur. J. Inorg. Chem., 2002,1827. J.D. Feldman, J.C. Peters and T.D. Tilley, Organometallics, 2002,21,4050.

+
77
C5Me5)(Me3P)(H)Ir{ Si(me~)~}]have been determined using NMR spectrocopy.^^^ The reaction of parahydrogen with [Ir(CF3)(CO)(dppe)( 1,2-I2C6H4)I2+ has been investigated by 'H and 31P NMR spectroscopy.993The activation of H2 by [IrBr2(C0)2] / S n B ~ - ~ , ~ [Ir(CO)C1L2],995 been studied using para~~and has hydrogen. Catalytic alkene hydrogenation using N-heterocyclic carbene-phosphine complexes of iridium has been investigated using p a r a h y d r ~ g e n . ~ ~ ~ 'H NMR spectroscopy has been used to follow oxidative addition of MeOH to [(CgH 14)IrC1(PMe3)3],9 and the reaction of [HBpz31r(H)(dppm-H)] with an excess of MeI.998 The reaction between [Ir(q2-COE)2C1]2and 1-Me0-3,5(But2PCH2)2C6H3 been followed using 31P has NMR spectroscopy.999 NMR studies have shown that (121) isomerises to (122) via (123).1000
Me&.
Ph
-11\
PPh,
Ir-PPh,
3.4.19 Nickel. The reductive elimination of R2 from [NiRz(bpy)] has been studied using ' H NMR spectroscopy.'001 'H NMR spectroscopy has been used to follow H/D exchange at the CH2groups in (124).'Oo2
2 t
3.4.20 Palladium and Platinum. The reaction of PhCZCH with parahydrogen, using colloidal Pd, leads to nuclear spin polarization in the hydrogenation products.'003 PHIP is observed when parahydrogen is used for hydroformyla992
993
994 995
996 997
998
999
'Oo0
'Ool
'Oo2
loo3
S.R. Klei, T.D. Tilley and R.G. Bergman, Organometallics, 2002,21,3376. P.J. Albietz, J.F. Houlis and R.Eisenberg, Inorg. Chem., 2002,41,2001. A. Permin and R. Eisenberg, Inorg. Chem., 2002,41,2451. S.K. Hasnip, S.A. Colebrooke, C.J. Sleigh, S.B. Duckett, D.R. Taylor, G.K. Barlow and M.J. Taylor, J. Chem. SOC.,Dalton Trans., 2002,743. L.D. Vazquez-Serrano, B.T. Owens and J.M. Buriak, Chem. Commun., 2002,2518. 0.Blum and D. Milstein, J. Am. Chem. SOC., 2002,124, 1 1 456. J.S. Wiley and D.M. Heinekey, Inorg. Chem., 2002,41,4961. H.A.Y. Mohammad, J.C. Grimm, K. Eichele, H.G. Mack, B. Speiser, F. Novak, M.G. Quintanilla, W.C. Kaska and H.A. Mayer, Organometallics, 2002,21, 5775. H.-P. Wu, S. Lanza, T.J.R. Weakley and M.M. Haley, Organometallics, 2002,21,2824. T. Yamamoto, M. Abla and Y . Murakami, Bull. Chern. Soc. Jpn., 2002,75,1997. M.V. Baker, B.W. Skelton, A.H. White and C.C. Williams, Organometallics, 2002,21,2674. A. Eichhorn, A. Koch and J. Bargon, J. Mol. Catal. A: Chem., 2001,174,293.
78
tion in the presence of [PtCl(COEt)(PPh&J and 3 equivalents of SnC12.1004 'H NMR spectroscopy has been used to follow the reaction of (125)with CO at high pressure,"" and between [PdMe(NCMe)L] +,L = pyridine-imidazoline ligand, and C0.'oo6 The intermediates involved in the Pt catalysed methoxycarbonylation of ethene have been characterised by in situ NMR spectr~scopy.~"~ 31P NMR spectroscopy has been used to study what happens to [(Ph2PCHMeCHMePPh2)Pd(02CMe)Junder CO/C2H4at high pressure.loo* Allene insertion into the Pd-C bond has been studied by 'H NMR spectrocopy.'^'^ 'H NMR spectroscopy has been used to study aryl halide addition to [ ( C Y ~ P ) ~ P ~ ]The~ ' . ~ ' reaction of [(Ph2PCH2CH2NMe2)PtMe2] CCl, has with been investigated."" 'H NMR spectroscopy has been used to follow the reaction of [Me(H20)Pt(ArN= CMeCMe = NAr)]+ with benzene,"12 and ring clolo' Intermediates in the sure in cis-[Ph2Pt(CO)(Ph2PCH2CH2-2-C5H4N)]. [Pt{ 2,6-(R2PCH2)2C6H3}(0Tf)] catalysed hydroamination of acrylonitrile with p-toluidine have been detected by NMR spectr~scopy.~''~ NMR spectro'H scopy has been used to monitor the reaction of (126) to give (127).lo1' The reactions of [Pd(dba)2] with 1,3-{Ph2PC6H4C(0)NH-2-C6H3N-6NHC(0)}2C6H4,'0'6 [Pf(~l~-norbornene)~] with 2Ph2PC6H4CH N(CH2)2Ph,1'1 have been followed by 31P = NMR spectroscopy. Two transient intermediates have been detected by 31PNMR spectroscopy during the reaction of [(Pri2PCH2CH2NMe2)Pd(q2-PhC=CPh)] with PhCECPh. lo' * [CH3C02]-/[CD3C02] - exchange on truns-4-CH3CO2-(q3-cyc1ohexenyl)Pd complexes has been studied by 'H NMR spectroscopy.' 13C NMR spectroscopy has been used to follow the insertion of CO into a Pd-0 The bond in [(tmeda)Pd(OC6H4-4-But)~].1'20 coordination of peptides to Pd"
''
loo4
'Oo5
A.B. Permin and R. Eisenberg, J. Am. Chem. Soc., 2002,124,12 406. P. Pelagatti, A. Bacchi, M. Carcelli, M. Costa, H.W. Fruhauf, K. Goubitz, C. Pelizzi, M. Triclistri and K. Vrieze, Eur. J. Inorg. Chem., 2002,439. ' O o 6 A. Bastero, A. Ruiz, C. Claver, B. Milani and E. Zangrando, Organometallics, 2002,21,5820. loo' J. Wolowska, G.R. Eastham, B.T. Heaton, J.A. Iggo, C. Jacob and R. Whyman, Chem. Commun., 2002,2784. 1o08 C. Bianchini, H.M. Lee, A. Meli, W. Oberhauser, M. Peruzzini and F. Vizza, Organometallics, 2002,21,16;C. Bianchini, A. Meli, G. Muller, W. Oberhauser and E. Passaglia, Organometallics, 2002,21,4965. loo9 L. Canovese, F. Visentin, G. Chessa, C. Santo, P. Uguagliati and G. Bandoli, J . Organomet. Chem., 2002,650,43. l o l o E. Galardon, S. Ramdeehul, J.M. Brown, A. Cowley, K.K. Hii and A. Jutand, Angew. Chem., Int. Ed. Engl., 2002,41, 1760. lo'' F. Stohr, D. Sturmayr, G. Kickelbick and U. Schubert, Eur. J. Inorg. Chem., 2002,2305. lo'' H.A. Zhong, J.A. Labinger and J.E. Bercaw, J . Am. Chem. Soc., 2002,124,1378. l o l 3 R. Romeo, L.M. Scolaro, M.R. Plutino, A. Romeo, F. Nicolo and A. Del Zotto, Eur. J . Inorg. Chem., 2002,629. J.M. Seul and S. Park, J. Chem. Soc., Dalton Trans., 2002,1153. '01' W.A. Herrmann, P. Harter, C.W.K. Gstottmayr, F. Bielert, N. Seeboth and P. Sirsch, J. Organomet. Chem., 2002,649,141. H.S. Sorensen, J. Larsen, B.S. Rasmussen, B. Laursen, S.G. Hansen and T. Skrydstrup, Organometallics, 2002,21, 5243. A. Ohtaka, N. Kato and H. Kurosawa, Organometallics, 2002,21,5464. C. Muller, R.J. Lachicotte and W.D. Jones, Organometallics, 2002,21, 11 18. lo'' H.K. Cotton, R.C. Verboom, L. Johansson, B.J. Plietker and J.-E. Backvall, Organometallics, 2002,21, 3367. l o Z o H. Yasuda, J.-C. Choi, S.-C. Lee and T. Sakakura, Organometallics, 2002,21,1216.
79
complexes has been determined by NMR spectroscopy.'021'H NMR spectroscopy has been used to follow the binding of ~is-[Pd(en)(OH~)~]~+ to val-ile-hisasn.1022 The hydrolysis of cis-[PtCl2(NH3)(NC5H4-2-CH$H20H)] has been followed by 'H NMR spectroscopy. The "N NMR spectrum was also reported. 1023 The reactions of carboplatin with L-selenomethionine have been followed by 'H,"N HSQC NMR spectroscopy.'024The reaction of a cationic dinuclear platinum anticancer drug with glutathione has been studied in detail by 195Pt NMR s p e c t r o s ~ o p y . The ~ ' ~ ~ reaction of compounds such as [{cisPt(NH3)2}2(pOH)(ppz)]with 9-ethylguanine has been monitored by 'H NMR spectroscopy. The '95PtNMR spectrum was also reported.'026 The interaction of a cis-dichloroaminopyrrolidine Pt" complex with poly(1)-poly(C)has been studied by 'H NMR s p e c t r o s ~ o p y . ' ~ ~ ~ reactions of trans-[PtCl{(E)The HN = C(OMe)Me}2]with a series of rib0 and deoxyribodinucleotides,"** and guanosine 5'-monopho~phate,'~~~been studied by 'H,"N HMQC. A crosshave over experiment between [Pd2C12(S,S-iproxp)z] [Pd2C12(R,R-iproxp)2] and has been followed by 'H NMR spectroscopy.'030The catalysis of Diels-Alder reaction by [(dppe)Pt(OTf)2]and [(R-BINAP)Pt(OTf)2] been studied by 'H and has 31PNMR spectroscopy.'0313*P NMR spectroscopy has been used to examine 1032 the reaction of [(Ph3P)2Pt(p-SCH2CH2S)Rh(q4-cod)]. The reaction of [(dppe)Pt(p-S)zPt(dppe)]with CH2C12has been followed by 'H, 13C and "P NMR spectroscopy.1033 Treatment of pyridine-2-thiol with D2in the presence of Pd" and Pt" dinuclear complexes of 5-methylpyridine-2-thiolate has been followed by 'H NMR spectroscopy.1034
(125)
1021 SO22 SO23
(126)
(127)
1024 1025 1026
1027 1028 1029 1030 1031 1032
1033
1034
N.M. MiloviE and N.M. Kostic, J. Am. Chem. SOC.,2002,124,4759. N.M. MiloviE and N.M. Kostic, Inorg. Chem., 2002,41,7053. A.C.G. Hotze, Y. Chen, T.W. Hambley, S. Parsons, N.A. Kratochwil, J.A. Parkinson, V.P. Munk and P.J. Sadler, Eur. J. Znorg. Chem., 2002, 1035. Q. Liu, J. Lin, P.J. Jiang, J.Y. Zhang, L.G. Zhu and Z.J. Guo, Eur. J. Inorg. Chem.,2002,2170. B.A.J. Jansen, J. Brouwer and J. Reedijk, J. Inorg. Biochem., 2002,89, 197. S. Komeda, M. Lutz, A.L. Spek, Y. Yamanaka, T. Sato, M. Chikuma and J. Reedijk, J. Am. Chem. SOC.,2002,124,4738. M. Vives, R. Tauler, V. Moreno and R. Gargallo, Anal. Chim. Acta, 2001,446,439. Y.Z. Liu, J. Vinje, C. Pacifico, G. Natile and E. Sletten, J. Am. Chem. SOC.,2002, 124, 12 854. Y.Z. Liu, F.P. Intini, G. Natile and E. Sletten, J. Chem. SOC.,Dalton Trans., 2002, 3489. C. Mazet and L.H. Gade, Chem.-Eur. J.,2002,8,4308. N.M. Brunkan and M.R. Gagne, Organometallics, 2002,21, 1576. J. Fornies-Camer, A.M. Masdeu-Bulto, C. Claver, C. Tejel, M.A. Ciriano and C.J. Cardin, Organometallics, 2002,21,2609. R. Mas-Balleste, M. Capdevila, P.A. Champkin, W. Clegg, R.A. Coxall, A. Lledos, C. Megret and P. Gonzalez-Duarte, Inorg. Chem., 2002,41,3218. K. Umakoshi, T. Yamasaki, A. Fukuoka, H. Kawano, M. Ichikawa and M. Onishi, Znotg. Chem., 2002,41,4093.
80

+
3.4.21 Gold. The decomposition of [O{AU(PP~~>}~] been studied by has 31P{1H} NMR spectroscopy.'035 3.4.22 Mercury. 'H NMR spectroscopy has been used to follow the reaction of [Hg(C6H5Me)2(GaC14)2] C6D6.036 with
'
3.4.23 Boron. "B NMR spectroscopy has been used to follow the reaction of [H3BSMe2] with 1 - h e ~ e n e . l 'The reaction of [B3H8]- with B2H6 has been ~~ studied by "B NMR s p e c t r o s ~ o p y . 'The~transformation of [(Me2S)B9H13] ~~ with PriNH2 to [(PriNH2)B8HllNHPri] has been investigated by "B NMR s p e c t r o s ~ o p y . '"B~NMR spectroscopy has been used to examine the reaction ~ ~ of closo-[3-Co(~S-NC4H4-1,2-C2B9H11)] with [(Et20)BF3]. '040 The stoichiometric reaction of [B(C6Fs)3] and NEt2Ph has been investigated by 'H, 'lB, 13C,I5N The and I9F NMR spectros~opy.'~~' stepwise conversion of [(F2B)3BCO] to [(C12B)3BCO] treatment with [BC13] has been followed by "B NMR spectroby scopy. 042 3.4.24 Aluminium. 'H NMR spectroscopy has been used to follow the reaction of [RA1(2,6-Pr'2C6H3NCH2CH2CH2NC6H3-2,6-Pri2)] with E-caprolactone.' 043 3.4.25 Indium. 'H NMR spectroscopy has been used to follow the reaction of [(C5H5)31n] with [(CSHS)In].'044 3.4.26 Silicon. CIDNP has been observed when [R3MCH2CH= CHJ, M = Si, Sn, reacts with [(Me3Si)2NBr].'045The reaction of (128) with KH has been monitored by 29SiNMR spectroscopy.1046The reaction of HN(SiMe3)2with (R)-(H0)2C20Hlo(SiMe3)2-3,3'the presence of [Ge{ N(SiMe3)2}2] been folin has lowed by 'H NMR s p e c t r o s ~ o p y .The cyclisation of a,w-HO(SiMe20),H and '~~~ purification has been monitored by 29SiNMR s p e c t r o s ~ o p y . '13C~ 29Si ~ ~ and NMR spectroscopic studies of the hydrolysis of [Me2Si(OEt)2]have been reported.' 049 The hydrolysis and condensation of silanes have been studied by 29Si
1035 1036 1037
1038
1039
1040 1041 1042 1043 1044
1045
1046 1047 1048
M. Bardaji, P. Uznanski, C. Aniens, B. Chaudret and A. Laguna, Chem. Commun., 2002,598. C.S. Branch and A.R. Barron, J. Am. Chem. SOC.,2002,124,14 156. B.B. Busch, M.M. Paz, K.J. Shea, C.L. Staiger, J.M. Stoddard, J.R. Walker, X.Z. Zhou and H.D. Zhu, J. Am. Chem. SOC.,2002,124,3636. L.A. Gavrilova, L.V. Titov, P.V. Petrovskii and N.T. Kuznetsov, Zh. Neorg. Khim., 2002, 47, 155. M.E. El-Zaria, U. Dorfler, M. Hofmann and D. Gabel, Angew. Chem., Int. Ed. Engl., 2002,41, 4498. J. Llop, C. Viiias, F. Teixidor and L. Victori, J. Chem. SOC.,Dalton Trans., 2002,1559. N. Millot, C.C. Santini, B. Fenet and J.M. Basset, Eur. J. Znorg. Chem., 2002,3328. J.A.J. Pardoe, N.C. Norman and P.L. Timms, Polyhedron, 2002,21,543. D. Chakraborty and E.Y.X. Chen, Organometallics, 2002,21,1438. O.T. Beachley, jun., D.J. MacRae, A.Y. Kovalevsky, Y.G. Zhang and X. Li, Organometallics, 2002,21,4632. M.B. Taraban, A.I. Kruppa,N.E. Polyakov, M.G. Voronkov, V.I. Rakhlin, S.V. Grigor'ev,O.S. Volkova, R.G. Mirskov and T.V. Leshina, J. Organomet. Chem., 2002,658,228. K. Naganuma and T. Kawashima, J. Organomet. Chem., 2002,643,504. C.S. Weinert, P.E. Fanwick and I.P. Rothwell, J. Chem. SOC.,Dalton Trans., 2002,2948. B.M. White, W.P. Watson, E.E. Barthelme and H.W. Beckham, Macromolecules, 2002,35,5345.
81
NMR spectroscopy.1050I3Cand 27Al NMR spectroscopy has been used to study the formation of zeolite A.'05'
5if3
/
P i
) -
But
3.4.27 Tin.The reaction of (129) with Li has been monitored by l19Sn NMR spectroscopy.' 0 5 2 The reaction of [Bu3SnCR= CHOEt] with MeCOBr has been investigated by 'H, I3C and '19Sn NMR s p e c t r o s ~ o p y . 'The ~ ~ ~ reaction of aheterosubstituted alcohols with one equivalent of p-tosyl chloride and one equivalent of Et3Nin the presence of [Bun2SnO]has been studied by 'I9SnNMR spectroscopy. 054
Ph
Ph
Ph
Ph
(129)
3.4.28 Nitrogen. 'H NMR spectroscopy has been shown to be a versatile and economical tool for monitoring reaction kinetics in ionic liquids. ' O S 5 3.4.29 Phosphorus. Stereomutation and apicophilicity of diastereomeric spirophosphoranes have been studied by NMR spectroscopy. 1056 The equilibrium in Scheme 16 has been followed by 31P NMR ~ p e ~ t r ~ ~ ~ NMR y . ' ~ ~ 31P ~ p spectroscopy has been used to follow the photolysis of [2,6-(2,4,6Me3C&)*C6H3P = PMe1].'058 The amination of [C1P(p-NBut)l2with NH3 has been followed by 31P NMR spectroscopy.
'
1049 1050
1051 1052 1053 1054
1055 1056
1057
1058 1059
M.-F. Tsai, Y.-D. Lee and K.-N. Chen, J. Appl. Polym. Sci., 2002,86,468. N. Moszner, T. Volkel, S.C. Von Clausbruch, E. Geiter, N. Batliner and V. Rheinberg, Macromol. Muter. Eng., 2002,287, 339. M. Smaihi, S. Kallus and J.D.F. Ramsay, Stud. Surf. Sci. Catal., 2001, 135, 271. M. Saito, R. Haga and M. Yoshioka, Chem. Commun., 2002,1002. T. Iebl, J. Holecek, M. Dymak and D. Steinborn, Collect. Czech. Chem. Commun., 2002,67,587. M.J. Martinelli, R. Vaidyanathan, J.M. Pawlak, N.K. Nayyar, U.P. Dhokte, C.W. Doecke, L.M.H. Zollars, E.D. Moher, V. Van Khau and B. Kosmrlj, J. Am. Chem. SOC., 2002,124,3578. A, Durazo and M.M. Abu-Omar, Chem. Commun., 2002,2002,66. M. Nakamoto, S. Kojima, S. Matsukawa, Y. Yamamoto and K. Akiba, J. Organornet. Chem., 2002,643,441 . S . Matsukawa, K. Kajiyama, S. Kojima, S. Furuta, Y. Yamamoto and K. Akiba, Angew. Chem., Int. Ed. En& 2002,41,4718. R.C. Smith, S. Shah and J.D. Protasiewicz, J. Organomet. Chem., 2002,646,255. A. Bashall, A.D. Bond, E.L. Doyle, F. Garcia, S. Kidd, G.T. Lawson, M.C. Parry, M. McPartlin, A.D. Woods and D.S. Wright, Chem.-Euur.J.,2002,8, 3377.
82
3.4.30 Selenium. The synthesis of azetidine and pyrrolidine derivatives through selenium-inducedcyclization of secondary homoallylamines has been studied by 77SeNMR spectroscopy.'060 "Se NMR studies of the redox behaviour of Na2Se03 the presence of peroxynitrite and H202/02 have been reported.'061 in
3.4.31 Tellurium. *25Te NMR spectroscopy has been used to follow the reaction of [Te(OPr')4] with HOCH2CH2NMe2 to give [Te(OPr'),(OCH2CH2NMe2)4 ,I.'O6
Paramagnetic Complexes
In this section, compounds of d-block transition elements will be considered first and then those of the lanthanide and actinide elements. Papers concerning the use of paramagnetic complexes as 'shift or relaxation reagents' are usually omitted. Ten reviews have appeared: 'Magnetic susceptibility in paramagnetic NMR',' 0 6 3 'Intermolecular nuclear relaxation in paramagnetic solutions: from free radicals to rare 'NMR of paramagnetic proteins: Structure, dynamics and ~tability',''~~ 'Structural investigations of paramagnetic metalloproteins using high-resolution NMR spectroscopy. Iron-sulfur and copper proteins',1066'Nuclear magnetic resonance of paramagnetic metal centres in proteins and synthetic ~ornplexes',''~~ 'Paramagnetic resonance of biological metal centres','06* 'Asymmetric synthesis by lanthanide complexes as asymmetric catalysts', which contains various chiral NMR lanthanide shift reagents,'069 'Chiral lanthanide complexes: Coordination chemistry and applications',' 07' 'Theories of structural and dynamic properties of ions in discrete solvents. Application to magnetic resonance imaging','' ' and 'Relaxivity of gadolinium(II1) complexes: theory and mechanism'. ' Small structural changes in metalloproteins have been detected by the use of NMT pseudocontact shifts.' Closed-form expressions for level-averaged electron spin relaxation times outside the Zeeman limit have been applied to
'
Io6' lo6'
1062
X. Pannecoucke, F. Outurquin and C. Paulmier, Eur. J. Org. Chem., 2002,995.

S . Albrecht, T. Zimmerman, D. Scheller, H.D. Saeger and W. Distler, Chemiluminescence at the Turn ofthe Millennium, 2001, 15. H. Fleischer, Y.Dienes and D. Schollmeyer,Eur. J. Inorg. Chem., 2002,2073. I. Bertini, C. Luchinat and G. Parigi, Prog. Nucl. Magn. Reson. Spectrosc., 2002,40,249. E. Belorizky, P.H. Fries and S. Rast, C.R. Chim., 2001,4,825. I. Bertini and I.C. Felli, NATO Science Series, Series A: Li$e Sciences, 2001,315, 117. A.I. Dikiy, Russ. Chem. Bull., 2001,50,1762. L.-J. Ming, Phys. Methods Bioinorg. Chem., 2002,375. M. Ubbink, J.A.R. Worrall, G.W. Canters, E.J.J. Groenen and M.Huber, Annu. Reu. Biophys. Biomol. Struct., 2002,31, 393. K. Mikami, Kidorui, 2000,37,47. H.C. Aspinall, Chem. Reu., 2002,102,1807. P.H. Fries, J. Richardi, S. Rast and E. Belorizky, Pure Appl. Chem., 2001,73,1689. 8. Tbth, L. Helm and A.E. Merbach, Chemistry of Contrast Agents in Medical Magnetic Resonance Imaging, 2001,45. M. Allegrozzi, I. Bertini, S.-N. Choi, Y.-M. Lee and C. Luchinat, Eur. J. Inorg. Chem., 2002, 2121.
lo6* lo6'
lo''
1073
83
paramagnetic NMR relaxation. 1074 Metal-chelated nucleic acid binding peptides have been applied as MRI contrast agents.' 07' Paramagnetic nanoparticles have been proposed as NMR contrast agents.'076
4.1 The Transition Metals. - 4.1.1 Titanium. The positions of the 'H NMR
signals of [(q5-C5Me4R)2Ti] follow the Curie law.'077

4.1.2 Vunadium.The 'H NMR spectrum of [V,(~-O)(phen)~Cl~]~+ that the shows two vanadium ions are coupled antiferromagnetically. 078 From the temperature-dependence of the 23NaT I of [H4{ (V02)3(0CH2)3CCH20H}2(P04)4]6+, the value of the two gaps separating the lower energy total spin states has been determined.'079 'H NMR data have also been reported for [(PhN = CMeCMe = NPh)VC12(THF)],'080and [(12-ane-P3Et3)VC13].'08'
4.1.3 Chromium. The signs of the NMR shifts of [(q5-C5H5)Cr(CNMe)4]2+ have established negative spin density in the cyclopentadienyl x-systems. 1082 The 'H and 'H NMR resonances of [Cr(salen)Cl] type complexes have been assigned.' 083 NMR data have also been reported for [Cr{(CNC5H4-q5)Fe(q5CsH5)}6]"+, n = 1, 2, 084 [HB(3,5-Me2pz)3Cr(N2C3HMeBut)], I o 8 [Ln+ and Cr"L315+, = ( 130),1086 [Cr1209(0H)3(pivalate)~5].'087 L
'
4.1.4 Molybdenum and Tungsten. NMR data have also been reported for [Fe(OHz)P2W~2M0506,]7+,1 O8 a-[P2w17061MI, 'O 8 and [(SCH2CH2S)2Mo2Fe4S9I3-. '090
R. Sharp, J. Magn. Reson., 2002,154,269. S.L. Mills and J.L. Mills, U.S. Pat. Appl. Publ., 2002, 9 pp., Us 2002155576, A l , 20021024. Application: 2001-774940,20010131. 1076 S. Haubold, C. Bobbert, M. Haase and B.M. Stoeckelhuber, Ger. Ofen., 2002, 10 pp., De 10111321, Al, 20020523. Application: 2001-101 11321,20010308. 1 0 7 7 L. Lukeiova, M. HoraCek, P. Stipnieka, K. Fejfarova, R. Gyepes, I. Cisafova, J. Kubiita and K. Mach, J. Organomet. Chem., 2002,663,134. lo'' H. Kumagai, S. Kitagawa, M. Maekawa, S. Kawata, H. Kiso and M. Munakata, J. Chem. SOC., Dalton Trans., 2002,2390. 1079 J.K. Jung, D. Procissi, Z.H. Jang, B.J. Suh, F. Borsa, M. Luban, P. Kogerler and A. Muller, J. Appl. Phys., 2002,91,7391. S . Milione, G. Cavallo, C. Tedesco and A. Grassi, J . Chem. Soc., Dalton Trans., 2002, 1839. l o 8 ' R.J. Baker, P.C. Davies, P.G. Edwards, R.D. Farley, S.S. Liyanage, D.M. Murphy and B. Yong, Eur. J . Inorg. Chem., 2002, 1975. l o 8 * O.M. Heigl, E. Herdtweck, S. Grasser, F.H. Kohler, W. Strauss and H. Zeh, Organometallics, 2002,21, 3572. K.P. Bryliakov, M.V. Lobanova and E.P. Talsi, J. Chem. Soc., Dalton Trans., 2002,2263. 1084 M.V. Barybin, T.C. Holovics, S.F. Deplazes, G.H. Lushington, D.R. Powell and M. Toriyama, J. Am. Chem. SOC.,2002,124,13 668. 1085 K. Qin, C.D. Incarvito, A.L. Rheingold and K.H. Theopold, Angew. Chem., Int. Ed. Engl., 2002, 41,2333. M. Cantuel, G. Bernardinelli, D. Imbert, J.C.G. Bunzli, G. Hopfgartner and C. Piguet, J. Chem. SOC.,Dalton Trans., 2002, 1929. lo8' A.C. Royer, R.D. Rogers, D.L. Arrington, S.C. Street and J.B. Vincent, Polyhedron, 2002, 21, 155. f o S 8 R. Belghiche, R. Contant, Y.W. Lu, B. Keita, M. Abbessi, L. Nadjo and J. Mahuteau, Eur. J. Inorg. Chem., 2002,1410. R. Contant, M.Richet, Y.W. Lu, B. Keita and L. Nadjo, Eur. J. Inorg. Chem., 2002,2587. lo90 H.C. Zhou, W.P. Su, C. Achim, V.P. Rao and R.H. Holm, Inorg. Chem., 2002,41,3191.
1074
1075
84
4.1.5 Manganese. Tl and T2 NMR dispersion profiles for a new manganese
porphyrin have been reported."" 'H and 170 relaxometric investigations of the binding of Mn2+to human serum albumin have been p ~ b 1 i s h e d . l 'NMR data ~~ have also been reported for dimanganese(II1) complexes of 1,5-bis(Xand [M n403( NO3)( 02CMe)3( PhCOCHsalicy1idenamino)pentan-3-01, ' COPh)3].'094
4.1.6 Rhenium. NMR data have been reported for [Re{Ir(SCH2CH2NH2)3}2]3 O 9 and [ReC13L]. O 9 ,
+
' '
'
4.1.7 Iron. The different substituents in a series of complexes, [(ArNCMeCHCMeNAr)Fe{N(SiMe3),},], have allowed the assignment of their paramagnetically shifted 'H NMR The results of variable-temperature 'H NMR spectra of lattice-dictated conformers in bis(pyrazoly1)pyridine-basedFe" complexes support the presence of high-spin and low-spin forms.1o98The 'H NMR spectrum of bis(N-Pr'-sa1icylaldiminato)Fe"exhibits six paramagnetically shifted ligand resonances ranging from + 195 to - 3 1 ppm that are consistant with a mononuclear high spin ( S = 2) Fe" complex in solution.'099 19F Isotropic shifts in paramagnetic Fe"' octaethyltetraphenylporphyrinate complexes have been analysed. ''Oo The spin states of mono(imidazo1e)-ligated { meso-(2,4,6Me4C6H2)4-porphyrinato}Fe1'' been studied using ' H and I3C NMR spechave
L.H. Bryant, jun. and G.A. Mercier, jun., International Journal o Molecular Sciences [online f 140. computer J; le], 2001,2, http://www.mpdi.org/ijms/papers/i2030140.pdf. S . Aime, S . Canton, S.G. Crich and E . Terreno, Magn. Reson. Chem., 2002,40,41. C. Palopoli, M. Gonzalez-Sierra, G. Robles, F. Dahan, J.P. Tuchagues and S . Signorella, J . Chem. SOC.,Dalton Trans., 2002,3813. G. Aromi, S. Bhaduri, P. Artus, K. Folting and G. Christou, Inorg. Chem., 2002,41,805. N. Mahboob, Y. Miyashita, Y. Yamada, K. Fujisawa and K. Okamoto, Polyhedron, 2002,21,
1092
1094
1095
1809. S.R. Banerjee, L.H. Wei, M.K. Levadala, N. Lazarova, V.O. Golub, C.J. O'Connor, K.A. Stephenson, J.F. Valliant, J.W. Babich and J. Zubieta, Inorg. Chem., 2002,41,5795. '0 9 7 A. Panda, M. Stender, R.J. Wright, M.M. Olmstead, P. Klavins and P.P. Power, Inorg. Chem., 2002,41,3909. lo9' P . Manikandan, K. Padmakumar, K.R.J. Thomas, B. Varghese, H. Onodera and P.T. Manoharan, Inorg. Chem., 2002,41,6930. 1 0 9 9 M.A. Torzilli, S . Colquhoun, J. Kim and R.H. Beer, Polyhedron, 2002,21,705. "''L. Yatsunyk and F.A. Walker, Inorg. Chim. Acta, 2002,337,266.
' 0 9 ~
85
troscopy. l o ' The spin distribution in low-spin iron porphyrins has been determined."02 The first detailed investigation of the 'H, 13C,''N and 19F NMR shifts in paramagnetic metalloporphyrins and metalloproteins has been reported. The effects of solvents on the electronic configurations of the low-spin [(NC)2Fe{5,10,15,20-(2,4,6-Et3C6H2)4-porphyrinato}] been studied using have 'H and I3C NMR s p e c t r o s ~ o p y . ~The interaction of anions with '~~ [Fe{ 5,10,15,20-(C6F5)4-porphyrinato}] been correlated with 'H chemical has shifts."05 'H NMR spectroscopy has been used to study O2 binding to Fe" porphyrins.' The variable temperature 'H NMR spectra of five-coordinate Fe'" 2,7,12,17-tetrapropylporphycene demonstrate anti-Curie behaviour. The transient complex of bovine myoglobin and cytochrome b5 has been investigated using a combination of NMR chemical shift mapping and 15Nrelaxation data.' The solution structure of cyanoferricytochrome c has been determined using NMR spectroscopy.llo9 99% of all the prolines have been assigned in the 15N NMR spectra of a monoheme ferrocytochrome c."" 13C NMR spectroscopy has been used to detect the 13CN signal of cyanide attached to heme proteins."" NMR data have been used to model the Fe"-bleomycin three13C} two-dimensional NMR spectroscopy has dimensional structure.' 'l 2 13C{ been introduced as a new strategy for the study of paramagnetic proteins.''l3 Iron oxide solution has been examined as a contrast agent for MRI,'114 and has been applied to 23NaMRI in myocardial infarction."" The effect of pH on the NMR dispersion of ferritin and ferritin-like magnetic particle solutions has been investigated.1116A 'H NMR investigation of the spin dynamics of [Fe3(p3OH)(H2L)3(HL)3], H3L = orotic acid, has been reported.' The spin dynamics in a tetranuclear Fe"' cluster have been examined. ' * NMR data have also been l9 reported for [(q5-C5H5)4Fe4(HC2H)2],1 Fe"'-corrolate,' I2O [((OC),Fe(p,q2A. Ikezaki and M. Nakamura, Inorg. Chem., 2002,41,6225. M.P. Johansson, D. Sundholm, G. Gerfen and M. Wikstrom, J. Am. Chem. Soc., 2002,124, 11 771. I o 3 J.H. Mao, Y. Zhang and E. Oldfield, J. Am. Chem. Soc., 2002,124,13 91 1. 1104 A. Ikezaki and M. Nakamura, Inorg. Chem., 2002,41,2761. " 0 5 B. Song, B. Park and C. Han, Bull. Korean Chem. Soc., 2002,23,119. l o 6 R.A. Ghiladi and K.D. Karlin, Inorg. Chem., 2002,41,2400. ' I o 7 K. Rachlewicz, L. Latos-Graiynski, E. Vogel, Z. Ciunik and L.B. Jerzykiewicz, Inorg. Chem., 2002,41, 1979. "08 J.A.R. Worrall, Y. Liu, P.B. Crowley, J.M. Nocek, B.M. Hoffman and M. Ubbink, Biochemistry, 2002,41,11 721. l o 9 Y. Yao, C. Qian, K. Ye, J. Wang, Z. Bai and W. Tang, JBIC, J . Biol. Inorg. Chem., 2002,7,539. l 1l o I. Bartalesi, I. Bertini, P. Hajieva, A. Rosato and P.R. Vasos, Biochemistry, 2002,41,5112. H. Fujii, J. Am. Chem. Soc., 2002,124, 5936. " T.E. Lehmann, JBIC, J. Biol. Inorg. Chem., 2002,7,305. T.E. Machonkin, W.M. Westler and J.L. Markley, J. Am. Chem. Soc., 2002,124,3204. l4 J. Qian, K. Yang, W. Fan, J. Song, C. Wang, M. Hu and Y. Pen, Hejishu, 2001,24,487; K.-C. Yu, Y. Zhang, Y.-H. Yang, G. Lu, M.-L. Liu and C.-H. Ye, Bopuxue Zazhi, 2002,19,143. l1 C.D. Constantinides, J. Rogers, D.A. Herzka, F.E. Boada, D. Bolar, D. Kraitchman, J. Gillen and P.A. Bottomley, Magn. Reson. Med., 2001,46,1164. l 1 l 6 Y. Gossuin, A. Roch, F. Lo Bue, R.N. Muller and P. Gillis, Magn. Reson. Med., 2001,46,476. l 1l 7 M. Fardis, G. Diamantopoulos, M. Karayianni, G. Papavassiliou, V. Tangoulis and A. Konsta, Phys. Rev. B: Condens. Matter Muter. Phys., 2002,65,014412/1. "18 D. Procissi, B.J. Suh, A. Lascialfari, F. Borsa, A. Caneschi and A. Cornia, J . Appl. Phys., 2002, 91,7173. '9 I M. Okazaki, T. Ohtani, M. Takano and H. Ogino, Inorg. Chem., 2002,41,6726.
'lo'
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'
86
C02R)3}2Fe],1'21 [{ (q'-C5H5)Ni[q5-CsH3- SiMe2)21,2-( 1,2-q5-CsH3]}2Fe], (29si)9' [Fe"{ trans- 1,2-(NC5H4-2-CH2NMe)2C6H lo)(NCCD3)2I2+,' ' [Fe{ 2,6-[(C5H4N-2)2methoxymethane]2pyridine} LIZ 124 FeC12 complexes of (NCsH4-2-CH2)3N,' FeC13adduct of N-isopropylsalicylaldimine,'126 cationic l2 2,6-bis(imino)pyridine iron and cobalt complexes,' chloroiron mesotriphenylcorrolates,1'28 Fe"' and Fe'" corro1es,'l2' a highly saddle shaped (porphyrinato) Fe'" iodide,' Fell' complexes of mono meso substituted octaethylporphyrins,' '31 five-coordinatedhalide ligated Fe"' porphyrin, porphycene and corrphycene complexes,' 1 3 2 [Fe{ 5,1,0,15,20-(4-N02C6H4coN)4porphyrin}C1],"33 Fe"' complexes of 5-HO-10,15,20-Ph3porphyrin,'134 superstructured Fe"' porphyrins,' 135 antimalarial drug-heme complexes,' '36 Fe complexes of 5,10,15,20-Ph4-2l-oxaporphyrin,' '37 [Fe(meso-Pb-chlorinate)(1-Meimida~ole)~] +,1138 the heme prosthetic group of mammalian laca toperoxidase,1'39 15Nlabelled cytochrome c3, (15N),"40 novel histidine-heme covalent linkage in a hemoglobin, ("N),' 14' heme peroxidase,''42 models of the low-spin Fell' hydroperoxide intermediate of heme oxygenase,' 143 a gallium complex of azoverdin,' 144 purple acid p h ~ s p h a t a s e , " ~[(THF)NaFe~
+
,'
'
1120
1121
1122 1123 1124 1125 1126
1127
1128
1129 1130 1131
1132
1133
1134 1135 1136
1137 1138 1139 1140
1141 1142
1143
1144 114s
0. Zakharieva, V. Schunemann, M. Gerdan, S. Licoccia, S. Cai, F.A. Walker and A.X. Trautwin, J. Am. Chem. Soc., 2002,124,6636. N. Le Gall, D. Luart, J.Y. Salaun, J. Talarmin, H. des Abbayes, L. Toupet, N. Memendez and F. Varret, Organometallics, 2002,21, 1775. M. Herker, F.H. Kohler, M. Schwaiger and B. Weber, J. Organomet. Chem., 2002,658,266. M. Costas and L. Que, Angew. Chem., Znt. Ed. Engl., 2002,41,2179. C.R. Goldsmith, R.T. Jonas, A.P. Cole and T.D.P. Stack, Inorg. Chem., 2002,41,4642. D. Mandon, A. Machkour, S. Goetz and R. Welter, Znorg. Chem., 2002,41, 5364. J.L. Kisko, M.A. Torzilli, K. Liu, A.E. McDermott and R.H. Beer, Znorg. Chem. Commun., 2002, 5,283. G.J.P. Britovsek, V.C. Gibson, S.K. Spitzmesser, K.P. Tellmann, A.J.P. White and D.J. Williams, J. Chem. Soc., Dalton Trans., 2002,1159. S . Cai, S. Lococcia, C. DOttavi, R. Paolesse, S. Nardis, V. Bulach, B. Zimmer, T.K. Shokhireva and F.A. Walker, Inorg. Chim. Acta, 2002,339, 171. L. Simkhovich, I. Goldberg and Z. Gross, Znorg. Chem., 2002,41,5433. M. Nakamura, T. Ikeue, Y. Ohgo, M. Takahashi and M. Takeda, Chem. Commun., 2002,1198. H. Kalish, J.E. Camp, M. Stqpien, L. Latos-Graiynski, M.M. Olmstead and A.L. Balch, Znorg. Chem.,2002,41,989. Y. Ohgo, S. Neya, T. Ikeue, M. Takahashi, M. Takeda, N. Funasaki and M. Nakamura, Znorg. Chem., 2002,41,4627. C.-H. Chen, Y.-Y. Lee, B.-C. Liau, S. Elango, J.-H. Chen, H.-Y. Hsieh, F.-L. Liao, S.-L. Wang and L.-P. Hwang, J. Chem. Soc., Dalton Trans., 2002, 3001. J. Wojaczyski, M. Stepien and L. Latos-Graiynski, Eur. J. Inorg. Chem., 2002,1806. H.R. Jimenez, J.M. Moratal and B. Loock, New J. Chem., 2002,26,323. A. Leed, K. DuBay, L.M.B. Ursos, D. Sears, A.C. de Dios and P.D. Roepe, Biochemistry, 2002, 41,lO 245. M. Pawlicki and L. Latos-Grazynski, Inorg. Chem., 2002,41,5866. G. Simonneaux, M. Kobeissi and L. Toupet, J. Chem. Soc., Dalton Trans., 2002,401 1. S.D. Zbylut and J.R. Kincaid, J. Am. Chem. Soc., 2002,124,6751. A. Kim, 1.-C. Jeong, Y.-B. Shim, S.-W. Kang and J.-S. Park, Bull. Korean Chem. Soc., 2001,22, 1197. B.C. Vu, A.D. Jones and J.T.J. Lecomte, J. Am. Chem. Soc., 2002,124,8544. J.S. de Ropp, S. Sham, A. Asokan, S. Newmyer, P.R.O. de Montellano and G.N. La Mar, J. Am. Chem. Soc., 2002,124,11029. M. Rivera, G.A. Caignan, A.V. Astashkin, A.M. Raitsimring, T.K. Shokhireva and F.A. Walker, J. Am. Chem. Soc., 2002,124,6077. E. Wasielewski, R.A. Atkinson, M.A. Abdallah and B. Kieffer, Biochemistry, 2002,41,12 488. A. Dikiy, E.G. Funhoff, B.A. Averill and S. Ciurli, J. Am. Chem. Soc., 2002,124,13 974.
87
(OBU')~]~,' 146 [Fe4(OHO)(OH),(02CMe)4(phen)4]3+,1147 [(HBpz3)VFe3S4C13]-,' 148 and [(HBpz3)MoFe3S4C13]-.' 149

4.1.8 Ruthenium. A chiral dichlororuthenium(1V)porphyrin catalyst has been characterised by 'H NMR spectroscopy.' 5 0
4.1.9 Cobalt. Paramagnetic Co" has been used as a probe for kinetic and NMR relaxation studies of phosphate binding and catalytic mechanism of Streptomyces dinuclear aminopeptidase.' ' ' NMR data have also been reported for (131),1'52 [{ B ( ~ - C ~ H ~ - P Z ) ~ } ~ C O ] , " ~ ~ [{B(~-C~H~-PZ)~)(HBPZ~)CO],' lS4 CO" complexes of poly(ary1ester) dendrimer porphyrins,' linear pentacobalt complexes of N,N'-bis(pyridyl)-2,6-diaminopyridineligands,' 5 6 Co" complexes of a pyridine containing self-assembling system,' ' a Co" complex of a helical peptide,1158 [PhB(CH2PPh2)3Co(p-Br)]2,' and [ C O ~ ( S P ~ ) ~160 ~ - . ' 159 ~]
(131) 4.1.10 Nickel. Peculiarities of NMR spectra of heterospin complexes have been
investigated using a Ni2+complex with a stable nitroxide."61 NMR data have also been reported for (132),"62 Ni" pseudoazurin,' '6 3 and [Ni{ Bu'N(Se)P(pNBU')~PNHBU'}~], ("Se).' 164
1146 1147
1148 1149 1150 1151 1152
1153
1154 115s 1156
1157
1158 1159
1160 1161
1162
1 I63
1164
Y.K. Gun'ko, U. Cristmann and V.G. Kessler, Eur. J. Znorg. Chem., 2002, 1029. A.K. Boudalis, N. Lalioti, G.A. Spyroulias, C.P. Raptopoulou, A. Terzis, A. Bousseksou, V. Tangoulis, J.-P. Tuchagues and S.P. Perlepes, Inorg. Chem., 2002,41,6474. C. Hauser, E. Bill and R.H. Holm, Znorg. Chem., 2002,41,1615 D.V. Fomitchev, C.C. McLauchlan and R.H. Holm, Znorg. Chem., 2002,41,958. R. Zhang, W.-Y. Yu, K.-Y. Wong and C.-M. Che, J. Org. Chew., 2001,66,8145. M.N. Harris, C.M. Bertolucci and L.-J. Ming, Znorg. Chem., 2002,41, 5582. P.L. Holland, T.R. Cundari, L.L. Perez, N.A. Eckert and R.J. Lachicotte, J. Am. Chem. Soc., 2002,124,14 416. A.L. Rheingold, G.P.A. Yap, L.N. Zakharov and S. Trofimenko, Eur. J . Znorg. Chem., 2002, 2335. S. Trofimenko, A.L. Rheingold and L.M.L. Sands, Znorg. Chem., 2002,41, 1889. M. Uyemura and T. Aida, J. Am. Chem. Soc., 2002,124. 11 392. C.Y. Yeh, C.H. Chou, K.C. Pan, C.C. Wang, G.H. Lee, Y.O. Su and S.M. Peng, J. Chem. Soc., Dalton Trans., 2002,2670. A. Moghimi, M. Ranjbar, H. Aghabozorg, F. Jalali, M. Shamsipur and K.J. Chadha, Can. J. Chew., 2002,80,1687. M.Gochin, V. Khorosheva and M.A. Case, J. Am. Chem. Soc., 2002,124, 11 018. D.M. Jenkins, A.J. Bilio, M.J. Allen, T.A. Betley and J.C. Peters, J. Am. Chem. Soc., 2002,124, 15 336. Z. Cui and R.A. Henderson, Znorg. Chem., 2002,41,4158. R.Z. Sagdeev, V.K. Voronov, A.V. Podoplelov, I.A. Ushakov, A.N. Chemezov, E.Y. Fursova, S.V. Fokin, G.V. Romanenko, V.A. Reznikov and V.I. Ovcharenko, Russ. Chew. Bull., 2001,50, 2078. I. Schmidt and P.J. Chrnielewski, Chern. Commun., 2002,92. C. Dennison and K. Sato, Inorg. Chem., 2002,41,6662. F. Chivers, M.Krahn and G. Schatte, Znorg. Chem., 2002,41,4348.
88
Spectroscopic Properties o Inorganic and Organometallic Compounds f Ph
Ph
Ph
Ph
4.1 .I 1 Copper. A correlation involving 'H NMR spectra and exchange coupling constants of a family of phenoxo-bridged macrocyclic dicopper(I1) complexes has been reported.' 1 6 5 19FNMR spectroscopy has been used as a versatile tool to control the synthesis of heteronuclear Cu"-Zn" complexes.' 166 A general method for determining the electron self-exchange rates of blue copper proteins by TImeasurements has been described.' 1 6 7 NMR data have also been reported for Cu" clotrimazole Complexes,' Cu" complexes of a calix[4]arene-based [Cu{ N-(2,5podand which incorporates two 2,2'-bipyridine ligands,' But~C~H3)salicylaldiminato}2],1Cu"-pseudoazurin and Cu"-rusticyanin.' ' ' '7 0
"'
4.2 Complexes of the Lanthanides and Actinides. - 4.2.1 Lanthanides. The investigation of the NMR relation rate dose-response of a ceric sulfate dosimeter has been achieved by adding copper sulfate.' 7 2 The ligand field parameters have been determined for Tb, Dy, Ho, Er, Tm and Yb complexes of phthalocyanines by fitting 'H paramagnetic shifts.' 173 Paramagnetic NMR spectra of triple-helical lanthanide complexes with 2,6-dipicolinic acid have been re-analysed.' '74 The structures of lanthanide complexes of the py2N6Ac4 ligand containing four carboxylate pendant arms have been analysed using lanthanide induced shifts and relaxation data.' '7 5 The stoichiometry of Pr"' complexes with 1,3,5-triazacyclohexaneligands has been determined using DOSY.' '76 'H and
1165 1166
1167 1168
1169
1170 1171
1172 1173
1174
1175
S. Mohanta, B. Adhikary, S. Baitalik and K. Nag, New J. Chem., 2001,25, 1466. S . Torelli, C. Belle, I. Gautier-Luneau, S. Hamman and J.L. Pierre, Inorg. Chim. Acta, 2002,333, 144. M.R. Jensen, D.F. Hansen and J.J. Led, J. Am. Chem. Soc., 2002,124,4093. M. Navarro, E.J. Cisneros-Fajardo, T. Lehmann, R.A. Sanchez-Delgado, R. Atencio, P. Silva, R. Lira and J.A. Urbina, Inorg. Chem., 2001,40,6879. J.O. Dalbavie, J.B. Regnouf-de Vains, R. Lamartine, M. Perrin, S. Lecocq and B. Fenet, Eur. J. Inorg. Chem., 2002,901. V.T. Kasumov and F. Koksal, Spectrochim. Acta, Part A, 2002,58A, 2199. A. Donaire, B. Jimenez, C.O. Fernandez, R. Pierattelli, T. Niizeki, J.-M. Moratal, J.F. Hall, T. Kohzuma, S.S. Hasnain and A.J. Vila, J. Am. Chem. SOC.,2002,124, 13 698. S.A.J. Back, M. Lepage and C. Baldock, Appl. Radiation Isotopes, 2002,56,895. N. Ishikawa, T. Iino and Y. Kaizu, J . Am. Chem. Soc., 2002,124,11440; N. Ishikawa, T. Iino and Y. Kaizu, J . Phys. Chem. A , 2002,106,9543. N. Ouali, B. Bocquest, S. Rigault, P.Y. Morgantini, J. Weber and C. Piguet, Inorg. Chem., 2002, 41, 1436. L. Valencia, J. Martinez, A. Macias, R. Bastida, R.A. Carvalho and C . Geraldes, Inorg. Chem., 2002,41,5300.
89
1 7 0 NMR spectroscopy has been used to study the reversible binding of acetate, lactate, citrate and selected amino acids to chiral diaqua Yb, Gd and Eu The affinity of LnI" ions for 0- and mixed O-N-donor ligands has been investigated using 'H NMR spectroscopy.' 1 7 8 The Eu" cryptate, [ E u ( ~ . ~ . ~ ) ( O+H ~ ) ~ ] ~ examined as a p(Oz) responsive MRI contrast has been agent.' '79 The analysis o lanthanide induced NMR shifts using a crystal field f independent method has been applied to [Ln(DOTA)]-.'180 13CNMR spectroscopy has been used to carry out an ab initio investigation of the conformation of [Ln(DOTA)]-.' '8 1 The separation of intra- and extra-cellular lactate NMR signals has been achieved using CPr(D03A)I as a shift reagent."82 The coordination equilibrium in a Ln"' macrocyclic chelate modulated by a reversible interaction with a weak donor substituent has been investigated using 13Cand I7ONMR spectroscopy."83 The amide protons of an Yb"' DOTA tetraamide complex have been shown to act as an efficient antennae for the transfer of magnetisation to bulk water. ''84 The complexation of Ln"' with polyhydroxy carboxylic acids in aqueous solutions has been studied using 13Cpseudocontact shifts.' '8 5 Multiexponential electronic spin relaxation and Redfield's limit in Gd"' complexes have been investigated using 'H and I7O NMR spectro~ c o p y . "Water exchange on some new Gd"' MRI contrast agents has been ~~ investigated.''87 Compartmentalization of a Gd"' complex in the apoferritin cavity has been proposed as a route to obtain high relaxivity contrast agents for MRI.' '8 8 Molecular dynamics simulation of [Gd(egta)(OH2)]- has been based on I7ONMR spectroscopy and nuclear magnetic relaxation dispersion.' '8 9 A new global analysis of EPR, I7O NMR relaxation and chemical shift and 'H NMRD profiles with physically meaningful parameters for [Gd(DOTA)(OH2)]and [Gd(DTPA)(OH2)I2-have been presented.' 1 9 0 By using 'H and 1 0 7 relaxation, the effect of the internal motion of the water molecule bound to [Ln(DOTAM)(OH*)]'- has been quantified.' '9 1 Accelerating water exchange for Gd"'
R.D. Kohn, Z.D. Pan, G. Kociok-Kohn and M.F. Mahon, J . Chem. SOC., Dalton Trans., 2002, 2344. '' 7 7 R.S Dickins, S. Aime, A.S. Batsanov, A. Beeby, M. Botta, J. Bruce, J.A.K. Howard, C.S. Love, D. Parker, R.D. Peacock and H. Puschmann, J . Am. Chem. Soc., 2002,124,12 697. '17' C. Comuzzi, P. Di Bernardo, R. Portanova, M. Tolazzi and P. Zanonato, Polyhedron, 2002,21, 1385. L. Burai, R. Scopelliti and 8. Toth, Chem. Commun., 2002,2366. 10 1 ' J.M. Ren, S.R. Zhang, A.D. Sherry and C. Geraldes, Inorg. Chim. Acta, 2002,339,273. 1 1 8 1 U. Cosentino, A. Villa, D. Pitea, G. Moro, V. Barone and A. Maiocchi, J. Am. Chem. SOC., 2002, 124,4901. 1 1 8 2 S. Aime, M. Botta, V. Mainero and E. Terreno, Magn. Reson. Med., 2002,47,10. 1 1 8 3 F.A. Dunand, S. Aime, S.G. Crich, G.B. Giovenzana and A.E. Merbach, M a p . Reson. Chem., 2002,40,87. 1184 S.R. Zhang, L. Michaudet, S. Burgess and A.D. Sherry, Angew. Chem., Znt. Ed. Engl., 2002,41, 1919. "*' S. Giroux, S. Aury, B. Henry and P. Rubini, Eur. J . Znorg. Chem., 2002,1162. l'" A. Borel, F. Yerly, L. Helm and A.E. Merbach, J . Am. Chem. Soc., 2002,124,2042. 1187 M.P. Lowe, Aust. J . Chem., 2002,55,551. "" S. Aime, L. Frullano and S.G. Crich, Angew. Chem., I n t . Ed. Engl., 2002,41, 1017. 1189 F. Yerly, K.I. Hardcastle, L. Helm, S. Aime, M. Botta and A.E. Merbach, Chem.-Eur. J.,2002,8, 1031. F.A. Dunand, A. Borel and L. Helm, Znorg. Chem. Commun., 2002,5,811. '19' F.A. Dunand, A. Borel and A.E. Merbach, J. Am. Chem. SOC.,2002,124,710.
90
chelates by steric compression around the water binding site has been inves2 tigated using I7ONMR spectroscopy.''92 TI and T values have been determined for metabolite solutions containing Gd"' MRI reagents.' 193 The impact of rigidity and water exchange on the relaxivity of a dendritic MRI contrast agent has been irivestigated using "0 NMR spectroscopy.' '94 Mechanistic studies of a calcium dependent MRI contrast agent have been reported.' 195 The substituent effects on water exchange kinetics have been investigated using "0 to study bis(alky1amide)derivatives of [Gd(DTPA)(0H2)]*-.' '96 The Tl relaxation properties of Gd"' chelates with diethylenetriaminepentaacetic acid bearing vitamin B6 have been reported.' 197 MRI imaging agents containing peptide side chains have been used to study specific peptide-protein binding.' 19' A solvent 'H NMRD study of biotinylated paramagnetic liposomes containing Gd-bis-SDADTPA or Gd-DMPE-DTPA has been reported.' 99 Novel Gd"' MRI reagents have been described.1200 [Tm(DOTP)]'- has been used as a shift reagent to identify 23Na in brain,12" hearts,1202 and fibrobacter succinogenes S85.1203 Lanthanide modulation of the orientation of macromolecules induced by purple membrane has been investigated.1204The interaction of MS-325 with human serum albumin and its effect on 'H and I7O relaxation rates have been studied.'205 Protein surfaces have been identified by NMR spectroscopy with a paramagnetic Gd"' chelate.' 206 The structures of Yb"' adducts of anthracyclines have been probed by paramagnetic NMR spectroscopy.'207 NMR data have 208 also been reported for [(q5-C5Me5)2Yb(bpy)],' ansasamarocenes,' 209
'
'
R. Ruloff, 8.Tbth, R. Scopelliti,R. Tripier, H. Handel and A.E. Merbach, Chem. Commun., 2002, 2630. 1193 P.S. Murphy, M.O. Leach and I.J. Rowland, Phys. Med. Biol., 2002,47, N53. '194 G.M. Nicolle, 8.Tbth, H. Schmitt-Willich,B. Raduchel and A.E. Merbach, Chem.-Eur.J.,2002, 8, 1040. '19' W.H. Li, G. Parigi, M. Fragai, C. Luchinat and T.J. Meade, Inorg. Chem., 2002,41,4018. 1196 F. Botteman, G.M. Nicolle, L. Vander Elst, S. Laurent, A.E. Merbach and R.N. Muller, Eur. J. Inorg. Chem., 2002,2686; T.-H. Cheng, K.-T. Lin, M.-H. Ou, H.-L. Shih, G.-C. Liu and Y.-M. Wang, J. Chin. Chem. SOC.(Taipei, Taiwan), 2001,48, 1099. J.-F. Wei, D.-P. He, W.-J. Pan and B.-H. Ma, Shaanxi Shifan Daxue Xuebao, Ziran Kexueban, 2001,29,70. '19' L.M. De Leon-Rodriguez, A. Ortiz, A.L. Weiner, S.R. Zhang, Z. Kovacs, T. Kodadek and A.D. Sherry, J . Am. Chem. SOC.,2002,124,3514. 1199 F. Alhaique, I. Bertini, M. Fragai, M. Carafa, C. Luchinat and G. Parigi, Inorg. Chim. Acta, 2002,331, 151. l 2 O 0 P. Ballesteros Garcia and S. Cerdan Garcia-Esteller, P C T Int. Appl., 2002,26 pp., Wo 0259097, Al, 20020801. Application: 2002-ES31,20020124. 1201 I. Ronen and S.-G. Kim, N M R in Biomedicine, 2001,14,448. I2O2 B. Gaszner, T. Simor, G. Hild and G.A. Elgavish, J. Mol. Cell. Cardiol., 2001,33, 1945. 1203 A.-M. Delort, G. Gaudet and E. Forano, Anal. Biochem., 2002,306,171. 1204 P. Bernado, R. Barbieri, E. Padros, C. Luchinat and M. Pons, J. Am. Chem. SOC.,2002,124,374. I2O5 P. Caravan, N.J. Cloutier, M.T. Greenfield, S.A. McDermid, S.U. Dunham, J.W.M. Bulte, J.C. Amedio, R.J. Looby, R.M. Supkowski, W.D. Horrocks, T.J. McMurry and R.B. Lauffer, J. Am. Chem. SOC.,2002,124,3 152. I2O6 G. Pintacuda and G. Otting, J. Am. Chem. Soc., 2002, 124, 372; R. Barbieri, I. Bertini, G. Cavallaro, Y.M. Lee, C. Luchinat and A. Rosato, J . Am. Chem. Soc., 2002,124,5581. 1207 L. Di Bari, G. Pintacuda, S. Ripoli and P. Salvadori, Magn. Reson. Chem., 2002,40,396. 1208 M. Schultz, J.M. Boncella, D.J. Berg, T.D. Tilley and R.A. Andersen, Organornetallics, 2002,21, 460. '209 D. Barbikr-Baudry, F. Bonnet, B. Domenichini, A. Dormond and M. Visseaux, J. Organomet. Chem., 2002,647,167.
192
91
[Pr/Cs2],' ' lanthanide complexes of lipophilic ligands derived from 1,3,5triamino- 1,3-5-trideoxy-cis-inositol,'2' Ln"' complexes of C22H26N6,'212chiral macrocyclic Ce"', PrlIl and Eu"' complexes with chloride anions,' 21 [(Et2NCH2CH2N CMeCHCMeNCH2CH2NEt2)Pr(BH4)2],1 = 214 Pr" complex of a Schiff base ligand,I2' [{ Et02CCH2NHC(0)CH2NCH2CH2}4Sm(OH2)I3,' Ln-Zn iminophenolate Complexes,' lanthanide complexes of 1,3,5-triamino-1,3,5-trideoxy-cis-inositol,' [Eu{ E~(2-02CCsH4N-2,6CsH3N-2-C5H4N)2}6]9+,1Eu3+ and Tb3+ macrocyclic complexes bearing an ' appended phenanthroline chromophore,' 220 GdL"'-M" complexes of N,N'ethylenebis(3-hydroxysalicylaldimine),'22' (133), (7Li)and (134).'222
+
'
'
''
But
But
Me
4.2.2 Uranium. NMR data have been reported for [(q5-C5Me5)2UMe2K],122 and [U{ N(CH~CH~NS~M~~BU~)~}I]. [(qS-C5Mes)U(CH2Ph)3],' (135),' 224
1210
1211
1212 1213 1214
121s 1216 1217
1218 1219 1220
1221 1222
1223 1224 1225 1226
T. Wakahara, S. Okubo, M. Kondo, Y. Maeda, T. Akasaka, M. Waelchli, M. Kako, K. Kobayashi, S. Nagase, T. Kato, K. Yamamoto, X. Gao, E. Van Caemelbecke and K.M. Kadish, Chem. Phys. Lett., 2002,360,235. S. Delagrange, C. Gateau, D. Chapon, C. Lebrun, P. Delangle and P. Vottero, Eur. J. Inorg. Chem., 2002,299 1. K.K. Fonda and L.M. Vallarino, Inorg. Chim. Acta, 2002,334,403. J. Lisowski and J. Mazurek, Polyhedron, 2002,21,811. D. Neculai, H.W. Roesky, A.M. Neculai, J. Magull, H.G. Schmidt and M. Noltemeyer, J. Organomet. Chem., 2002,643,47. J.P. Costes, J.P. Laussac and F. Nicodeme, J. Chem. Soc., Dalton Trans., 2002,2731. S.R. Zhang, K.C. Wu and A.D. Sherry, J. Am. Chem. SOC., 2002,124,4226. R. Rodriguez-Cortiiias, F. Avecilla, C. Platas-Iglesias, D. Imbert, J.-C.G. Bunzli, A. de Blas and T. Rodriguez-Blas,Inorg. Chem., 2002,41,5336. D. Chapon, P. Delangle and C. Lebrun, J. Chem. Soc., Dalton Trans., 2002,68. Y. Bretonniere, M. Mazzanti, J. Pecaut and M.M. Olmstead, J. Am. Chem. SOC., 2002,124,9012. S . Quici, G. Marzanni, M. Cavazzini, P.L. Anelli, M. Botta, E. Gianolio, G. Accorsi, N. Armaroli and F. Barigelletti, Inorg. Chem., 2002,41,2777. R. Miyamoto, T. Sugai and S. Sudoh, Polyhedron, 2002,21,2127. P.L. Arnold, L.S. Natrajan, J.J. Hall, S.J. Bird and C. Wilson, J. Organornet. Chem., 2002,647, 205. W.J. Evans, G.W. Nyce, K.J. Forrestal and J.W. Ziller, Organometallics, 2002,21, 1050. J.L. Kiplinger, D.E. Morris, B.L. Scott and C.J. Burns, Organometallics, 2002,21, 5978. F.G.N. Cloke and P.B. Hitchcock, J . Am. Chem. SOC.,2002,124,9352. P. Roussel, R. Boaretto, A.J. Kingsley, N.W. Alcock and P. Scott, J. Chem. Soc., Dalton Trans., 2002,1423.
92
Group 13 Compounds
Five reviews have appeared entitled 'Phosphorus insertion into borane clusters' 1 2 2 7 Recent developments in the chemistry of the nine-vertex monocar-
baboranes',1228 'Chemistry of cho-dodecaborate anion, [BI2Hl2]*-:A review',1229all three of which contain IlB NMR data, 'Aqueous aluminium polynuclear complexes and nanoclusters: A review',' 30 and 'Aluminium in tea. Concentrations, speciation and bioavailability', which contains 27Al NMR data.'
'
5.1 Boron Hydrides and Carboranes. - [2-Bu'-1,2-PCB3H5]has an unusual 31P NMR shift of - 500.5 p.p.m. The "B NMR spectrum was also recorded.'232The coordination chemical shift of [7-(Pri2PBH3)-8-Me-7,8-C2B9Hlo] been cal- has culated and a relationship has been established between J("B'H) and J(31P11B).1233 calculated I'B chemical shifts of nido-[7,8,9-PC2BgH11] and The nido-[7,8,9-PC2B8Hlo] have been compared with experimental ones.1234The stereoselective deboration of two thioether o-carborane derivatives has been 'H{"B} NOESY has been used to investigated by IlB NMR show a strong C - H - . . O bond in o-carboranyl P - 1 a ~ t o s i d e .NMR data have l~~~ also been reported for [BH4]-, (1'B),'237 [PhNHNH2BH3],("B, 15N),1238 [(2,4,6But3C6H20)PH2BH3], (11B),1239 [HB(N = PBu'~)~], (11B),1240 (11B),1241 (136), [1,21227 1228 1229 1230 1231 1232 1233
1234
1235
1236
1237 1238
1239 1240
B. Ztibr, Collect. Czech. Chem. Commun., 2002,67, 843. B. Stibr and B. Wrackmeyer, J . Organornet. Chem., 2002,657,3. I.B. Sivaev, V.I. Bregadze and S. Sjoberg, Collect. Czech. Chem. Commun., 2002,67,679. W.H. Casey, B.L. Phillips and G. Furrer, Rev. Mineral. Geochem., 2001,44,167. T.P. Flaten, Coord. Chem. Rev., 2002,228,385. P.N. Condick, M.A. Fox, R. Greatrex, C. Jones and D.L. Ormsby, Chem. Commun., 2002,1448. R. Nufiez, C. Viiias, F. Teixidor, R. Sillanpaa and R. Kivekas, J . Organomet. Chem., 2002,657, 224. B. Stibr, J. Holub, M. Bakardjiev, D. Hnyk, O.L. Tok, W. Milius and B. Wrackmeyer, Eur. J . Inorg. Chem., 2002,2320. R. Brockman, K. Challis, G. Froehner and T.D. Getman, Main Group Metal Chem., 2002,25, 629. A. Donati, S. Ristori, C. Bonechi, L. Panza, G. Martini and C. Rossi, J . Am. Chem. SOC.,2002, 124,8778. R. Custelcean, M. Vlassa and J.E. Jackson, Chem.-Eur. J., 2002,8,302. B. Wrackmeyer, A.G. Giumanini, A. Gambi, G . Verardo, G. Gilli and V. Bertolasi, Heteroatom Chem., 2002,13,366. E. Rivard, A.J. Lough and I. Manners, J . Chem. SOC., Dalton Trans., 2002,2966. S. Courtenay, J.Y. Mutus, R.W. Schurko and D.W. Stephan, Angew. Chem., Int. Ed. Engl., 2002, 41,498.
93
C6H6)Fe(Et2C2B4H3-7-C'CSiMe3)],'B),' 246 (' C=C)Co(q5-C5Me5)], (11B),1247 [(q5-C5Me5)Co(Et2C2B4H3)-5-O(CH2)4-(q4C5Me~)CoH(Et2C2B4H3-5-I)], (11B),1248 ~ ~ ~ o - C S - ( R ) - ~ , ~ - ( M ~ ~ S ~ ) ~ - ~ , (l'B),' 249 closo-[2-CB6H7]-, ("B),' 2 5 0 closo-[2-Ph-2-CB6H6] -, (l'B),' 2 5 ' [(R1C5H4N)B8H 1NHR2], ("B),' 5 2 C E O S ~ - [ P ~ C B ~ H ~ ] 1 -, ~los~-[PhCBloHlo] -, arachno-[B9H12-4,8-Br2] ("B),' 5 4 arachno-[6-C&H14] -, ("B),' -, ("B),' a r a ~ h n o - [ 4 - C B ~ H ~ ~ ] ~ - , 2 5 6 2,1-[PCB8H9], ("B),' ("B),' [8,8-(~~-dppm)-8-(~'dppm)-nido-8,7-RhS&Hlo], ("B),' [BloHlo-,(OH),]2-, (' 'B),' 5 9 [C7H6B10Hg] -, (' 'B),'260 [2-BloH9NH= CHC&4-4-NHCOMe]-, ("B),' 2 6 1 [l-Ph-closo1-CBgH4- 10-I-6,7,8,9-(C6H4-4-Me)4] ("B),' 2 6 2 [3-C1- l-(r16-arene)-isonido-1,2,4-, R U C ~ B ~ H (11B),1263 ~], [9,9-(Ph3P)-nido-9,7,8-RhC2B8Hll], (11B),1264arachno[5,6,9-C2SB7H 113, ("B),' 26 [R' HBgHloR'], (' 'B),' 266 [l-SBgHg], ('' B),' 2 6 [8,8{q2-(CH2),(PPh2)2}-nido-8,7-RhS&Hlo], (' 1B),1268 [l-(q5-C5Me5)-2-Me-closo1241
i242
1243
1244 1245
C5Me5)R~}2-4,5-Me2-4,5-c2B2H6], ['OBSHg], (' 'B),'244
{ (q5-C5Me5)Fe}CO(CO)~}B~H~], { ("B),'
242
[2-FB4H9], ("B),'
nido-[ 1,7-{(q5('OB),' 2 4 5 C($[(q5-C5Me5)Co(2,3-Et2C2B3H2-5243
1246
i247
1248 i249 12'0

1251
1252 1253
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1256
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1258 1259
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1261
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263
1264 1265
1266 1267
C. Prasang, M. Hofmann, G. Geiseler, W. Massa and A. Berndt, Angew. Chem., Int. Ed. Engf., 2002,41, 1526. M.A. Peldo, A.M. Beatty and T.P. Fehlner, Organometalfics, 2002,21,2821. M.A. Fox, R. Greatrex and D.L. Ormsby, Chem. Commun., 2002,2052. H. Yan, A.M. Beatty and T.P. Fehlner, Angew. Chem., Int. Ed. Engl., 2002,41,2578. L. Adams, S.N. Hosmane, J.E. Eklund, J.H. Wang and N.S. Hosmane, J. Am. Chem. SOC.,2002, 124, 7292; L. Adams, S. Tomlinson, J.H. Wang, S.N. Hosmane, J.A. Maguire and N.S. Hosmane, Inorg. Chem. Commun., 2002,5,765. J.M. Russell, M. Sabat and R.N. Grimes, Organometaffics, 2002,21,4113. H.J. Yao, M. Sabat and R.N. Grimes, Organometallics, 2002,21,2833. J.M. Russell, M. Sabat and R.N. Grimes, Organometaffics, 2002,21, 5613. J.A. Maguire, J.Q. Wang, C. Zheng, C.Z. Li and N.S. Hosmane, Inorg. Chim. Acta, 2002,334,91. B. Stibr, O.L. Tok, W. Milius, M. Bakardjiev, J. Holub, D. Hnyk and B. Wrackmeyer, Angew. Chem., Int. Ed. Engf.,2002,41,2126. A. Franken, D.L. Ormsby, C.A. Kilner, W. Clegg, M. Thornton-Pett and J.D. Kennedy, J . Chem. SOC.,Dalton Trans., 2002,2807. C. Bauer, D. Gabel, T. Borrmann, J.D. Kennedy, C.A. Kilner, M. Thornton-Pett and U. Dorfler, J. Organomet. Chem., 2002,657,205. A. Franken, C.A. Kilner, M. Thornton-Pett and J.D. Kennedy, J. Organomet. Chem., 2002,657, 180. J. Bould, R. Greatrex, J.D. Kennedy, D.L. Ormsby, M.G.S. Londesborough, K.L.F. Callaghan, M. Thornton-Pett, T.R. Spalding, S.J. Teat, W. Clegg, H. Fang, N.P. Rath and L. Barton, J. Am. Chem. SOC.,2002,124,7429. T. Jelinek, M. Thornton-Pett and J.D. Kennedy, Collect. Czech. Chem. Commun., 2002,67,1035. D.E. Kadlecek and L.G. Sneddon, Inorg. Chem., 2002,41,4239. J. Holub, M. Bakardjiev, B. Stibr, D. Hnyk, O.L. Tok and B. Wrackmeyer, Inorg. Chem., 2002, 41,2817. 0. Volkov, N.P. Rath and L. Barton, Organometallics, 2002,21, 5505. K.Y. Zhizhin, 0.0.Vovk, E.A. Malinina, V.N. Mustyatsa, L.V. Goeva, I.N. Polyakova and N.T. Kuznetsov, Russ. J. Coord. Chem.,2001,27,613. K.M. Harmon, T.E. Nelson and B.M. Stackowski, J. Mol. Struct., 2002,605,27. I.B. Sivaev, N.A. Votinova, V.I. Bragin, Z.A. Starikova, L.V. Goeva, V.I. Bregadze and S. Sjoberg, J. Organomet. Chem., 2002,657, 163. A. Franken, C.A. Kilner, M. Thornton-Pett and J.D. Kennedy, Chem. Cornmun., 2002,2048. V.E. Konoplev, I.V. Pisareva, D.A. Lemenovskii, P.V. Petrovskii, O.L. Tok, F.M. Dolgushin and I.T. Chizhevsky, Collect. Czech. Chem. Commun., 2002,67,936. 0. Volkov, N.P. Rath and L. Barton, Collect. Czech. Chem. Commun., 2002,67,769. D. Hnyk and J. Holub, Collect. Czech. Chem. Cornmun., 2002,67,813. P. Paetzold and E. Leuschner, 2. Anorg. Aflg. Chem., 2002,628,658. H. Mdlendal, S. Samdal, J. Holub and D. Hnyk, Inorg. Chem., 2002,41,4574.
94
1,2,3,4-RuC3B7H9], (11B),1269 nido-[(BuMeHN)-But-7-CBloH12],(11B),1270 [lH2N-2,2,2-(OC)3-closo-2, - M o C B ~ ~ H( I ~ ~ ] ~ - , 1,2-p-(NHCMe = 0)-2,2,2~ 'B),' [ -, (OC)3-closo-2,1-MoCBloH~~] ( I 1B),1272[2,2,2-(OC)3-2-X-3-NMe3-closo-2,1( l B), [1,2-p-NHBut-2,2-( OC)2-3,2-~:~2MoCBloHlol-, {C(= CHBu')CH = CHBu'}-closo-2,l-ReCBloH9], (11B),1274 1-NH = CMe2-2[ (' 1B),1276 [3-X-7-R-7,8C1-2-PPh3-~l0~0-2,1-RhCBloHlo],7 5 [C2B9HI ("B),' 2 nido-C2B9Hlo]-, (11B),1277 [10-(SMe2)-7,8-C2B9H11], (11B),'278 closo-[2,3-R1,R22,3-C2B9H9],(I'B),' 79 [4,4,4-( Me2N)3-4-Me-3,1,2-closo-TaC2B9Hlo],("B),' 280 [Cl(Me2N)2TaC2B9H11], ("B),' 2 8 1 [MO(~~-C~H~)(CO)~(~,~-~-SCH nido-C2B9Hlo)],(' 'B),12 [Re(C0)3(q5-2-R-2,3-C2B9Hlo)] (11 B),' 2 8 3 [3-(q5-, C5H5)-4-SMe2-7,8-(CF3C02)212-HgC1-3,1 ,2-FeC2B9H7], ( I B), 84 [{ Br(Ph3P)2R~}-5,6,10-(p-H)310-H-7,8-C2B9H8], ( l lB), 28 C h 5C5Me5)Ru(C2B9H11)Ru(q5-C5Me5)], (11B),'286 [{ 8-Ph2P(O)(CHZCH20)21,2CZB9H10}( 1 , ' C B H 1 - , ' C ] '2-2g1)33-0, B), 28 C ~ O S O - [ 8-(2{ MeOC5H40)(CH2CH20)2-1,2-C2B9Hlo}( 1',2'-C2B9Hll)-3,3'-Co]-, ( 11B),'2ss closo-[ { 8-( 15-crown-5-CH20)( CH2CH20)2-,2-C2B9H -3,3'-Co-( 1',2'1 C2B9H1i)] -, ("B),' 289 [3,3'-Co( 1,2-C2BsHI1){ 1,2-C2BgHlo-4-(OCH2CH2>2X}],
'
'
'
'
'
1268 1269 1270 1271 1272 1273

1274
1275 1276
1277 1278 1279 1280 1281 1282 1283 1284 1285 1286 1287
1288
1289
0.Volkov, R. Macias, N.P. Rath and L. Barton, J. Organomet. Chem., 2002,657,40. B.M. Ramachandran, S.M. Trupia, W.E. Geiger, P.J. Carroll and L.G. Sneddon, Organometallics, 2002,21, 5078. A.S. Batsanov, M.A. Fox, A.E. Goeta, J.A.K. Howard, A.K. Hughes and J.M. Malget, J. Chem. SOC., Dalton Trans., 2002,2624. S.W. Du, J.A. Kautz,T.D. McGrath and F.G.A. Stone, J. Chem. SOC., Dalton Trans., 2002,1553. J.A. Kautz, D.A. Kissounko, N.S. Kissounko and F.G.A. Stone, Organometallics, 2002,21,2547. S.W. Du, J.A. Kautz, T.D. McGrath and F.G.A. Stone, Inorg. Chem., 2002,41,3202. S.W. Du, J.A. Kautz, T.D. McGrath and F.G.A. Stone, Chem. Commun., 2002,1004. J.A. Kautz, D.A. Kissounko, N.S. Kissounko and F.G.A. Stone, J. Organomet. Chem., 2002,651, 34. M.A. Fox, A.K. Hughes, A.L. Johnson and M.A.J. Paterson, J. Chem. SOC., Dalton Trans., 2002, 2009; M.A. Fox, A.E. Goeta, A.K. Hughes and A.L. Johnson, J. Chem. SOC., Dalton Trans., 2002, 2132. G. Barbera, C. Viiias, F. Teixidor, A.J. Welch and G.M. Rosair, J . Organomet. Chem.,2002,657, 217. 0. Tutusaus, F. Teixidor, R. Nuiiez, C. Viiias, R. Sillanpaa and R. Kivekas, J. Organomet. Chem., 2002,657,247. M.A. Fox, A.K. Hughes and J.M. Malget, J. Chem. SOC.,Dalton Trans., 2002,3505. A.K. Hughes, J. Organomet. Chem., 2002,657,9. M.A. Fox, A.E. Goeta, A.K. Hughes, J.M. Malget and K. Wade, Collect. Czech. Chem. Commun., 2002,67, 791. G. Barbera, C. Viiias, F. Teixidor, G.M. Rosair and A.J. Welch, J. Organomet. Chem., 2002,663, 221. J.F. Valliant, P. Morel, P. Schaffer and J.H. Kaldis, Inorg. Chem., 2002,41,628. V.I. Bregadze, I.A. Lobanova, S.V. Timofeev, A.R. Kudinov, V.I. Meshcheryakov, O.L. Tok, P.V. Petrovskii and Z.A. Starikova, J. Organomet. Chem., 2002,657, 171. S.V. Timofeev, I.A. Lobanova, P.V. Petrovskii, Z.A. Starikova and V.I. Bregadze, Russ. Chem. Bull., 2001,50,2245. A.R. Kudinov, D.S. Perekalin, S.S. Rynin, K.A. Lyssenko, G.V. Grintselev-Knyazev and P.V. Petrovskii, Angew. Chem., Znt. Ed. Engl., 2002,41,4112. B. Gruner, J. PleSek, J. BaEa, I. Cisafova, J.F. Dozol, H. Rouquette, C. Viiias, P. Selucky and J. Rais, New J . Chem., 2002,26, 1519. J. PleSek, B. Gruner, S. Hermanek, J. BaEa, V. Marecek, J. Janchenova, A. Lhotsky, K. Holub, P. Selucky, J. Rais, I. Cisaiova and J. Caslavsky, Polyhedron, 2002,21,975. B. Gruner, J. Plelek, J. BaEa, J.F. Dozol, V. Lamare, I. Cisaiova, M. Belohradsky and J. Caslavsky, New J. Chem., 2002,26,867.
1: N M R SpectroscopJ9 in the Liquid and Gas Phase
95
(' 'B),' 290 [8,8'-p-MeCOz( 1,2-C2B9Hl&-3-Co],( I B),129 [8,8'-p-Et2NP03(1,2-
'
C2B9H10)2-3,3'-C~] , ("B),' 2 9 2 closo-[3-Co(q'-NC4Me2H2)-1,2-Ph2-1,2-C2B~H9], (I1 B), 2 9 [(9-Me2S-7,8-C2B9Hlo)RhX2]2, ( I IB),' 294 [{ q5:u(Pr12NB)(C9H7)(C2BloH 1)}Zr(NMe2)2], ( I 'B),' 9 5 nido-[7,8,1O-PC2BgH I ("B),' 296 [10-X-nid0-7,8,9,1 l-P2C2B7Hs], ( I 'B),' 2 9 7 [{ Ph2P(0)}2NHBl2Hl1]-, (11B),'298 [MeSB12HII]2-, ('1B),'299[B12X12]"-, = H, OH, Me, F, NH,; (X 11B),1300 [BIIHI2 .(02CR),,]' , (11B),'301 [l-X-CBIIHIII-, (11B),'302 [12-(HO)-lCBI H I I] - , ( I IB), 3 0 3 [Pr13Si(1-H-CBI HSBr6)], (29Si),' 304 [{ (Ph3P)(Ph2P-q6( I B),' O6 C6H5)Rh}2(closo-CB11H6Br6)2], (11B),'305 [Ag(PPh3)( B 1 I H I2)] c ( I 'B),' 308 ( I IB),' O [Agz(closo-CBI I H I 2)43' - , [RSnB, 1H1 I3 -, -, ("B),' [(dppp)Pt(SnBiI H I i)2I2-, 'B),' 309 [MeNBi I H I I { Fe(~5-CsH~)(Co)2}l [7,10-C2BloH1-, ("B),' 3 1 1 [2-(l-naphthyl)-p-carborane], (11B),1312 3] carboranyl derivatives of anthraquinones, fluorenones and sulfones, (11B),'3'3 [BloHlo(lC02H)( 12-CNBocNHBoc)], ( I 'B),' 314 closo-[ 1,l2-C2BloH lo-l-formamide], (11B),'315 [p- 1,2-{2-CsH4(CH2)2}-1,2-C2BloH101, ( I 'B),' 3 1 6 [1-( 1,27
290
1291
1293
294
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1296 1297
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I.B. Sivaev, Z.A. Starikova, S. Sjoberg and V.I. Bregadze, J . Organornet. Chem., 2002,649, 1. J. Plekk, B. Gruner, J. BaEa, J. Fusek and I. Cisaiova, J. Organomet. Chem., 2002,649,181. J. PleSek, B. Gruner, I. Cisafova, J. BaEa, P. Selucky and J. Rais, J. Organomet. Chem., 2002,657, 59. J. Llop, C. Viiias, F. Teixidor, L. Victori, R. Kivekas and R. Sillanpaa, Inorg. Chem., 2002,41, 3347; ihid., Organometallics, 2002,21, 355. A.R. Kudinov. D.S. Perekalin, P.V. Petrovskii, K.A. Lyssenko, G.V. Grintselev-Knyazev and Z.A. Starikova, J. Organomet. Chem., 2002,657, 115. G.F. Zi, H.W. Li and Z.W. Xie, Organometallics, 2002.21, 3850. D.L. Ormsby, R. Greatrex, B. Stibr and J.D. Kennedy, J. Organomet. Chem., 2002,657,279. J. Holub, M. Bakardjiev and B. Stibr, Collect. Czech. Chem. Commun., 2002,67,783. R. Bernard, D. Cornu, B. Gruner, J.-F. Dozol, P. Miele and B. Bonnetot, J . Organomet. Chem., 2002,657, 83. R.G. Kultyshev. J.P. Liu, S.M. Liu, W. Tjarks, A.H. Soloway and S.G. Shore, J. Am. Chem. SOC., 2002,124,2614. M.L. McKee, Inorg. Chem., 2002,41,1299. K.Y. Zhizhin and N.T. Kuznetsov, Zh. Neorg. Khim., 2002,47,401. Z. Janousek. C.L. Hilton, P.J. Schreiber and J. Michl, Collect. Czech. Chem. Commun., 2002,67, 1025. B. Gruner. I. Cisaiova, J. Caslavsky, B. Bonnetot and D. Cornu, Collect. Czech. Chem.
Commun.,2002,67,953. D. Stasko and C.A. Reed, J. Am. Chem. Soc., 2002,124, 1148. A. Rifat, N.J. Patmore, M.F. Mahon and AS. Weller, Organometallics, 2002,21,2856. N.J. Patmore, C. Hague, J.H. Cotgreave, M.F. Mahon, C.G. Frost and A.S. Weller, Chem.-Eur. J . , 2002,8, 2088. M.A. Fox, M.F. Mahon, N.J. Patmore and A.S. Weller, Inorg. Chem., 2002,41,4567. B. Ronig, I. Pantenburg and L. Wesemann, Eur. J. Znorg. Chem., 2002,319; T. Marx, B. Ronig, H. Schulze, I. Pantenburg and L. Wesemann, J. Organomet. Chem., 2002,664,116. L. Wesemann, S. Hagen, T. Marx, I. Pantenburg, M. Nobis and B. Driessen-Holscher, Eur. J. Znorg. Chem., 2002,226 I . P. Paetzold, P. Lomme and U. Englert, Z. Anory. Allg. Chem., 2002,628,632. C . Viiias, G. Barbera and F. Teixidor, J. Organornet. Chem., 2002,642,16. L. Eriksson, I.P. Beletskaya, V.I. Bregadze, I.B. Sivaev and S. Sjoberg, J . Organomet. Chem., 2002,657, 267. K. Vyakaranam, G. Rana. A. Ratanasuwan, S.N. Hosmane, J.A. Maguire and N.S. Hosmane, Organometallics, 2002,21,3905. J.F. Valliant, 0.0. Sogbein, P. Morel, P. Schaffer, K.J. Guenther and A.D. Bain, Znorg. Chem., 2002,41,2731 . P. Schaffer, P. Morel, J.F. Britten and J.F. Valliant, Inorg. Chem., 2002,41,6493. G.-f. Zi, H.-W. Li and Z.-w. Xie, Organometallics, 2002, 21. 5415.
304
30s
130h
1307
I3O8
1309
I3l0 31 1312
1313
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l3Is
1316
96
XCH2C6H4CH2)-2-Bu'Me2Si1,2-C2BloHlO], ( I ' B),' ' [Pri2NB(C9H6)(C2B10Hio)I2-,(11B),1318 [q6-[1,2-{ ~,~-C~H~(CH~)}-~,~-C~B~OH~O]MCI(THF) (M = Y, Nb, Er; 'IB),l3l9 [{q5:q6:~-Me2Si(C9H6)(C2BloHl~CH2NMe)}Zr(py)], (11B),1320 [PdClMe{ 1,2-(Ph2P)2-,2-C2BloH 1 [(r5-C5Me~)COC2BioHi2], ("B),l 321 (11B),1322 [4,1,6-closo-SnC2BloH12], (11B),1323 [(NO2)-BI2Hl1l2-, (11B),1324 [9,1012-l-C-7-PBloHlo], (13B),1325 [(C2BloH9PPh2)MMe2X], = Si, Ge, Sn; 11B),1326 (M [BloHloC2(SnMe2)2SnMe2], ( II9Sn),' [PdBr2{ 1,2-(Ph2P)2-1,2-C2B1oHlo}], 1 (11B),1328cEoso-[1,2-(PhS)2-,2-C2B10H10],(' 'B),' 29 [(q5-C5H5)2Fe2(CO)3(pSe2C2B10H10)], (11B),1330 [(q5-C5Mes)M(H2C2Se2C2BloHlo)], Rh, Ir; I1B,77Se, (M = 103Rh),1331 ~(q5-C5H5)Co(1,2-S2C2B10H10)1, (11B),1332 [1,2-~loso-P2BloHlo], (l lB),' [(Ph3P)4ClPd4B16H17(PPh3)2], (11B),1334 [ u ~ ~ ~ - B I ~ H & o ( C O ) ~ ] , ( I 'B),' and [B18HzoNi(q5-C5H5)] IB). 36 -, ( I
Other Compounds of Boron. - Isotope-induced chemical shifts, 28(10B,1 1B)29Si alkenylsilanes containing three- and four-coordinate boron have in been reported.1337 NMR data have also been reported for (137), (11B),1338 [MeB(CsF5)3]-, (11B),1339 [Me3SiCH2B(C6H5)3]-,(11B),'340 [BuB(C~&)~]-, (11B),1341 [BPh&, (11B),1342 (138), (11B),1343 [B(C6F5)4]-, (11B),1344 [MeB(C65.2
1317
1318
1319 1320
1321
1322
1323
1324
1325
1326
1327 13"
1329
1330
1331 1332
1333
334
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1336
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339
1340
A.S. Batsanov, C.K. Broder, A.E. Goeta, J.A.K. Howard, A.K. Hughes and J.M. Malget, J. Chem. SOC., Dalton Trans., 2002, 14. G.-f. Zi, H.-W. Li and Z.-w. Xie, Organometallics, 2002,21, 1136. G.-f. Zi, H.-W. Li and Z.-w. Xie, Organometallics, 2002,21, 3464. Y.R. Wang, H.O. Wang, H.-W. Li and Z.-w. Xie, Organometallics, 2002,21,3311. A. Burke, R. McIntosh, D. Ellis, G.M. Rosair and A.J. Welch, Collect. Czech. Chem. Commun., 2002,67,991. S. Paavola, F. Teixidor, C. Viiias and R. Kivekas, J . Organomet. Chem., 2002,645,39. N.M.M. Wilson, D. Ellis, A.S.F. Boyd, B.T. Giles, S.A. Macgregor,G.M. R0sairandA.J. Welch, Chem. Commun., 2002,464. K.Y. Zhizhin, N.A. Votinova, L.V. Goeva and N.T. Kuznetsov, Russ. J. Coord. Chem., 2001,27, 625. L.I. Zakharkin, G.G. Zhigareva, K.A. Lysenko, M.Y. Antipin and P.V. Petrovskii, Russ. J. Gen. Chem., 2001,71,196. T. Lee, S. Kim, M.S. Kong, S.O. Kang and J. KO, Bull. Korean Chem. SOC., 2002,23,845. C. Lee, J. Lee, S.W. Lee, S.O. Kang and J.J. KO,Znorg. Chem., 2002,41,3084. S . Paavola, F. Teixidor, C. Viiias and R. Kivekas, J . Organomet. Chem., 2002,657,187. J. Llop, C. Viiias, J.M. Oliva, F. Teixidor, M.A. Flores, R. Kivekas and R. Sillanpaa, J . Organomet. Chem., 2002,657,232. S.X. Lu, G.X. Jin, S. Eibl, M. Herberhold and Y. Xin, Organometallics, 2002,21,2533. M. Herberhold, H. Yan, W. Milius and B. Wrackmeyer, Chem.-Eur. J., 2002,8,388. J.-H. Won, D.-H. Kim, B.Y. Kim, S.-J. Kim, C. Lee, S. Cho, J. KOand S.O. Kang, Organometallies, 2002,21, 1443. B. Gruner, D. Hnyk, I. Cisaiova, Z. Plzak and B. Stibr, J . Chem. SOC., Dalton Trans., 2002,2954. M.G.S. Londesborough, C.A. Kilner, M. Thornton-Pett and J.D. Kennedy, J. Organomet. Chem., 2002,657,262. J.W. Taylor, U. Englich, K. Ruhlandt-Senge and J.T. Spencer, Organometallics, 2002,21,3054. J.W. Taylor, U. Englich, K. Ruhlandt-Senge and J.T. Spencer, J. Chem. Soc., Dalton Trans., 2002, 3392; J.W. Taylor, U. Englich, K. Ruhlandt and J.T. Spencer, Znorg. Chem. Commun., 2002,5,274. B. Wrackmeyer and O.L. Tok, Magn. Reson. Chem., 2002,40,406. C . Prasang, A. Mlodzianowska, Y. Sahin, M. Hofmann, G. Geiseler, W. Massa and A. Berndt, Angew. Chern., Znt. Ed. Engl., 2002,41,3380. R. Choukroun, C. Lorber and B. Donnadieu, Organometallics, 2002,21, 1124; A. Antiiiolo, R. Fernandez-Galan, I. Orive, A. Otero and S. Prashar, Eur. J. Znorg. Chem., 2002,2470. S. Arndt, T.P. Spaniol and J. Okuda, Chem. Commun., 2002,896.
97
(136)
F5)3]-, (11B),1345 [Bu3Sn][c6F4-1,2-{ B(C6F5)2}2(p-OMe)]-, ("B, 1'9Sn),'346 [(C6F5)4-.B(N3),]-, ("B, 14N),1 347 [(F3C)3BCO], (11B),'348 (11B),'349 [n-ClsH37EHB(C6F5)3], = 0, S, (E [CH2 = CHOC{ = OB(C6F5)3}Me], ''B), O [closo-B1 2Me12]- , ( I 1 B),' ' [(Ph3P)Ag(HCBI1Me1I)], ( 'B),' 5 2 [&(NMe2)6), ("B),' 3 5 (139), (* B, 29Si),13 [BC2H4SiH2(NCN)o.5]3, 29Si),' 5 5 54 ("B, 3 (140), ("B, 29Si, 119Sn),1356(141), ("B, 15N, 29Si, 119Sn),1357 [(H2C = CHCHJzB(CH2= CHCH2)C= C(SiMe3)CH CHC(SiMe3) C(CH2C = = H = CH2)B(CH2CH= CH&], ("B, 29si),'358 [( Me&CH2)2B(CH2SiMe2CH2SiMe3)], B, 29Si), ( (142), ("B), 360 [1 -(2,4,6Me3C6H2)2B-8-Me3Sn-naphthalene], ("B, 'I9Sn),' 361 (143), (' B),' [(C6F5)3BNCI], (11B),1364 (C6F5)3BO R] [H2N{ B(C6F5)3}2] -, ("B),'36 (11B),1365 12-ArCH(CH2CH =CH2)OB(C6F5)3]-, ("B, 119Sn),'366 (144), ( 'B),' 36
'
1341 1342 1343 1344
1345 1346 1347
1348
1349 1350 1351 1352
1353
1354 1355
1356
1357
1358 1359 1360 1361 1362
1363
1364
S. Doring, G. Erker and R. Frohlich, J. Organomet. Chem., 2002,643,61. P.K. Baker, M.G.B. Drew and D.S. Moore, J. Organomet. Chem., 2002,664,37. J.D. Hoefelmeyer and F.P. Gabbai, Organometallics, 2002,21,982. J.A.R. Schmidt and J. Arnold, Organometallics, 2002,21,2306; F. Delpech, I.A. Guzei and R.F. Jordan, Organometallics, 2002,21, 1167. M.D. Hannant, M. Schormann and M. Bochmann, J . Chem. SOC.,Dalton Trans., 2002,4071. L.D. Henderson, W.E. Piers, G.J. Irvine and R. McDonald, Organometallics, 2002,21,340. W. Fraenk, T.M. Klapotke, B. Krumm, H. Noth, M. Suter, M. Vogt and M. Warchhold, Can. J. Chem., 2002,80,1444. A. Terheiden, E. Bernhardt, H. Willner and F. Aubke, Angew. Chem., Znt. Ed. Engl., 2002,41, 799; M. Finze, E. Bernhardt, A. Terheiden, M. Berkei, H. Willner, D. Christen, H. Oberhammer and F. Aubke, J. Am. Chem. SOC.,2002,124,15 385. A.K. Dash and R.F. Jordan, Organometallics, 2002,21,777. M.J. Drewitt, M. Niedermann, R. Kumar and M.C. Baird, Znorg. Chim. Acta, 2002,335,43. M.F. Hawthorne and T. Peymann, U.S.,2002,6 pp., US 6355840, B1,20020312. M.J. Ingleson, M.F. Mahon, N.J. Patmore, G.D. Ruggiero and A.S. Weller, Angew. Chem., Int. Ed. Engl., 2002,41, 3694. A. Maier, M. Hofmann, H. Pritzkow and W. Siebert, Angew. Chem., Int. Ed. Engl., 2002, 41, 1529. B. Wrackmeyer, W. Milius and A. Badshah, J. Organomet. Chem., 2002,656,97. M. Weinmann, M. Horz, F. Berger, A. Muller, K. Muller and F. Aldinger, J. Organomet. Chem., 2002,659,29. B. Wrackmeyer, M.H. Bhatti, S. Ali, O.L. Tok and Y.N. Bubnov, J. Organomet. Chem., 2002, 657, 146. B. Wrackmeyer, A. Pedall, W. Milius, O.L. Tok and Y.N. Bubnov, J. Organomet. Chem., 2002, 649,232. B. Wrackmeyer, W. Milius, O.L. Tok and Y.N. Bubnov, Chem.-Eur. J . , 2002,8,1537. D.V. Yandulov, J.C. Huffman and K.G. Caulton, Organometallics, 2002,21,4030. X.L. Zheng, B. Wang and G.E. Herberich, Organometallics, 2002,21, 1949. M. Schulte and F.P. Gabbai, Chem.-Eur. J., 2002,8,3802. D. Vagedes, G. Kehr, D. Konig, K. Wedeking, R. Frohlich, G. Erker, C. Muck-Lichtenfeld and S. Grimme, Eur. J. Znorg. Chem., 2002,2015. S.J. Lancaster, A. Rodriguez, A. Lara-Sanchez, M.D. Hannant, D.A. Walker, D.H. Hughes and M. Bochmann, Organometallics, 2002,21,451. W. Fraenk, T.M. Klapotke, B. Krumm, P. Mayer, H. Piotrowski and M. Vogt, 2. Anorg. Allg. Chem., 2002,628,745.
98
(145),
(11B),1368 [si{ (CH2)3SiMe2-3-OCsH4-4-c6F~B(c6F5)2}4], ("B),' 369 [LA10*B(CtF5)3], (' 'B),' 70 [(C6F5)3BClB(C6F5)3]-,("B), ' '' (146), (llB, 29Si), and [(Bu'C=C)~B], ("B). 373
'
SiMe,
(141)
H Me ,Me3Si i Me3Siq h
H,
5;
B -B
(dur) d u r )
Ab initio GIAO-MP2 calculated IlB and 13CNMR chemical shifts have been reported for hypercoordinate onium-carbonium dications and isoelectronic onium-boronium cations.' 74 Field-cycling NMR spectroscopy has been used to observe IlB pure quadrupole resonance of two peptide boronic acid inhibitors. The simultaneous determination of 4-boronophenylalanine and boric acid using IlB NMR spectroscopy has been described.'376 NMR data have also
1365
13"
1367
1368
1369 1370
1371
1372
1373
1374
1375
N. Millot, A. Cox, C.C. Santini, Y.Molard and J.M. Basset, Chem.-Eur. J., 2002,8, 1438. J.M. Blackwell, W.E. Piers and R. McDonald, J. Am. Chem. Soc., 2002,124, 1295. D. Vagedes, G. Erker and R. Frohlich, J. Organomet. Chem., 2002,641, 148. M. Schulte and F.P. Gabbal, J. Organomet. Chem., 2002,643, 164. R. Roesler, B.J.N. Har and W.E. Piers, Organometallics, 2002,21,4300. D. Neculai, H.W. Roesky, A.M. Neculai, J. Magull, B. Walfort and D. Stalke, Angew. Chem.,Int. Ed. Engl., 2002,41,4294. R.M. Bellabarba, G.P. Clancy, P.T. Gomes, A.M. Martins, L.H. Rees and M.L.H. Green, J. Organomet. Chem., 2002,640,93. D. Scheschkewitz, M. Hofmann, A. Ghaffari, P. Amseis, C. Prasang, W. Mesbah, G. Geiseler, W. Massa and A. Berndt, J. Organomet. Chem., 2002,646,262. M.J. Bayer, H. Fritzkow and W. Siebert, Eur. J. Znorg. Chem., 2002,2069. G. Rasul, G.K.S. Prakash and G.A. Olah, Proc. Natl. Acad. Sci. U.S.A., 2002,99,9635. D. Ivanov, W.W. Bachovchin and A.G. Redfield, Biochemistry, 2002,41,1587.
99
been reported for (147), = S, NMe, 0; 11B),1377 (31B),1378 (E (148), [(Ph2B)20], 'B),' 79 [(Ph2BO),P(S)SH), ("B),' 380 [Me4C202BB02C2Me4], ("B),' ' (l49), ( I B, 29Si), 8 2 (150),(' 'B, 'I9Sn),'38 [4-MeOC6H4CH2C{ B(OZC~H~)}~], 384 ( B), salen-supported dinuclear and trinuclear boron compounds, ("B),' 3 8 5 (151), ("B, 15N),1386substituted 2-Ph-6-N-1,3-O-2-borabenzocyclononenes, 3 8 7 ("B),' phenyl boronate, ( I 'B),' 8 8 [4-MeC6H4B(OH)2], "B),' 389 [B506Ar4] ("B),' 390 ( -, [(Me4C202B)CPh C{ P(O)(OEt)2}(BO2C2Me4)], ("B),' 391 [Me4C2O2-BC6H3= 3,5-C&], ("B),' 392 [4-BrC6H4BO2SiBut2]2, ("B, 29Si),1393[Me4C202B-4(152), (11B),1395 [Me3SiCH= C(BC12)2], ("B, C6H4(CH2),C02Me], (1'B),1394 29Si),'396 (153), (11B).1397 and The influence of the nature of the solvent on the 19Fchemical shift of [BF4]has been examined.' 398 NMR data have also been reported for polyborazylene, [{($(11B),1399copolymer of borazine and [(MeNHB)3(NH)3], a ("B, 15N),1400 C5H5)Fe(q5-C5H4)B}3(NH)3], (11B),1401 { (Me2N)3SiNHB}3(NH)3],'B, 29Si),'402 [ ('
(I
1376
1377 1378 1379 1380
1381
1382 1383
1384
1385
1386
1387 1388 1389 1390 1391
1392
1393
1394 1395 1396 1397 1398
1399
1400
1401
1402
K. Yoshino, Y. Tanaka, H. Kakihana, M. Ichihashi and Y. Mishima, Frontiers in Neutron Capture Therapy, [Proceedings o the International Symposium on Neutron Capture Therapyfor f Cancer], 8th, Los Angeles, C A , U.S.A.,Sept. 13-18,1998,2001,2,863. T. Kohler, J. Faderl, H. Pritzkow and W. Siebert, Eur. J. Znorg. Chem., 2002,2942. A. Eckert, H. Pritzkow and W. Siebert, Eur. J. Znorg. Chem., 2002,2064. T. Lange, U. Bohme and G. Roewer, Znorg. Chem. Commun., 2002,5,377. C. Gabriela, T. Reka, B. Delia, J. Oxana and I. Silaghi-Dumitrescu, Studia Uniuersitatis Babes-Bolyai, Chemia, 1999,44, 177. H. Abu Ali, I. Goldberg, D. Kaufmann, C. Burmeister and M. Srebnik, Organometallics, 2002, 21, 1870. M. Suginome, T. Fukuda and Y. Ito, J. Organomet. Chem., 2002,643,508. L. Weber, A. Rausch, H.B. Wartig, H.G. Stammler and B. Neumann, Eur. J. Znorg. Chem., 2002, 2438. P. Nguyen, R.B. Coapes, A.D. Woodward, N.J. Taylor, J.M. Burke, J.A.K. Howard and T.B. Marder, J. Organomet. Chem., 2002,652,77. M. Sanchez, T.S. Keizer, S. Parkin, H. Hopfl and D.A. Atwood, J. Organomet. Chern., 2002,654, 36. H.I. Beltran, L.S. Zamudio-Rivera, T. Mancilla, R. Santillan and N. Farfan, J. Organomet. Chem., 2002,657, 194. H.I. Beltran, S.J. Alas, R. Santillan and N. Farfan, Can. J. Chem., 2002,80, 801. J. Rohovec, J. Kotek, J.A. Peters and T. Maschmeyer, Eur. J. Org. Chem., 2001,3899. T.M.B. Islam, K. Yoshino, H. Nomura, T. Mizuno and A. Sasane, Anal. Sci., 2002,18,363. Y. Nishihara, K. Nara and K. Osakada, Inorg. Chem., 2002,41,4090. H. Abu Ali, A. El Aziz A1 Quntar, I. Goldberg and M. Srebnik, Organometallics, 2002, 21, 4533. T. Ishiyama, J. Takagi, J.F. Hartwig and N. Miyaura, Angew. Chem., Int. Ed. Engl., 2002, 41, 3056. A.G. Avent, S.E. Lawrence, M.M. Meehan, T.G. Russell and T.R. Spalding, Collect. Czech. Chem. Commun., 2002,67,1051. M. Zaidlewicz and A. Wolan, J. Organomet. Chem., 2002,657,129. M. Enders, G. Ludwig and H. Pritzkow, Organometallics, 2002,21,3856. M.J. Bayer, H. Pritzkow and W. Siebert, Eur. J. Znorg. Chem., 2002,1293. M. Yamashita, K. Kamura, Y. Yamamoto and K. Akiba, Chem.-Eur.J., 2002,8,2976. V.N. Plakhotnyk, R. Schmutzler, L. Ernst, Y.V. Kovtun and A.V. Plakhotnyk, J. Fluorine Chem.,2002,116,41. J.A. Perdigon-Melon, A. Auroux, D. Cornu, P. Miele, B. Toury and B. Bonnetot, J. Organomet. Chem., 2002,657,98. C. Duriez, E. Framery, B. Toury, P. Toutois, P. Miele, M. Vaultier and B. Bonnetot, J . Organomet. Chem., 2002,657,107. K.B. Ma, H.W. Lerner, S. Scholz, J.W. Bats, M. Bolte and M. Wagner, J. Organomet. Chem., 2002,664,94. F. Cheng, B. Toury, S.J. Archibald and J.S. Bradley, J . Organomet. Chem., 2002,657,71.
100
[(2-C12B-3,5But2C6H2CH NCH2)2],( 11B),1404(154), ('lB),1405oligonucleoside boranophos= phates, (10B),1406 4,4-Ph2-1,3,2-dioxaborolan-2-y1 carbonyls, (11B),1407 boron and silicon containing oligomers, ("B),'408 (155), ("B),1409and [BF4]-, ('1B).1410
[2-Br-1,3-Et~-2,3-H2-H-1,3,2-benzodiazaborole], (''B),l4O3
Complexes of Other Group 13 Elements. - The change in the 'H NMR spectrum of [AlMe3] produced by the complexation of THF has been cal~ u 1 a t e d .ll Isomers of [Me2MN(H)CH2Ph], have been assigned using 'H and ~~ 13CNMR spectros~opy.'~'~ 'H and 13CNMR spectra of [R2AlN(CH2Ph)2]2 The have been assigned.1413NMR data have also been reported for [(3,5-But2pz5.3
1403
1404
1405
1406
1401
1408 1409
1410
141 1 1412
1413
L. Weber, H.B. Wartig, H.G. Stammler, and B. Neumann, Z. Anorg. Allg. Chem., 2002, 627, 2663. T.S. Keizer, L.J. De Pue, S. Parkin and D.A. Atwood, Can. J. Chem., 2002,80, 1463. 2002,124,1864. T.S. Keizer, L.J. De Pue, S. Parkin and D.A. Atwood, J. Am. Chem. SOC., D.S. Sergueev, Z.A. Sergueeva and B.R. Shaw, Nucleosides, Nucleotides & Nucleic Acids, 2001, 20,789. S . Toyota, M. Asakura and T. Sakaue, Bull. Chem. SOC.Jpn., 2002,752667. G. Ambadas, S. Packirisamy and K.N. Ninan, J. Mater. Sci. Lett., 2002,21, 1003. S . Thormeier, B. Carboni and D.E. Kaufmann, J. Organomet. Chem., 2002,657,136. P.K. Baker, M.G.B. Drew and D.S. Moore, J. Organomet. Chem., 2002, 664, 45; P.K. Baker, M.G.B. Drew and D.S. Moore, J. Organomet. Chem., 2002,658,77. J.A. Tossell, Organometallics, 2002,21,4523. E.K. Styron, C.H. Lake, D.H. Powell, L.K. Krannich and C.L. Watkins, J. Organomet. Chem., 2002,649, 78. E.K. Styron, C.H. Lake, D.H. Powell, C.L. Watkins and L.K. Krannich, Polyhedron, 2002,21, 1747.
101
(154)
(155)
CH = CSiMe3)AlH2], (27Al, 29S1),1414 [(AlH)6(AlNMe2)2(CCH2CH2SiMe3)6], (27Al, [( OSiPh20SiPh20)(GaH)2( OBu'),], (29si),141 29si),141 [But3Al(NH2CH2)2CMe2], (27~1),1417 [K(THF){2,6Pri2C6H3N(SiMe3)}Al(C=CPh)3]2,' (29Si), 1 4 [(q5-C5Me5)Ga], (71Ga),1419 [M2Ga@iB~t3)4], (M = Na, K; 29Si),'420 [(BUt3S1)6Ga8], (29s1), ' 142 [C3H6Si(NBut)2(AlMe2)2], [C3H6Si(NB~t)2Sn]2, 'I9Sn), (27Al, 1422 [Me2Al(OC6H22-CH-4,6-Bul2)I3, (27Al),1 42 [Me2GaBi(SiMe3)2I3, (29Si),1424 [M-{ (2,4,6Me3C6H2)B(OH)O}GaMe2]2, 'B),142 [( Me3Si)3CA1Me(02CCF3)]2, 1426 (' (29Si), [(CH2= CHCH2)2Al(p-OCH2CH2NMe2)]2, (27A1),'427 [MeAl(p-NBut)(pO)P(NHBU')~]~, (27Al), 142 [( MeA1)(2,6-Pr'2C6H3N)3{ OP(OSiMe3)3] A1[ }2(03POSiMe3)],(29Si),'429(156), (R = xanthene or anthracene, 27A1),1430 [(Salophen)(THF)Bu'A102PHPh12, (27Al),43 ' [ B U ' ~ A ~ ~ A ~ ~ B ~ O ~ (Ar ~ H ~ N ) ] , (C = 2,6-Pi2C6H3; I B, 27Al),1 432 [Bu'A1(OCMe2CH2CMe20)I2, (27A1),1 43 [Al(OSiPh3)2{ SiMe3)3}( F)], (27Al,29Si), C( TH l4 [Ga(q5-P3C2B~'2)], (71Ga), '
1414
1415
l4I6
1417
1' 4*
1419
1420
1421 1422
1423
1424
1425
1426
1427
1428
1429 1430
1431
1432
1433
1434
1435
W.J. Zheng, H.W. Roesky, N.C. Mosch-Zanetti, H.G. Schmidt and M. Noltemeyer, Eur. J. Inorg. Chem., 2002,1056. A. Stasch, M. Ferbinteanu, J. Prust, W.J. Zheng, F. Cimpoesu, H.W. Roesky, J. Magull, H.G. Schmidt and M. Noltemeyer, J. Am. Chem. SOC.,2002,124,5441. M. Veith, H. Vogelgesang and V. Huch, Organometallics, 2002,21,380. S.J. Obrey, S.G. Bott and A.R. Barron, J. Organomet. Chem., 2002,643,53. M. Schiefer,H. Hatop, H.W. Roesky, H.G. Schmidt and M. Noltemeyer, Organometallics, 2002, 21, 1300. P. Jutzi and L.O. Schebaum, J. Organomet. Chem., 2002,654,176. N. Wiberg, T. Blank, M. Westerhausen, S. Schneiderbauer, H. Schnockel, I. Krossing and A. Schnepf, Eur. J . Inorg. Chem., 2002,351. N. Wiberg, T. Blank, H. Noth, M. Suter and M. Warchhold, Eur. J. Inorg. Chem., 2002,929. S.-J. Lee, Y.-J. Lee, S.H. Kim, J.-j. KO,S. Cho and S.O. Kang, Organometallics, 2002,21, 5358. A. Cottone, D. Morales, J.L. Lecuivre and M.J. Scott, Organometallics, 2002,21,418. F. Thomas, S. Schulz and M. Nieger, Organometallics, 2002,21,2793. R. Anulewicz-Ostrowska, S. Lulinski, E. Pindelska and J. Serwatowski, Inorg. Chem., 2002,41, 2525. H. Hatop, M. Ferbinteanu, H.W. Roesky, F. Cimpoesu, M. Schiefer, H.G. Schmidt and M. Noltemeyer, Inorg. Chem., 2002,41, 1022. H. Schumann, J. Kaufmann, S. Dechert and H.-G. Schmalz, Tetrahedron Lett., 2002,43,3507. P. Blais, T. Chivers, G. Schatte and M. Krahn, J. Organomet. Chem., 2002,646,107. J. Pinkas, J. Lobl, D. Dastych, M. Necas and H.W. Roesky, Inorg. Chem., 2002,41,6914. A. Cottone and M.J. Scott, Organometallics, 2002,21,3610. Y. Wang, S. Parkin and D. Atwood, Inorg. Chem., 2002,41,558. B. Richter, A. Meetsma, B. Hessen and J.H. Teuben, Angew. Chem.,Int. Ed. Engl., 2002,41,2166. W. Ziemkowska, S. Kwaniewska, R. Wroblewski and R. Anulewicz-Ostrowska, J. Organomet. Chem., 2002,651,72. A.G. Avent, C. Eaborn, I.B. Gorrell, P.B. Hitchcock and J.D. Smith, J . Chem. SOC., Dalton Trans., 2002, 397 1. M.D. Francis, P.B. Hitchcock, J.F. Nixon, H. Schnockel and J. Steiner, J. Organomet. Chem., 2002,646,191.
102
[Ga22{N(SiMe3)2}10]2-, (71Ga),'436 and [ ( B u ~ ~ S ~ ) ~ M ~ S ~ ~ ] , T1; 29Si, (M = In, 77Se).'437
But But But But
27AlNMR spectroscopy has been used to investigate the influence of cation type on aluminosilicate solutions.1438 The compartmentation of aluminium in the leaves of an aluminium accumulator has been studied by 27Al NMR spectros c ~ p y . *05TlTImeasurements have been made on [T1(OH)n(OH2)6-,]3+'as a '~~~ function of magnetic field.1440 27AlNMR spectroscopy shows the predominance of [Al2Cl7]- in [l-Et-3-Me-imidazolium][A12C17].1441 data have also NMR (157), (27A1),1443 been reported for [X3MN(SnMe3)3], = Al, Ga, In; 119Sn),'442 (M Al"' complexes of azo dyes derived from anthranilic acid, (I5N,27A1),'444 Al"' complexes of N-arylsalicylaldimine, (27A1),1 445 [(PhN = CHC6H4-20)2Al(OPr')(p-OPri)2A1(OPri)2],446 Ga"' complex of 2-acetylpyridine N (27Al),1 4-dimethylthiosemicarbazone, ( 15N, 71Ga), 447 [TI{ (H2NCH2CH2)2NH)2l3 +, (205T1),1448 phenanthroline-T13 complexes, ("'Tl), 1449 [(AlCl)4(p3-PR)2(p(27~1),1450 [(THF)3Li(Pri3Si)A~ p= Ga{ PR)2(0Et2)23, A~(siPr'~)}~Ga = AS(S~P?~)L~(THF)~], (29Si),145 [GaCl(PPr"2Ph)(SbSiPri3)]2, '
+
1436
1437
1438 1439
1440
1441
1442
1443
1444
1445
1446
1447
1448 1449
10 4 '
1451
A. Schnepf, G. StoDer and H. Schnockel, Angew. Chem., Znt. Ed. Engl., 2002,41,1882. N. Wiberg, T. Blank, K. Amelunxen, H. Noth, H. Schnockel, E. Baum, A. Purath and D. Fenske, Eur. J . Znorg. Chem., 2002,341. N. Azizi, R.K. Harris and A. Samadi-Maybodi, Magn. Reson. Chem., 2002,40,635. R. Shen, J.F. Ma, M. Kyo and T. Iwashita, Planta, 2002,215,394. A. Bodor, I. Banyai, J. Kowalewski and J. Glaser, Magn. Reson. Chem., 2002,40,716. S.J. Nara, J.R. Harjani and M.M. Salunkhe, J. Org. Chem., 2001,66,8616. Q.M. Cheng, 0.Stark, K. Merz, M. Winter and R.A. Fischer, J. Chem. SOC.,Dalton Trans., 2002, 2933. Z.Y. Zhong, P.J. Dijkstra and J. Feijen, Angew. Chem., Znt. Ed. Engl., 2002,41,4510. A. Lycka, D. Lustinek, J. Holecek, M. Nadvornik and M. Holcapek, Dyes Pigm., 2001,50,203. M. Goyal, S. Mishra and A. Singh, Main Group Met. Chem., 2001,24,829. N. Sharma, R.K. Sharma, R. Bohra, J.E. Drake, M.B. Hursthouse and M.E. Light, . . I Chem. SOC.,Dalton Trans., 2002, 1631. V.B. Arion, M.A. Jakupec, M. Galanski, P. Unfried and B.K. Keppler, J . Znorg. Biochem., 2002, 91,298. M. Kritikos, G.B. Ma, A. Bodor and J. Glaser, Znorg. Chim. Acta, 2002,331,224. G.B. Ma and J. Glaser, Chin. Chem. Lett., 2002,13,695. C . von Hanisch and F. Weigend, 2. Anorg. Allg. Chem., 2002,628,389. C. von Hanisch and 0.Hampe, Angew. Chem., Int. Ed. Engl., 2002,41,2095.
103
(29Si),'452 polyaluminium chloride, (27A1),145 alumina aerogels in the presence of a complexing agent, (27A1),1454[Al(OR)4]-, (27A1),145 [(a~ac)~Al(p OPri)2Al(ON CMeC4H3S-2),], = (27~1),146 5 [(acac)2A1(p(27A1),1457 [ZnM2(OR)s],(M = Al, Ga; 27A1),1458 OCH2CH20)Al(OCH2CH20)], [A15(~5-O)(p-OBui)8(OBu')5], 459 organic acid masked aluminium sulfate (27A1),1 1460 J2, (27Al), 146 [Ga(S2CNR2)3], (71Ga),'462 complexes,(27Al), [Al( ~-SBU')(SBU')~ [C~I~{T~(NBU')~}~], [AlChJ- and [Al2C17I2-, (27A1).1464 ('25Te),'463
But
But
Group 14 Compounds
Six reviews have appeared entitled 'Silicon chemistry: [R3SiJ+- Free at last', 46 (29Si),1 'Unusual behaviour of silicon oligomers and polymers having functional groups', (29Si),'466 NMR analysis as a useful tool for structural 'I3C 'Synthetic applicaassignment of vinyl- and dienyltin derivatives', ( I 19Sn),'467 tions of a series of organotin hydrides', ( I 19Sn),'468 '[Organotin(IV)P complexes formed with biologically active ligands: equilibrium and structural studies, and some biological aspects', (119Sn),1469 'Application o 207PbNMR parand f ameters'.'470
1452 1453 14s4
14"
1456 1457
* ' 4 1
14s9
1460
1461 1462 1463

1464 1465
1466 1467
1" 4
1469 1470
C. von Hanisch, P. Scheer and B. Rolli, Eur. J. Znorg. Chem., 2002,3268. L.-S. Kang, S.-W. Han and C.-W. Jung, Korean J. Chem. Eng., 2001,18,965. L. Le Bihan, F. Dumeignil, E. Payen and J. Grimblot, J. Sol-Gel Sci. Technol.,2002,24,113. M. Gonsio, 1. Krossing, L. Muller, I. Raabe, M. Jansen and L. van Wullen, Chem.-Eur.J., 2002, 8,4475. N. Sharma, R.K. Sharma and R. Bohra, Main Group Met. Chem., 2001,24,781. S . Nagar, R. Bohra and R.C. Mehrotra, Main Group Met. Chem., 2002,25, 277; S. Nagar, A. Dhammani, R. Bohra and R.C. Mehrotra, J. Coord. Chem.,2002,55,381. S . Daniele, D. Tcheboukov and L.G.H. Pfalzgraf, J. Phy. ZV:Proc., 2001,11,283. I. Abrahams, D.C. Bradley, H. Chudzynska, M. Motevalli and R.A. Sinclair, J. Chem. Soc., Dalton Trans., 2002,259. K.Ding, T. Zhang and Y.He, Zhongguo Pige, 2001,30,3. S. Daniel and D.M. Hoffman, Inorg. Chem., 2002,41,3843. D.P. Dutta, V.K. Jain, A. Knoedler and W. Kaim, Polyhedron, 2002,21,239. T. Chivers and G. Schatte, Eur. J. Inorg. Chem., 2002,2266. V.V. Namboodiri and R.S. Varma, Chem. Commun., 2002,342; 917. P.P. Gasper, Science (Washington, DC, U.S.), 2002,2!W,785. Y. Hatanaka, Yuki Gosei Kagaku Kyokaishi, 2001,59,996. J.-F. Betzer, P. Le Menez, J. Prunet, J.-D. Brion, J. Ardisson and A. Pancrazi, Synlett, 2002,l. I. Shibata, T. Suwa and A. Baba, Main Group Met. Chem., 2001,24,637. L. Pellerito and L. Nagy, Coord. Chem. Rev., 2002,224,111. B. Wrackmeyer, Annu. Rep. N M R Spectrosc., 2002,47,1.
104
29SiNMR shifts and relative stabilities for hypercoordinated silicon-polyalcoho1 complexes,1471 [SinH2n+211472 been calculated. NMR data have and have also been reported for [1-H3Si-2-MeOC6H4], (29Si),1473 [(But2MeSi)2SiH2], (29Si),'474( B U ' M ~ ~ S ~ ) ~ S(7Li,29Si),'475 [ ~HL~], [(CH2 = CH)3B], [MeSiH(C=CR)2], (1 'B, 29si),1 4 7 6 [R'2R2Si(CH2)2SiH],, (29Si), 147 [{ B U N ( C H ~ C ~ H ~ ) ~ } S ~ H P ~ ] , (29Si),1478 (158), (29Si),1479 [HSiMe20(SiMe20),SiMe2H], (29Si),'480 [(PhSiH),], 29Si).'482 (29Si),1481 (159), (15N, and
J(29Si29Si) J(29Si'3C) and and 12C,13C(29Si) 28Si,29Si(13C) and isotope induced shifts have been determined for silenes stabilised by intramolecular N-Si coordination. 1 4 8 3 Exceptionally small ' J ( '19Sn13C) values have been observed in some organometallic substituted s t a n n 0 1 e s . l ~1J(29Si'3C) ~~ indicates that the Si = C = bond order is smaller in [(Bu'Me2Si)(Me3Si)Si (2-adamantyl)] than in simpler ~ i 1 e n e s . A~ relationship between the half-width of 73GeNMR signals and l ~~ hyperconjugation has been observed in some ~ h e n y 1 g e r m a n e s . 'H,'17Sn J l~~~ HMBC NMR spectroscopy has been implemented as a tool for the determinaI7Sn1H) 2-Me2NCH2C6H4 t a n n a n e sDFT calculaof ~ .~~~~ tion of long range "J(l tions of '19Sn chemicals shifts have been carried out using gauge-including atomic orbitals and interpretated via group proper tie^.'^^' NMR data have also been reported for [Me4Sn], (119Sn),'489 [Me3SiR], (29Si),'490 [(Me3Si)2R1SiR2],
1471 1472 1473 1474
1475 1476
1477 1478 1479 1480 1481
1482 1483 1484 1485
1486 1487
1488
N. Sahai and J.A. Tossell, Inorg. Chem., 2002,41,748. C. Corminboeuf, T. Heine and J. Weber, Chem. Phys. Lett., 2002,357,l. 0.Minge, N.W. Mitzel and H. Schmidbauer, Organometallics, 2002,21,680. A. Sekiguchi, T. Fukawa, M. Nakamoto, V.Y. Lee and M. Ichinohe, J. Am. Chem. SOC., 2002, 124,9865. T. Iwamoto, J. Okita, C. Kabuto and M. Kira, J. Am. Chem. Soc., 2002,124,ll 604. B. Wrackmeyer, O.L. Tok, M.H. Bhatti and S. Ali, Collect. Czech. Chem. Commun., 2002, 67, 822. R. Shankar, A. Saxena and A.S. Brar, J. Organomet. Chem., 2002,650,223, K. Saruhashi, K. Goto and T. Kawashima, Chem. Hetrocycl. Compd. ( N . Y.),2001,37,1394. B.-H. Kim and H.-G. Woo, Organometallics, 2002,21,2796. J.M. Mabry, M.K. Runyon and W.P. Weber, Macromolecules, 2002,35,2207. F.G. Fontaine and D. Zargarian, Organometallics, 2002, 21, 401; B.J. Grimmond and J.Y. Corey, Inorg. Chim. Acta, 2002,330,89. A.A.E. Ahdab, G. Rima, H. Gornitzka and J. Barrau, J. Organomet. Chem., 2002,6658,94. B. Wrackmeyer and H. Oehme, 2. Naturjiorsch., B: Chem. Sci., 2001,56,947. B. Wrackmeyer, G. Kehr, S. Willbold and S. Ali, J. Organornet. Chem., 2002,646,125. M. Bendikov, Y. Apeloig, S. Bukalov, I. Garbuzova and L. Leites, J. Phys. Chem. A , 2002,106, 4880. Y. Takeuchi, K. Tanaka, S. Aoyagi and H. Yamamoto, Magn. Reson. Chem., 2002,40,241. M. Biesemans, J.C. Martins, R. Willem, A. Lycka, A. Ruzicka and J. Holecek, Magn. Reson. Chem., 2002,40,65. R. Vivas-Reyes, F. D Proft, M. Biesemans, R. Willem and P. Geerlings, J. Phys. Chem. A , 2002, e 106,2753.
105
(29si),'49 (la), (29Si),'492 (161), (29Si),'493 [(Me3Si)2C(p-SiC12)2PPButPri], ' (29si), 1494 (162),(29si),'495 (29Si), (163), 1496 [Sn{ C(SiMe3)3}(pSBut)2Li(THF)2], (7Li, 29Si,119Sn),1497 [1,4-{(Me3SiCH2)C12SnCH2SiMe2}2C6H4], (29Si,119Sn),'498 [(Me3SiCH2)2SnX2], (29Si, 119Sn),'499 (Me3Si)3C}SnO]3, lL9Sn),' ( W , [Cl{ (29Si, (R = PhCH2; 29Si, 119Sn),1s01 (la), (R = E ; X = I; 29Si, 1'9Sn),f502 t [(Me&)2SiFCH(SiMe3)CH = CMe2], (29Si),1 [Np2Si(X)SiMe3], (29Si),1 '03 [ M 3 i 3 i S H S M 3 ( S M 3(29Si),' 0 5 (165), (29Si),' (eS)SOi(ie)Oie), ' ] '06 C(Me3Si)n Me3-,SiEHJ, (E = S, Se, Te; 29Si, "Se, 12sTe),1507 (I&), (29Si),'508 [(Me3SiO)(Me3Si)2SiCH2CButCBu'(OBu')], (29Si),' (167),(29Si,i19Sn),1 o = l [Bi{ Si(SiMe3)3}2]-, (29Si),'1 ' (E)-[Me3SnCH =C(BEt2)EtJ, ("B, 'I9Sn),'12 5 ' [Me(Me3Sn)C= CHMe], (119Sn),'513 [Me3SnC14H1103SJ, ('l9Sn),''14 [(qsA. Althoff, P. Jutzi, N. Lenze, B. Neumann, A. Stammler and H.-G. Stammler, Organometallics, 2002,21,3018. 1490 G. Maier, J. Neudert, 0. Wolf, D. Pappusch, A. Sekiguchi, M. Tanaka and T. Matsuo, J. Am. Chem. Soc., 2002, 124, 13 819; T. Kato, H. Gornitzka, A. Baceiredo, W.W. Schoeller and G. 2002,124,2506; M. Movassaghi and E.N. Jacobsen, J. Am. Chem. Bertrand, J. Am. Chem. SOC., SOC.,2002,124,2456; A. Happer, N.G. Janice, B. Pool and J. White, J. Organomet. Chem., 2002, 659,lO; D. Ostendorf, W. Saak, M. Weidenbruch and H. Marsmann, Organometallics, 2002,21, 636. 1491 C. Kayser, R. Fischer, J. Baumgartner and C. Marschner, Organornetallics, 2002,21,1023. 1492 N. Takeda, A. Shinohara and N. Tokitoh, Organometallics, 2002, 21, 256; N. Takeda, A. Shinohara and N. Tokitoh, Organometallics, 2002,21,4024. 1493 J. Ohshita, H. Kai, T. Sumida, A. Kunai, A. Adachi, K. Sakamaki and K. Okita, J. Organomet. Chem., 2002,642,137. 1494 W.-W. du Mont, T. Gust, E. Seppalii,C. Wismach, P.G. Jones, L. Ernst, J. Grunenberg and H.C. Marsmann, Angew. Chem., Int. Ed. Engl., 2002,41,3829. 1495 C. Ackerhans, H.W. Roesky, T. Labahn and J. Magull, Organornetallics, 2002,21,3671. 1496 A. Sekiguchi, R.Izumi, S. Ihara, M. Ichinohe and V.Y. Lee, Angew. Chem., Int. Ed. Engl., 2002, 41, 1598. 1497 I.V. Borisova, C. Eaborn, M.S. Hill, V.N. Khrustalev, M.G. Kuznetzova, J.D. Smith, Y.A. Ustynyuk, V.V. Lunin and N.N. Zemlyansky, Organometallics, 2002,21,4005. 1498 D. Dakternieks, A. Duthie, B. Zobel, K. Jurkschat, M. Schurmann and E.R.T. Tiekink, Organornetallics, 2002,21,647. 1499 J. Beckmann, M. Henn, K. Jurkschat, M. Schurmann, D. Dakternieks and A. Duthie, Organometallics, 2002,21, 192. "O0 J. Janssen, J. Magull and H.W. Roesky, Angew. Chem.,Int. Ed. Engl., 2002,41,1365. "O' A. Asadi, A.G. Avent, C. Eaborn, M.S. Hill, P.B. Hitchcock, M.M. Meehan and J.D. Smith, Organometallics, 2002,21,2183. 1502 A. Asadi, C. Eaborn, M.S. Hill, P.B. Hitchcock, M.M. Meehan and J.D. Smith, Organometallics, 2002,21,2430. 1503 K. Schmohl, D. Wandschneider, H. Reinke, A. Heintz and H. Oehme, Eur. J. Znorg. Chem., 2002, 597. 504 K. Tamao, M. Asahara, A. Kawachi and A. Toshimitsu, J. Organomet. Chem., 2002,643,479. " 0 5 T.A. Chesnokova, E.V. Zhezlova, A.N. Kornev, Y.V. Fedotova, L.N. Zakharov, G.K. Fukin, Y.A. Kursky, T.G. Mushtina and G.A. Domrachev, J. Organomet. Chem., 2002,642,20. 506 K. Sakamoto, J. Ogasawara, Y.Kon, T. Sunagawa, C. Kabuto and M. Kira, Angew. Chem., Int. Ed. Engl., 2002,41, 1402. 1507 H. Lange and U. Herzog, J. Organomet. Chem., 2002,660,36. D. Bravo-Zhivotovskii, S. Melamed, M. Kapon and Y. Apeloig, Organometallics, 2002,21,2049. 1509 A. Naka, J. Ikadai, S. Motoike, K. Yoshizawa, Y. Kondo, S.Y. Kang and M. Ishikawa, Organometallics, 2002,21,2033. l 5 l 0 C. Kayser, G. Kickelbick and C. Marschner, Angew. Chem., Int. Ed. Engl., 2002,41,989. 1 5 1 1 G. Linti, W. Kostler and H. Pritzkow, Eur. J. Inorg. Chem., 2002,2643. 1 5 1 2 B. Wrackmeyer, H.E. Maisel and K. Wagner, Chem. Hetrocycl. Compd. (N. Y.),2001,37,1396. 1 5 1 3 J.C. Cochran, V. Prindle, H.A. Young, M.H. Kumar, S. Tom, N.D.K. Petraco, C. Mohoro and B. Kelley, Synth. React. Inorg. Met.-Org. Chem., 2002,32, 885.
1489
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106
Spectroscopic Properties o Inorganic and Urganometallic Compounds f
C5H5)Fe(q5-C5H4)SiMe2(indenyl)], (29Si),' ' (168), (29Si, l19Sn),' ' (1691, (29si), ' [3-MeC6H4CH2SiMe2CH20H], (29Si),1 ' [Me2Si(CH2R)CH2CH(NH2)C02H], (29Si),' ' [PhCHMeSiMe2CH2(2-MeOCH2-pyrrole)], (29si),1520 B U ' M ~ ~ S ~ ) ~ S ~ P5~ 1 [C6H6(SiMe2CH2)2CH2], 5 2 2 (170), [( (29Si),'2 ~ ] , (29Si),' (171), (29Si),1 [{ ( C ~ F I ~ C ~ ~ C H M ~ C H ~ ) M (29si),12 } ~ S ~ ~ O ~ 24 ~~S5 ~ (119Sn),'523 (172), (' 19Sn),' [Ar2SnMe2], ('19Sn),' [{ C H ( 0 2 ( H ) S M 2 2 C 2 6 , 64C)NC23ie}(H)] (15N, 29si),1528 [Si4(CH2)6Me3( OTf)], (29si), 29 (173), (29Si),1 (174), (29Si),1 ' ' 30 (175), (7Li, 29Si),' 532 [(BU'~S~)~M~S~S~X = S~XM~(S~BU'~)~], 533 (29Si),' [MePh2SiCPh= CHB(C6H2-2,4,6-Me3)2], 29si), 34 [Ph2MeSiSiMePhCH2NCsHlo],(29Si),' 3 5 silylated carboxonium ions, (29Si),1 5 536 [HOCH2SiPh(Cy)CH2CH2NCsHlo], (29Si),' 537 (176), (29si), ' [(Bu$Si)MeSi= SiMe(SiBut3)], (29Si),' 539 [( B~'3Si)SiPh(p.-Se)~SiPh( SiBut3)], [(But&)SiPh(p-Te)SiPh(SiBut3)],(29Si,77Se, '"Te),' 540 [1,2,3,4-&-1,2,3,4-PhSLI, (29si),54 (177), (29si), '542 (17% (29si),' 543 [Me2Sn(OCOCHR1CHR2GeR33)2], (119Sn),'544[Bun3SnSH2SR], (119Sn),1545
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"I4
F. Ahmad, M. Parvez, S. Ali, M. Mazhar and A. Munir, Synth. React. Inorg. Met.-Org. Chem., 2002,32,665. "" M. Herberhold, A. Ayazi, W. Milius and B. Wrackmeyer, J. Organomet. Chem., 2002,656,71. M. Schurmann and F. Uhlig, Organometallics, 2002,21,986. L.E. Gusel'nikov, V.V. Volkova, E.N. Buravtseva, A.S. Redchin, N. Auner, B. Herrschaft, B. Solouki, G. Tsantes, Y.E. Ovchinnikov, S.A. Pogozhikh, F.M. Dolgushin and V.V. Negrebetsky, Organometallics, 2002,21, 1101. R . Tacke, T. Schmid, C. Burschka, M. Penka and H. Surburg, Organometallics, 2002,21,113. 1 5 1 9 R. Tacke and V.I. Handmann, Organometallics, 2002,21,2619. 1520 C. Strohmann, K. Lehmen, K. Wild and D. Schildbach, Organometallics, 2002,21,3079. 1 s 2 1 M. Kira, T. Iwamoto, T. Muruyama, T. Kuzuguchi, D.Z. Yin, C. Kabuto and H. Sakurai, J. Chem. SOC.,Dalton Trans., 2002, 1539. R. Meyer, K. Werner and T. Muller, Chem.-Eur.J., 2002,8, 1163. M. Huttenhofer, F. Schaper and H.H. Brintzinger, J . Organomet. Chem., 2002,660,85. M.J. Hanson, M. Spiniello and J.M. White, J. Organomet. Chem., 2002,654, 3. D. Hoebbel, C. Weber, H. Schmidt and R.-P. Krueger, J . Sol-Gel Sci. Technol., 2002,24,121. 1s26 G.P.M. van Klink, H.J.R. de Boer, G. Schat, O.S. Akkerman, F. Bickelhaupt and A.L. Spek, Organometallics, 2002,21,2119. P. Apodaca, F. Cervantes-Lee and K.H. Pannell, Main Group Met. Chem., 2001,24,597. J.O. Daiss, S. Duda-Johner, C. Burschka, U. Holzgrabe, K. Mohr and R. Tacke, Organometallics, 2002, 21, 803. K.K. Laali, G.F. Koser, S.P.D. Huang and M. Gangoda, J. Organomet. Chem., 2002,658,141. A. Naka, M. Ishikawa, S.H. Cha, K.K. Lee and Y.W. Kwak, J. Organomet. Chem., 2002,645,47. V.Y. Lee, M. Ichinohe and A. Sekiguchi, J. Am. Chem. Soc., 2002,124,9962. T. Matsuno, M. Ichinohe and A. Sekiguchi, Angew. Chem., Int. Ed. Engl., 2002,41,1575. 533 N. Wiberg, W. Niedermayer, G. Fischer, H. Noth and M. Suter, Eur. J. Inorg. Chem., 2002,1066. 1s34 J.C.A. Da Silva, M. Birot, J.P. Pillot and M. Petraud, J. Organomet. Chem., 2002,646,179. 153s C. Strohmann, J. Hornig and D. Auer, Chem. Commun., 2002,766. G.K.S. Prakash, C. Bae, G. Rasul and G.A. Olah, J. Org. Chem., 2002,67, 1297. s37 R. Tacke, T. Kornek, T. Heinrich, C. Burschka, M. Penka, M. Pulm, C. Keim, E. Mutschler and G. Lambrecht, J. Organomet. Chem., 2002,640,140. S . Deerenberg, M. Schakel, A. de Keijzer, M. Kranenburg, M. Lutz, A.L. Spek and K. Lammertsma, Chem. Commun., 2002,348. N. Wiberg, W. Niedermayer and K. Polborn, 2. Anorg. Allg. Chem., 2002,628,1045. N. Wiberg, W. Niedermayer, K. Polborn and P. Mayer, Chem.-Eur. J., 2002,8, 2730. H. Lange, U. Herzog, G. Rheinwald, H. Lang and G. Roewer, Main Group Met. Chem., 2002,25, 155. s42 Y.X. Liu, T.C. Stringfellow,D. Ballweg, I.A. Guzei and R. West, J . Am. Chem. SOC., 2002,124,49. M. Oba, Y. Watanabe and K. Nishiyama, Organometallics, 2002,21,3667. 1s44 M.A. Choudhary, M. Mazhar, S. Ali, X.Song and G. Eng, Metal-Based Drugs, 2001,8,275.
"''
''" '
'
107
[(PhCMe2CH2)3SnCR1 CHR')], (lt9Sn),'546 [(2,6-Pr'2C6H~)SnSn(CsH3-2,6= Pf$J, (1'9Sn),' 4 7 [R1R2R3Sn(8-Me2N-1-C10H6)], 5 ("N, '19Sn),' 548 [ArPhzSn]', (It9Sn). (lt9Sn),'549 and [Sn(q4-P2C2B~t2)2], ' 5 0
Ct-$SiMe,
Me,SiH,C
ChSiMe,
R - S i- S k R
Me,Si
SiMe,
Me$
ASiMe,
Me2Si-SiMe
SiMe,
Me3Sk Me,Si/'!
,So ,SiM% Me2

SiM% SiSi Me2 Me2
?'
But
DFT calculations of Il9Sn chemical shifts for [Me3Sn(NC)2]- have been reported.' 5 5 ' I7ONMR spectra have been recorded for some butyitin(1V)acetates. Only one I7Osignal was observed.'552The coordination of tin in triorgano tin cinnamate containing polymers has been investigated by 'I7Sn NMR spectros c ~ p y . ' NMR data have also been reported for (179), (29Si),1554 ~~~ [( MePhCH)(Me3Si)NSiCI3], (29Si), ' [( Me3SiNSNhSe (I4N, 77Se),' 5 6 1, [(Me3Si)(9-borabicyclo[3.3.1]nonyl)NSnC13], ("B, "N, 29Si, I 19Sn),1
154s 1546 1547 1548
1549
1550
1551
1552
1553
1554 1555 1556
R.I. Yousef, T. RiifTer, H. Schmidt and D. Steinborn, J . Organomet. Chem., 2002,655,111. V.I. Dodero, L.C. Koll, S.D. Mandolesi and J.C. Podestk J. Organomet. Chem., 2002,650, 173. A.D. Philips, R.J. Wright, M.M. Olmstead and P.P. Power, J . Am. Chem. Soc., 2002,124,5930. A. Ruzicka, M. Hajny, J. Holecek, A. Lycka and K.Jacob, Scientific Papers o the University of f Pardubice, Series A: Faculty of Chemical Technology, 2002,6,13. A. Ruzicka, L. Dostal, R.Jambor, V. Buchta, J. Brus, I. Cisafova, M. Holcapek and J. Holecek, Appl. Organomet. Chem., 2002,16,315. M.D. Francis and P.B. Hitchcock, Chem. Commun., 2002,86. P. Avalle, R.K. Harris and R.D. Fischer, Phys. Chem. Chem. Phys., 2002,4,3558. A. Lycka and J. Holecek, Magn. Reson. Chem., 2002,40,289. L. Angiolini, E. Salatelli, D. Caretti, M. Biesemans, H. Dalil, R. Willem, N.A. Chaniotakis, E. Gouliaditi and K. Perdikaki, Macromol. Chem. Phys., 2002,203,219. H.-W. Lerner, M. Bolte and N. Wiberg, J. Organomet. Chem., 2002,649,246. M.G. Walawalkar and R. Murugavel, Phosphorus, Sulfur Silicon Relat. Elem., 2001,174,229. J. Konu, A. Maaninen, K. Paananen, P. Ingman, R.S. Laitinen, T. Chivers and J. Valkonen, Znorg. Chem., 2002,41, 1430.
108
But
(170)
But
Me2N- - - SiMe2(CH=CH2)
I I
-Sil Me2
C"'rBut
Si MePh
MePh
But2 Si MeBut2Si -S<-.$-SiBut2Me Li+ ?i SiBut2Me

(174)
(177)
(180), (29Si),1 organotin(1V) complexes of benzil monoxime thiosemi''' carbazone, ("'Sn), [RnSn(PhN2C*S3)4 n3, ( l 19Sn),1 60 P( (CN)(0 = CMe2)], (29Si), [Me3 R], (29Si), SiO CN(CH2CH2NMe)3 SiMe3)
'
'
1557
15"
1559
lS6O
1561
1562
B. Wrackmeyer, A, Pedal1 and J. Weidinger, Z. Naturforsch., B: Chem. Sci., 2001,56, 1009. D. Amsallem, S. Mazieres, V. Piquet-Faurt, H. Gornitzka, A. Baceiredo and G. Bertrand, Chem.-Eur. J., 2002,8,5306. M.S. Singh and K. Tawade, Indian J. Chem., Sect. B: Org. Chem. Incl. Med. Chem., 2002,41B, 419. V. Berceanc, C. Crainic, I. Haiduc, M.F. Mahon, K.C. Molloy, M.M. Venter and P.J. Wilson, J. Chem. SOC., Dalton Trans., 2002, 1036. Z.G. Wang, B. Fetterly and J.G. Verkade, J. Organomet. Chern., 2002,646,161. D.J. Brauer, M. Hingst, K.W. Kottsieper, C. Liek, T. Nickel, M. Tepper, 0. Stelzer and W.S.
109
octa(pentamethyldisiloxy)silsesquioxane, (29Si),' [Me3Si(OSiMe2),0SiMe3], ' (29Si),' [SiMe20],, (29Si),'6 5 triorganotin(1V)complexes with amoxicillin and 564 5 ampicillin, ( I 19Sn),' organotin derivatives of 3-benzoyl-a-methylphenylacetic acid, (' I9Sn),'567 organotin(1V)complexes with 2-(6-methoxynaphthyl)propionic acid, ('''Sn),' 5 6 8 [Me3Sn(2-HOC6H4CMe NCH2C02)], (119Sn),1569 = triorganotin(1V)derivatives of 4-acyl-5-pyrazolones, (' 19Sn),' [R3SnONCMeAr], 570 (' 19Sn),' organotin(1V)derivatives of 4-(4-C1C6H4)-2-Ph-5-thiazoleacetic acid, 5 573 ('19Sn),' 7 2 organotin(1V) complexes of Schiff bases, (l19Sn),' (29si), [PhSiMe2( OSiMe2CH2CH2SiMe2),0SiMe2CH2CH2SiMe20Pri], ' 74 [HC(SiMe2Se)3SnMe], (29Si, 77Se, '19Sn),'5 7 5 [R' SiMe20R2], (29Si),1 6 7 [PhSiF20N(SiMe2But)2], (29si), ' [C1SiMe2P , h] (29si), ' [MeR(HO)SiSi(OH)RMe], (29Si),'79 [C1MePhSi(CH2)&3iPhMeCl],(29Si),'8 0 5 [RCOTeMPPh3], (M = Ge, Sn, Pb; 125Te),'581 [Bu3SnOR], ('17Sn),'5 8 2 butyltin(1V)N-substituted 2-aminoethanethiolates, ( I I9Sn),'583 [(PhMe2CCH2)3SnX], (119Sn),1584 [1-PhCySi(OH)CH2CH2CH2-2-Me-imidazole1, (29si), '
'
'
1s63
1s64
lS6'
1566
1s67
lS6'
1s69
Sheldrick, J. Organomet. Chem., 2002,645,14; V.A. Wright and D.P. Gates, Angew. Chem.,Int. Ed. Engl., 2002,41,2389; B.A. Omotowa, M.R. Judd, B. Twamley and J.n.M. Shreeve, J. Org. Chem., 2002,67,1588; V.R. Ziatdinov, G. Cai and W.P. Weber, Macromolecules, 2002,35,2892; G. Cai and W.P. Weber, Polymer Preprints (Amer. Chem. SOC., Polymer Chem.), 2002, 43, Diu. 530. C. Yuan and C. Hu, Youjigui Cailiao, 2001, 15, 1. J.R. Desmurs, L. Ghosez, J. Martins, T. Deforth and G. Mignani, J. Organomet. Chem., 2002, 646,171. Z. Zhang, N. Zhou, C. Xu and Z. Xie, Youjigui Cailiao, 2001,15,8. R. Di Stefano, M. Scopelliti, C. Pellerito, T. Fiore, R. Vitturi, M.S. Colomba, P. Gianguzza, G.C. Stocco, M. Consiglio and L. Pellerito, J. Znorg. Biochem., 2002,89,279. M.T. Masood, S. Ali, M. Danish and M. Mazhar, Synth. React. Inorg. Met.-Org. Chem., 2002, 32,9. S . Ali, F. Ahmad, M. Mazhar, A. Munir and M.T. Masood, Synth. React. Inorg. Met.-Org. Chem.,2002,32,357. T.S.B. Baul, S. Dutta, E. Rivarola, R. Butcher and F.E. Smith, J. Organomet. Chem., 2002,654,
100.
F. Marchetti, C. Pettinari, A. Cingolani, R. Pettinari, M. Rossi and F, Caruso, J. Organomet. Chem., 2002,645,134. lS7' V. Sharma, R.K. Sharma, R. Bohra and V.K. Jain, Main Group Met. Chem., 2002,25,445. 1s72 S. Ali, M.N. Khokhar, M.H. Bhatti, M. Mazhar, M.T. Masood, K. Shahid and A. Badshah, Synth. React. Inorg. Met.-Org. Chem., 2002,32, 1373. 1573 H.L. Singh, M.K. Gupta and A.K. Varshney, Res. Chem. Intermed., 2001,27,605. 1 5 7 4 K. Matsubara, J. Terasawa and H. Nagashima, J. Organomet. Chem., 2002,660,145. lS7' U. Herzog, G. Rheinwald and H. Borrmann, J. Organomet. Chem., 2002,660,27. 1s76 A.A. Tishkov, A.D. Dilman,V.I. Faustov, A.A. Birukov, K.S. Lysenko, P.A. Belyakov, S.L. Ioffe, Y.A. Strelenko and M.Y. Antipin, J. Am. Chem. SOC., 2002,124,ll 358. 1577 S. Schmatz, F. Diedrich, C. Ebker and U. Klingebiel, Eur. J. Znorg. Chem., 2002,876. lS7' F. Stohr, D. Sturmayr and U. Schubert, Chem. Commun., 2002,2222. 1579 D. Hoffman, H. Reinke and C. Krempner, J. Organomet. Chem., 2002,662,l. 1580 M. Ishikawa, S. Shirai, A. Naka, H. Kobayashi, J. Ohshita, A. Kunai, Y. Yamamoto, S.H. Cha, K.K. Lee and Y.W. Kwak, Organometallics, 2002,21,4206. K. Tani, R. Yamada, T. Kanda, M. Suzuki, S. Kato and T. Murai, Organometallics, 2002, 21, 1487. l S s 2 L. Angiolini, E. Salatelli, D. Caretti, M. Biesemans, H. Dalil, R.Willem, N.A. Chaniotakis, E. Gouliaditi and K. Perdikaki, Macromolecular Chem. Phys., 2002, u)3,219. l S s 3 A. Smicka, V. Buchta and K. Handlir, Met.-Based Drugs, 2001,8,165. lSs4 J.A.S. Bomfim, C.A.L. Filgueiras, R.A. Howie, J.N. Low, J.M.S. Skakle, J.L. Wardell and S. Wardell, Polyhedron, 2002,21, 1667. 1 5 8 5 R. Tacke, V.I. Handmann, K. Kreutzmann, C. Keim, E. Mutschler and G. Lambrecht, OrlS7O
''''
110
[HOPh2SiSiPh20H], (29Si),1 rner-[(Bu3SnO)3Te(OH),1, (Il9Sn,12'Te),' 587 organotin tropolonato complexes, (Il9Sn),'5 8 8 [Cy3SnOR], (119Sn),1589 [( PhCH2)3Sn( 2-N-ethylamino-1-cyclopentene-1-carbodithioate)], ( I9Sn),' 90 [C1(2triorganotin carboxylates containing germanium, (Il9Sn),' Me2NCH2C6H4)SiPhSiPh2Cl], (29Si), ' [2,5-(B~'~FSi)~-furan),(29Si),' [But2SnXSnYBut2], ('I9Sn),'594 [{ 2-(Me2NCH2C6H4)}stannanes], (I5N, 'I9Sn),' 5 9 5 [{ 2,6-(Me2N)2C6H3}2SnClSiC13],'19Sn),' 5 9 6 and [4-But-2,6(29Si, { P(O)(OEt)2}2C2H2PbPh3], (207Pb).1 597
'
''
29Si NMR spectroscopy has been used to establish the sequencedistribution in polymers from 2,2,4,4,-Me4-6,6-Ph2-cyclotrisiloxane. H relaxation and pul98 sed gradient NMR diffusion measurements of ultrasonically devulcanised triple resonance poly(dimethylsi1oxane) have been reported. '599 1H,13C,29Si three-dimensionalNMR spectroscopycombined with pulsed field gradient techniques has been used for characterising [Me2Si0],.'600 The sequencing of the siloxane units in a polymer has been performed using 29SiNMR spectrocopy.'^^' The structural changes which occur on the y-radiolysis of [Me2SiO], have been investigated by I3C and 29SiNMR spectroscopy.'602 The effect of phenyl content on the degradation of poly (dimethyl diphenyl) siloxane
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1586
1587
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1589
1590
1591
1592
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1596 1597 1598 1599 1600 1601
1602
ganometallics, 2002,21,3727. R. Tacke, J. Heermann, M. Penka, I. Richter and B. Wagner, 2.Naturforsch., B: Chem. Sci., 2002,57,731. J. Beckmann, D. Dakternieks, J. O'Connell, K. Jurkschat and M. Schurmann, Eur. J. Inorg. Chem., 2002,1484. C. Camacho-Camacho, R. Contreras, H. Noth, M. Bechmann, A. Sebald, W. Milius and B. Wrackmeyer, Magn. Reson. Chem., 2002,40,31. J.-x. Li, Y.-p. Xiao, Q. Liu, B.-z. Zhao, J.-f. Liu, Y.Xing, H.-q. Jia and Y.-h. Lin, Gaodeng Xuexiao Huaxue Xuebao, 2001,22,1667. A. Tarassoli, A. Asadi and P.B. Hitchcock, J. Organomet. Chem., 2002,645,105. M.A. Choudhary, M. Mazhar, S. Ali, U.-E. Salma, S. Ashraf and A. Malik, Turk. J. Chem., 2002, 26, 125. J. Belzner, U. Dehnert, D. Schar, B. Rohde, P. Muller and I. Uson, J. Organomet. Chem., 2002, 649,25. U. Klingebiel,P. Neugebauer, I. Muller, M. Noltemeyer and I. Uson, Eur. J. Inorg. Chem., 2002, 717. U. Englich, U. Hermann, I. Prass, T. Schollmeier, K. Ruhlandt-Senge and F. Uhlig, J. Organomet. Chem., 2002,646,27 1. A. Ruzicka, Chem. Listy, 2001,%, 807. C. Drost, P.B. Hitchcock and M.F. Lappert, Organometallics, 2002,21,2095. K. Peveling, M. Schurmann and K. Jurkschat, 2. Anorg. Allg. Chem., 2002,628,2435. M. Cypryk, Polimery (Warsaw, Poland), 2001,46,468. S.E. Shim, J.C. Parr, E. von Meerwall and A.I. Isayev, J. Phys. Chem. B, 2002,106,12 072. M. Chai, P.L. Rinaldi and S. Hu, ACS Symp. Ser., 2003,834, 137. J. Chojnowski, M. Cypryk, W. Fortuniak, K.Rozga-Wijas and M. Scibiorek, Polymer, 2002,43, 1993. D.J.T. Hill, C.M.L. Preston and A.K. Whittaker, Polymer, 2001,43,1051.
111
copolymers has been studied using 29Si NMR s p e c t r o ~ c o p y .NMR data have '~~~ also been reported for [(R1R2Si)X],, (29Si),' organotin(1V) derivatives of '04 MeNHCH2C02H,('I9Sn),'' 0 5 Schiff base amino acid complexes of Me2Si0, (29Si),'06 carbosiloxane dendrimers with a Me2Si02core, (29Si),' poly(sily1 ' 607 ethers), (29Si),1 8 poly(silary1ene and silalkylene silsesquioxane) networks, '0 (29Si), functionalisedsilsesquioxanes,(29Si),1 polymethylsioxane, (29Si),' '' ''09 ' diphenyl dimethyl polysiloxane, (29Si),1 " [{ R2SnON= CMe(py)}20]2, (l '9Sn), ' [R2Sn{(0PMe2)(OPPh2)N)zl,("9Sn),16'4organotin(1V) complexes ' of bis(pyrazolones), ('I9Sn),' '' diorganotin(1V) complexes of ~ ( 2 - h ~ droxyary1idene)aminoacetic acid, ('19Sn),' ' diorganotin(1V)complexes of salen ligands, ( I I9Sn),' ' diorganotin(1V) complexes of hindered N-arylsalicylaldimine, (*I9Sn),'6 1 * [R2Sn(OAr)2], ( l 19Sn), ' ' [(R2SnX)20]2, (1'9Sn),'620 [Ph2Pb(Se)2Si2Me2(Se)2PbPhz], 77Se, (29Si, '07Pb),'6 2 1 [{ R2(Cl)Sn}2S], (Il9Sn),'622 [Si3Me2Cl71-, (29Si),'623 [RMeSi(OTf)2],(29S1),1624 (181),(29Si),1625poly(si1sesa
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1603 1604
1605
1606
1607 1608
1609
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161 1
1612 1610
1614 1615
1616
1617 1618 1619 1620
1621 1622
1623
1624 1625
G. Deshpande and M.E. Rezac, Polymer Degradation Stability, 2001,74,363. H. Watanabe, H. Suzuki, S. Takahashi, K. Ohyama, Y. Sekiguchi, H. Ohmori, M. Nishiyama, M. Sugo, M. Yoshikawa, N. Hirai, Y. Kanuma, T. Adachi, M. Makino, K. Sakata, K. Kobayashi, T. Kudo, H. Matsuyama, N. Kamigata, M. Kobayashi, M. Kijima, H. Shirakawa, K. Honda and M. Goto, Eur. J. Inorg. Chem., 2002,1772. L. Ronconi, C. Marzano, U. Russo, S. Sitran, R. Graziani and D. Fregona, J. Inorg. Biochem., 2002,91,413. M. Sharma, B. Khungar, S. Varshney, H.L. Singh, U.D. Tripaathi and A.K. Varshney, Phosphorus, Suyur Silicon Relat. Elem., 2001,174,239. R. Buschbeck, K. Bruning and H. Lang, Synthesis, 2001,2289. M.K. Runyon, J.M. Mabry and W.P. Weber, Polym. Prepr. ( A m . Chem. SOC., Div. Polym. Chem.), 2002,43,650 S . Biscazzo, M. Vittadello, S. Lavina and V. Di Noto, Solid State Zonics, 2002,147,377. B. Zhu, D.E. Katsoulis, B.T. Nguyen, J.R. Keryk and F.J. McGarry, International SAMPE Technical Conference, 200433,697. K.-M. Kim and Y. Chujo, J . Polym. Sci., Part A: Polym. Chem., 2001,39,4035; C. Liu, Y. Liu, P. Xie, D. Dai and R. Zhang, Polym. Adv. Technol., 2001,12,475; H. Xu, P. Xie and R. Zhang, Eur. Polymer J., 2001,37,2397. H.D. Tang, J. Sun, J.Q. Jiang, X.S.Zhou, T.J. Hu, P. Xie and R. Zhang, J. Am. Chem. SOC.,2002, 124, 10 482; K. Nakahara, S. Yoshida, K. Komatsu, K. Ishiwata and 0. Sakamoto, Nippon Keshohin Gijutsusha Kaishi, 2000,34, 142. B.X. Mayer, P. Zollner, E. Lorbeer and W. Rauter, J. Sep. Sci., 2002,25,60. V. Sharma, R.K. Sharma, R. Bohra, R. Ratnani, V.K. Jain, J.E. Drake, M.B. Hursthouse and M.E. Light, J. Organomet. Chem., 2002,651,98; V. Sharma, R.K. Sharma, R. Bohra, V.K. Jain, J.E. Drake, M.E. Light and M.B. Hursthouse, J . Organomet. Chem., 2002,664,66. C. Silvestru, R. Rosler, A. Silvestru and J.E. Drake, J. Organomet. Chem., 2002,642,71. C. Pettinari, F. Marchetti, R. Pettinari, A. Cingolani, A. Drozdov and S. Troyanov, J. Chem. SOC.,Dalton Trans., 2002, 188. T.S. Basu Baul, S. Dutta, E. Rivarola, M. Scopelliti and S. Choudhuri, Appl. Organomet. Chem., 2001, 15,947. R. Garcia-Zarracino, J. Ramos-Quifiones and H. Hopfl, J. Organomet. Chem., 2002,664,188. S. Mishra, M. Goyal and A. Singh, Main Group Met. Chem., 2002,25,437. H. Yasuda, J.-C. Choi. S.-C. Lee and T. Sakakura, J. Organomet. Chem., 2002,659,133. J. Beckmann, D. Dakternieks, F.S. Kuan and E.R.T. Tiekink, J. Organomet. Chem., 2002,659, 73. U. Herzog and G. Rheinwald, J. Organomet. Chem., 2002,648,220. J. Beckmann, D. Dakternieks, A. Duthie, C. Jones, K. Jurkschat and E.R.T. Tiekink, Main Group Met. Chem., 2002,25,77. C. Knopf, U. Herzog, G. Roewer, E. Brendler, G. Rheinwald and H. Lang, J . Organomet. Chem., 2002,662, 14. W. Uhlig, Polym. Adv. Technol., 2001,12,607. I. Richter, M. Penka and R. Tacke, Organometallics, 2002,21,3050.
112
quioxane) gel containing optically active 1,3-Me2-1,3-Ph2disiloxane, (29Si),1626 copolysilanes, (29Si),1 7 [{ Ph2P(CH2)3}2SnC12],19Sn),' 2 8 (182), (29Si),'2 9 62 (' 6 6 [ B u " ~ S ~ ( O H ~ )(119Sn),'630B u " ~ S ~ ( O H derived compounds from 1,3~]~+, [ )~] diketone malonates, (119Sn),'631[(PhCH&Sn( 02P(OH)B~f}4]2, (119Sn),1632 [(b~ac)~SnR~], (119Sn),1633 organotin(1V)compounds with Schiff bases of heterocyclic aldehydes and sulfa drugs, (119Sn),1634 [{(C1CH2)2Sn(Cl)}20], (119Sn),1635 [cyclo-Ph2Si(OSnBut2)20But2SnF2], (29Si, '19Sn),'636 C{ (X)Rf2Sn}2012, (1'9Sn),' [{ Ph(HO)SnCH,Sn(I)Ph}O]4,(1'9Sn),'638 [Ph2SnEI3,(E = S, Se, Te; 77se, l19sn, 125~~),1639 [{ C2H402PS2SnBu2}20], (' 19Sn),'640 and [{ C2H402PS2Sn(C6H4-4-Me)2}20], (' 19Sn). 641 '
Variable temperature 'H and 29SiNMR experiments have revealed that the configuration of the lithium bearing silicon atom of some (diaminosily1)lithiums is stable up to 333K in THF.1642 structure and reactivity of the oligomer The obtained by free radical polymerisation of [(CH2= CH)Si(OMe)3]with butyl '~~~ acrylate have been studied by 'H, 13Cand 29SiNMR ~ p e c t r o s c o p y . NMR
1626 1627 1628 1629 1630 1631 1632 1633
1634
1635 1636 1637 1638 1639 1640 1641 1642 1643
M. Seino, M. Oishi, I. Imae and Y. Kawakami, Polym. J . (Tokyo, Jpn.), 2002,34,43. Z. Peng, W. Si, H. Fu, H. Zeng and H. Miao, Gaofenzi Xuebao, 2002,301. M. Seibert, K. Merzweiler, C. Wagner and H. Weichmann, J . Organomet. Chem., 2002,650,25. 2002,124, D.F. Moser, T. Bosse, J. Olson, J.L. Moser, I.A. Guzei and R. West, J. Am. Chem. SOC., 4186. V. Chandrasekhar, R. Boomishankar, S. Singh, A. Steiner and S . Zacchini, Organometallics, 2002,21,4575. D.A. Nieto-Alvarez, F. Jimenez-Cruz and T. Mancilla, Polyhedron, 2002,21,417. V. Chandrasekhar, V. Baskar, A. Steiner and S . Zacchini, Organometallics, 2002,21,4528. C. Pettinari, F. Marchetti, R. Pettinari, A. Gindulyte, L. Massa, M. Rossi and F. Caruso, Eur. J . Znorg. Chem., 2002, 1447. M. Sharma, B. Khungar, M.K. Gupta, H.L. Singh and A.K. Varshney, ACGC Chem. Res. Commun., 2000,12,40. M. Veith, D. Agustin and V. Huch, J . Organomet. Chem., 2002,646,138. J. Beckmann, K. Jurkschat, M. Schurmann, D. Suter and R. Willem, Organometallics, 2002,21, 3819. J.N. Xiang, A. Orita and J. Otera, J. Organomet. Chem., 2002,648,246. M. Mehring, G. Gabriele, S. Hadjikakou, M. Schurmann, D. Dakternieks and K. Jurkschat, Chem. Commun., 2002,834. H. Lange, U. Herzog, U. Bohme and G. Rheinwald, J. Organomet. Chem., 2002,660,43. M.A.A. El-Araj, A.A.S. El-Khaldy and O.S.M. Nasman, Main Group Met. Chem., 2001,24,851. M.A.A. El-Araj, A.A.S. El-Khaldy and O.S.M. Nasman, Main Group Met. Chem., 2002,25,301. A. Kawachi, H. Maeda and K. Tamao, Organometallics, 2002,21, 1319. M.C. Douskey, M.S. Gebhard, A.V. McCormick, B.C. Lange, D.W. Whitman, M.R. Schure and K. Beshah, Athens Conference on Coatings: Science and Technology, Proceedings, 27th, Athens, Greece, July 26,2001,2001,97.
113
data have also been reported for (183),(29Si),1644 organotin Schiff base chelates, bis-N,N-dialkylaminocarbonylethyl-tin-bis-iso-octyl sul(119Sn),'645 fenylacetates, ('I9Sn),' 646 [0{ CH2(0)CHCH20(CH2)3}Si(OMe)]n,(29Si),1 647 648 [(cocta(C1CH2CH2CH2) silsesquioxane, (29si),' C5H9)7Si709(OSiR' R22)02SiC12],(29Si),1 649 [{ CH2(CH2CMe2)2NCH2Si}8012], (29si),150 (184), (29Si), ' [(MeO)&- 1,4-C6H4C=C-1,4-C6H4Si(OMe)3], ' (29Si),1652 [PhSi(O)OHI4, (29Si),1653 HC(CMeNC6H3-2,6-Pr'2)2}GeMe(Se)], [{ (77Se), 54 (RSn)& 14( OH)6I2+, (It9Sn),' (185), (' I9Sn),'ti and [RSnC13], ( l I9Sn). 6 5 7 '
'
\/
Bun
'H, I3C and 15NNMR spectroscopy has been used to determine the complexing sites of a lactam for Pb2+..'658 *'Si NMR structure analysis of water glass A samples has been r e ~ 0 r t e d . 29Si ~ l~~ NMR spectra have provided evidence of a transient hexavalent silicon complex in the diatom Navicula pelliculosa.'660 29Si NMR shifts have been calculated for hypercoordinated silicon-polyalcoholcom1644 1645 1646 1647
1648
1649
1650 1651 1652
1653
1654
1655
1656
1657
1658 1659 1660
J. Wagler, U. Bohme and G. Roewer, Angew. Chem.,Znt. Ed. Engl., 2002,41,1732. B.Yearwood, S.Parkin and D.A. Atwood, Znorg. Chim. Acta, 2002,333,124. R.-b. Wei, Y.Liang and J. Li, Yingyong Huaxue, 2001, 18,764. W. Ziche, M.Holzner, E. Beer and E. Schwiebacher, Ger. Oflen., 2002,lO pp., De 10064071,A l , 20020711. Application: 2000-10064071,20001221. C. Yuan and C. Hu, Chem. J. Internet [online computer Jile], 2002, 2. http://www.chemistrymag.org/cji/2000/025026pc.htm. T.W. Dijkstra, R. Duchateau, R.A. van Santen, A. Meetsma and G.P.A. Yap, J. Am. Chem. Sac., 2002,124,9856. I. Richter, C. Burschka and R. Tacke, J. Organomet. Chem., 2002,646,200. J.J. Pak, J. Greaves, D.J. McCord and K.J. Shea, Organometallics, 2002,21, 3552. G. Cerveau, S.Chappellet, R.J.P. Corriu, B. Dabiens and J. Le Bideau, Organometallics, 2002, 21, 1560. 0.1. Shchegolikhina, Y.A. Pozdnyakova, Y.A. Molodtsova, S.D. Korkin, S.S. Bukalov, L.A. Leites, K.A. Lyssenko, AS. Peregudov, N. Auner and D.E. Katsoulis, Znorg. Chem., 2002, 41, 6892. Y.Q. Ding, Q.J. Ma, H.W. Roesky, R. Herbst-Irmer, I. Uson, M. Noltemeyer and H.G. Schmidt, Organometallics, 2002,21, 5216. R. Vivas-Reyes, F.De Proft, P. Geerlings, M. Biesemans, R. Willem, F. Ribot and C. Sanchez, New J. Chem., 2002,26,1108. L.A. Gomez-Ortiz, R. Cea-Olivares, V. Garcia-Montalvo and S. Hernandez-Ortega, J . Organomet. Chem., 2002,654,51. B. Jousseaume, H. Riague, T. Toupance, M. Lahcini, P. Mountford and B.R. Tyrrell, Organometallics, 2002,21,4590; M. Lahrech, J. Thibonnet, S. Hacini, M. Santelli and J.-L. Parrain, Chem. Commun., 2002,644. D.T. Gryko, A. Pecak, W. Kozminski, P. Piatek and J. Jurczak, Supramol. Chem., 2000,12,229. L.Mokos, E.Kozubek, P. Jelinek and J. Pavlovsky, Chem. Listy, 2001,95,716. S.D. Kinrade, A.M.E. Gillson and C.T.G. Knight, J . Chem. Soc., Dalton Trans., 2002,307.
114
plexes.1661NMR data have also been reported for [Si(N3)6]2-, (14N, 29Si),'662 (186), (29Si),1663 (187), (29Si),'664 [Br2Si(OCR= NN = CMe2)2], (29Si),1665 [Sn(NR)]4, (119Sn),1666 [M{(2,4,6-Me3C6H2)N=CHCH=N(C6H2-2,4,6-Me3)}], (M = Sn, Pb; "N, 'I9Sn,207Pb),'667 heterobimetallic complexes of 1,8-dihydro1,3,6,8,10,13-hexaazacyclotetradecane [SnC14] with Ni" or Cu", (119Sn),'668 of [C~HS(NP~)~S~CI], (119Sn),1669 complexes of Schiff bases, (119Sn),'670 Sn'" Pb" complexes of 3,4-toluenediamine tetraacetate, (207Pb),1' cubic octameric sili67 cate cages, (29Si),'672 [Si(OR)4], (29Si),1673 [(b~rnoxy)~SiOH],(29Si),1674 [(C2H4O2)3SiI2-, (29Si),' [(C2H&)2SiSPh] -, (29Si),'676[Sn(OCH2Bu')2],, (119Sn),16 [{ MeC(CH20)3}2Sn3], ( I 19Sn),' 7 8 [( 3,5-BUt2C6H2-1,2-O2)Sn], 6 ( I 19Sn),' 79 and [(Et2NCS2)2(RS)2Sn], ('I9Sn).'680
Me2N, ,NMe2 Si- Si Cl3 CI3
N. Sahai and J.A. Tossell, Inorg. Chem., 2002,41,1993. A.C. Filippou, P. Portius and G. Schnakenburg, J. Am. Chem. SOC.,2002,124,12 396. 1663 S.B. Clendenning, B. Gehrhus, P.B. Hitchcock, D.F. Moser, J.F. Nixon and R. West, J. Chem. Soc., Dalton Trans.,2002,484. 1664 J.C. Yang and J.G. Verkade, J. Organomet. Chem., 2002,651,15. 1665 1. Kalikhman, B. Gostevskii, 0.Girshberg, S. Krivonos and D. Kost, Organometallics,2002,21, 2551. 1666 D.R. Armstrong, F. Benevelli, A.D. Bond, N. Feeder, E.A. Harron, A.D. Hopkins, M. McPartlin, D. Moncrieff,D. Saez, E.A. Quadrelli, A.D. Woods and D.S. Wright, Inorg. Chem.,2002,41, 1492. 1667 T. Gans-Eichler, D. Gudat and M. Nieger, Angew. Chem.,Znt. Ed. Engl., 2002,41,1888. 1668 S . Tabassum, S.H. Rafiqi, N. Nishat, F. Arjmand and S. Srivastava, Indian J. Chem., Sect. A: Inorg., Bio-inorg., Phys., Theor. Anal. Chem., 2001,40A, 1237. 1669 A.E. Ayers and H.V.R. Dias, Inorg. Chem., 2002,41,3259. 1670 M.S. Singh, B.K. Singh and K. Tawade, Indian J. Chem.,Sect. A: Inorg., Bio-inorg.,Phys., Theor. Anal. Chem., 2001,40A, 1295. 1671 J. Sanchiz, P. Esparza, D. Villagra, S. Dominguez, A. Mederos, F. Brito, L. Araujo, A. Sanchez and J.M. Arrieta, Znorg. Chem.,2002,41,6048. 1672 S.D. Kinrade, J.C.H. Donovan, A.S. Schach and C.T.G. Knight, J. Chem. SOC., Dalton Trans., 2002,1250. 1673 Y. Abe, T. Gunji, R. Shimano and K. Motoyama, Jpn. Kokai Tokkyo Koho, 2002, 6 pp., Jp 2002265605, A2,20020918. Application, 2001-62829,20010307. 1674 J. Beckmann, D. Dakternieks and E.R.T. Tiekink, J. Organomet. Chem., 2002,648,188. 1675 I. Richter, M. Penka and R. Tacke, Znorg. Chem., 2002,41,3950. 1676 U. Herzog, Main Group Met. Chem., 2001,24,757. 1677 T.J. Boyle, T.M. Alam, M.A. Rodriguez and C.A. Zechmann, Inorg. Chem., 2002,41,2574. 1678 T.J. Boyle, J.M. Segall,T.M. Alam, M.A. Rodriguez and J.M. Santana, J. Am. Chem. SOC.,2002, 124,6904. 1679 J. Rouzaud, M. Joudat, A. Castel, F. Delpech, P. Riviere, H. Gornitzka, J.M. Manriquez and I. Chavez, J. Organomet. Chem., 2002,651,44. G. Barone,T. Chaplin,T.G. Hibbert, A.T. Kana, M.F. Mahon, K.C. Molloy, I.D. Worsley, I.P. Parkin and L.S. Price, J. Chem. SOC.,Dalton Trans., 2002,1085.
1661
1662
115
Group 15 Compounds
An NMR study of quaternary ammonium ion conformations in solution has been reported.'681 31P NMR chemical shifts have been calculated using self31P interaction free, gradient corrected DFT.1682 NMR spectroscopy and added chiral shift reagent or chiral solvating agent have been used to show that unsymmetrically substituted single bridged macrocyclic phosphazene compounds exist as 1:1 diastereois~mers.'~~~ Correlations have been found between 31P NMR shifts, relative binding strengths and the electronic nature of phosphorus t r i f l a t e ~ . 'A ~ ~ NMR study of antimony(II1)fluoride complexes in ~ 19F solution has been reported.1685 NMR data have also been reported for [Me2AsSe2]-, (77Se),'686 [M(N3)4]+, [M(N3)& (14N, 7 5 A ~ , 121Sb),'687 [AsCl(N3)2(NC,H5)], [SbC12(N3)(NC5H5)2f,I4N),' ( and [TeSb2C12(NBut)4], (125Te).' 689
Compounds of Group 16
One review has been published entitled 'Recent developmentsin the chemistry of selenoethers and telluroethers', which contains 77Seand 125Te NMR application~.'~~' The relative importance of electron correlation and basis set effects on the calculated 'H and 1 0 7 NMR isotropic shieldings and shielding anisotropies in small water clusters has been studied by the Hartree-Fock and second-order Moller-Plesset approaches using gauge-including atomic 0rbita1s.l~~' proThe 7 ton shielding anisotropy in liquid water has been determined.'692 2H and 1 0 relaxation times have been determined in H2170, D2I60and D2170.1693 77Se NMR data have also been reported for [R'R'C = CHCH2SeH],'694 and [HSe03] - . 69 Heavy-row effects on the strength of the weak nonbonded interactions beV.B. Luzhkov, F. Osterberg, P. Acharya, J. Chattopadhyaya and J. Aqvist, Phys. Chem. Chem. Phys., 2002,4,4640. 1682 S . Patchkovskii and T. Ziegler, J. Phys. Chem. A, 2002,106, 1088. l m 3 I. Porwolik-Czomperlik, K. Brandt, T.A. Clayton, D.B. Davies, R.J. Eaton and R.A. Shaw, Znorg. Chem., 2002,41,4944. 1684 S.L. Renard and T.P. Kee, J. Organomet. Chem., 2002,643,516. 1685 E.V. Kovaleva, L.A. Zemnukhova and V.V. Kon'shin, Russ. J. Coord. Chem., 2002,28,758. 1686 J. Gailer, G.N. George, H.H. Harris, I.J. Pickering, R.C. Prince, A. Somogyi, G.A. Buttigieg, R.S. Glass and M.B. Denton, Znorg. Chem., 2002,41,5426. K. Karaghiosoff, T.M. Klapotke, B. Krumm, H. Noth, T. Schutt and M. Suter, Znorg. Chem., 2002,41, 170. "" T.M. Klapotke, H. Noth, T. Schutt and M. Suter, Eur. J . Inorg. Chem., 2002,2511. 1689 T . Chivers and F. Schatte, Znorg. Chem.,2002,41, 1002. 1690 W. Levason, S.D. Orchard and G. Reid, Coord. Chem. Reu., 2002,225,159. 1691 P.B. Karadakov, J. Mol. Struct., 2002,602403,293. 1492 K.Modig and B. Halle, J . Am. Chem. Soc., 2002,124,12 031. 1693 T.C. Farrar and J.A. Ropp, J. Mol. Liq., 2002,98-W, 103. 1694 E.H. Riague and J.-C.Guillemin, Organometallics, 2002,21,68. 1695 E. Lukevics, P. Arsenyan, 1. Shestakova, I. Domracheva, I. Kanepe, S. Belyakov, J. Popelis and 0.Pudova, Appl. Organornet. Chem., 2002,16,228.
16"
116
tween divalent selenium and halogen atoms have been studied using 77Se NMR spectroscopy.'696 Enantiomeric discrimination of phenylselenylmenthane derivatives has been achieved using 'H and 13CNMR spectroscopy in the presence of a chiral dirhodium complex.' 697 The temperature dependence of J(77Se19F) has been investigated for 2-(fluoromethyl)phenylselenyl cyanate.' 698 77Se,19F Two-dimensional NMR correlation spectroscopy of fluoro(organylse1eno)alkenes and -alkanes has been reported.' 699 Relativistic spin-orbit coupling effects in secondary isotope shifts of 13Cnuclear shielding in CE2, E = 0, S, Se, have been calculated.' 700 NMR data have also been reported for [PhCHC(Se)SBu], 701 [AsC(Se)SeCH2CH2SiMe3], (77Se),' 0 2 [PhCH(OMe)CH2SeAr], 7 (77Se),' (77Se),'703 (188),(E = Se, Te; 77Se,12'Te),'704 (189),(77Se),1705 [R2Te(N3)*], (14N, 125Te),1706 [1,2-C6H4(CH2TeMe21)2], ('2sTe),1707 [CSH10Te(02CPh)2], (12STe),'708 [(RTe)2CH2],(12'Te),' 709 (190), (125Te),'' N-alkyl-Se-alkylselenocarbamates, (77Se),'711 (191), (77Se),'l 2 1,2,5-selenadiazolo[3,4]indole, (77Se),' 1 3 [67 MeCSH3N-2-Sel2, (77Se),'714 [MeTeC4],, (125Te),1 [Cl3TeCH2CH(CH2C1)OCMe 01, (125Te),' ti and [R2Te2],(12'Te).' 7 1 = 71 A theoretical study of the 77SeNMR properties of [Se,Ss-,] molecules has been reported.' 7 1 The effects of intramolecular interactions on 33Smagnetic shielding in gaseous SF6 have been studied both experimentally and theoreti~ a 1 l y . l NMR data have also been reported for [S02(N3)]-, (14N),1720 ~'~ [{(ada1696 1697 1698 1699 1700 1701 1702 1703 1704 1705 1706 1707 1708
1709
M. Iwaoka, T. Katsuda, S. Tomoda, J. Harada and K. Ogawa, Chem. Lett., 2002,518. S . Malik, S.Moeller, H. Duddeck and M.I. Choudhary, Magn. Reson. Chem., 2002,40,659. M. Iwaoka, H. Komatsu, T. Katsuda and S . Tomoda, J. Am. Chem. Soc., 2002,124,1902. H . Poleschner and K. Seppelt, Magn. Reson. Chem., 2002,40,777. P. Lantto, J. Vaara, A.M. Kantola, V.-V. Teikki, B. Schimmelpfennig,K. Ruud and J. Jokisaari, J. Am. Chem. SOC.,2002,124,2762. T. Murai, S.Hayakawa and S . Kato, J. Org. Chem., 2001,66,8101. K . Tani, T. Murai and S . Kato, J. Am. Chem. SOC.,2002,124,5960. M. Tiecco, L. Testaferri, C. Santi, C. Tomassini, F. Marini, L. Bagnoli and A. Temperini, Chem.-Eur. J., 2002,8, 1 18. 1 J.M. White, J.B. Lambert, M. Spiniello, S.A. Jones and R.W. Gable, Chem.-Eur.J.,2002,8,2799. P. Bhattacharyya, A.M.Z. Slawin and J.D. Woollin, Chem.-Eur. J.,2002,8,2705. T.M. Klapotke, B. Krumm, P. Mayer, H. Piotrowski, O.P. Ruscitti and A. Schiller, Znorg. Chem., 2002,41,1184. N.J. Hill, W. Levason, G. Reid and A.J. Ward, J . Organomet. Chem., 2002,642,186. P.C. Srivastava, S.Bajpai, R. Lath, C. Ram, M. Srivastava, R.J. Butcher, M. Zimmer and M. Veith, J . Organomet. Chem., 2002,658,34; P.C. Srivastava, S. Bajpai, R. Lath, C. Ram, R.J. Butcher, M. Zimmer and M. Veith, J. Organomet. Chem., 2002,649,70. D. Selvakumar, R. Singh, M. Nasim and G.N. Mathur, Phosphorus Sulfur Silicon Relat. Elem.,
2001,171-172,501.
1710
M. Abe, D.G. Hilmey, C.E. Stilts, D.K. Sukumaran and M.R. Detty, Organometallics, 2002,21,
2986.
1711 1712 1713 1714 1715
M. Koketsu, M. Ishida, N. Takakura and H. Ishihara, J. Org. Chem., 2002,67,486. S . Sase, N.Kano and T. Kawashima, J. Am. Chem. SOC.,2002,124,9706. M. Edin and S . Grivas, ARKIVOC [online computer file], 2001, 2, 1036.http://www.arkat.org/arkat/journal/Issue7/ms0096.pdf. K.K. Bhasin and J. Singh, J . Organomet. Chem., 2002,658,71. J. Pietikainen, R.S. Laitinen, J. Konu and J. Valkonen, 2.Naturforsch., B: Chem. Sci., 2001,56,
1716 1717
1718 1719
1369 H . Fleischer, B. Mathiasch and D. Schollmeyer, Organometallics, 2002,21,526. G . Mugesh, A. Panda, S. Kumar, S.D. Apte, H.B. Singh and R.J. Butcher, Organometallics, 2002, 21,884. J. Komulainen, R.S. Laitinen and R.J. Suontamo, Can. J. Chem., 2002,80,1435. K. Jackowski, M.Wilczek, W. Makulski and W. Kozminski, J . Phys. Chem. A , 2002,106,2829.
117
g?y
E'
Ph
PhI ,ge MeO2C,,PVCO2Me
Ph
w
\ \
Ph
(191)
mantyl)N}2Se],(14N,77Se),1 [1,3-{Ph2(Se)P}2C4H6c7Se),'722 [XeOEF5]+, 721 1, (E = Se, Te; 77Se, 125Te),'2 3 [Te(SR)2],(125Te),1724 [Te3Cl13]-, 7 and (125Te).1725
Periodic trends in indirect nuclear spin-spin coupling tensors have been examined for X2 and XY, X, Y = F, Cl, Br, I, At, using theoretical calculation. (19F,35Cl, 37Cl, 79Br, *'Br, 1271, 211At).1726 NMR spectroscopy has been used to 35Cl study the structure and stability of [C14010]4- HydroXan(R).'727A Cl- has in been identified in metallothionein by 35Cl NMR spectroscopy.' 7 2 8
10
A review entitled 'The synthesis and characterisation of fullerene hydrides' which contains 3HeNMR spectroscopy has been published.' 7 2 9 The internal magnetic field in [CbOl6and [C70]6- has been probed by 3He
1720
1721
'
722
1723
724 1725
1726
'
1727
728
1729
K.O. Christe, J.A. Boatz, M. Gerken, R. Haiges, S. Schneider, T. Schroer, F.S. Tham, A. Vij, V. Vij, R.I. Wagner and W.W. Wilson, Znorg. Chem., 2002,41,4275. T. Maaninen, R. Laitinen and T. Chivers, Chem. Commun., 2002,1812. T. Stampfl, G. Czermak, R. Gutmann, C. Langes, H. Kopacka, K.H. Ongania and P. Bruggeller, Inorg. Chem. Commun., 2002,5,490. B.A. Fir, H.P.A. Mercier, J.C.P. Sanders, D.A. Dixon and G.J. Schrobilgen, J . Fluorine Chem., 2001,110,89. H. Fleischer and D. Schollmeyer,Znorg. Chem., 2002,41,4739. J. Pietkainen, A. Maaninen, R.S. Laitinen, R. Oilunkaniemi and J. Valkonen, Polyhedron, 2002, 21,1089. D.L. Bryce, R.E. Wasylishen, J. Autschbach and T. Ziegler, J . Am. Chem. Soc., 2002,124,4894. K. Witke, T. Steiger, H. Jancke, K. Beining and W. Polak, Z. Anorg. Allg. Chem.,2002,628,707. W. Maret, G. Heffron, H.A.O. Hill, D. Djuricic, L.-L. Jiang and B.L. Vallee, Biochemistry, 2002, 41, 1689. J. Nossal, R.K. Saini, L.B. Alemany, M. Meier and W.E. Billups, Eur. J . Org. Chem.,2001,4167.
118
NMR spectroscopy with two He in the cavity.'730 3He NMR spectroscopy has X 3He been used to investigate the molecular behaviour of C 5 a 2 , = H, F.1731 chemical shifts have been calculated for helium encapsulated in some f ~ l l e r e n e s . 'Multiple spin exchange in two-dimensional films of 3He has been ~~~ investigated using 3He NMR spectroscopy.' 3 3 Hyperpolarised 3He has been used to study human lung at very low magnetic fields.1734 129Xe-'29Xe molecular spin relaxation has been studied.' 7 3 5 The chemical shift of hyperpolarised '29Xedissolved in liquid nitrogen has been determined.1736A rapid and precise probe for measurement of liquid xenon polarization has been Solid and liquid 129Xe NMR signals enhanced by spin-exchange optical pumping under flow have been described.'7 3 8 The 129Xe NMR spectrum NMR spectra of laser-polarised of xenon inside C60has been described.'739 129Xe xenon in molecules, materials and organisms have been r e ~ 0 r t e d . I ~ ~ ' Hyperpolarised '29Xehas been used for 'H magnetisation enhancement of solvents in very low magnetic Gradient echo imaging of flowing hyperpolarised nuclei has been applied to 129Xe dissolved in EtOH. 742 Laser-polarised '29Xe NMR spectroscopy has been applied to MRI at ultralow magnetic field.'743 Rat brain perfusion measurements with hyperpolarised '29Xe NMR spectroscopy has been applied to study biological fluids for the delivery of '29Xe.'744 first I3lXe The NMR study of xenon in a compound has been applied to [Xe04].'745 The indirect nuclear spin-spin coupling tensors of polyatomic xenon fluorides and group 17 fluorides have been interpreted.' 746
1730 173
1732
1733
1734
1735
T. Sternfeld, R.E. Hoffman, M. Saunders, R.J. Cross, M.S. Syamala and M. Rabinovitz, J. Am. Chem. SOC., 2002,124,8786. X.F. Xu, Y. Xing, Y .M. Liang, Z.F. Shang, G.C. Wang, Z.S. Cai, Y.M. Pan and X.Z. Zhao, Phys. Chem. Chem. Phys., 2002,4,5572. Z. Chen, J. Cioslowski, N. Rao, D. Moncrieff, M. Buhl, A. Hirsch and W. Thiel, Theor. Chem. Acc., 2001,106, 364. C. Parks, N.S. Sullivan and P. Stachowiak, Int. J. Mod. Phys. B, 2002,16,3123. C. Bidinosti, J. Choukeife, P.-J. Nacher and G. Tastevin, Los Alamos National Laboratory, Preprint Archioe, Physics, 2002,1. http://xxx.lanl.gov/pdf/physics/O207129. B. Chann, I.A. Nelson, L.W. Anderson, B. Driehuys and T.G. Walker, Phys. Rev. Lett., 2002,88,
1736 1737
1738
1739
1740
1741
1 1 3201/1. B. Patton, N.N. Kuzma and W. Happer, Phys. Reo. B: Condens. Matter, 2002,65,020404/1. A.S. Verhulst, 0. Liivak, M.H. Sherwood and I.L. Chuang, J . Magn. Reson., 2002,155,145. X.Zhou, J. Luo, X.-P. Sun, X.-Z. Zeng, M.-L. Liu and W.-Y. Liu, Wuli Xuebao, 2002,51,2221. M.S. Syamala, R.J. Cross and M. Saunders, J. Am. Chem. SOC.,2002,124,6216. B.M. Goodson, J. Magn. Reson., 2002,155,157. S.Appelt, F.W. Haesing, S. Baer-Lang, N.J. Shah and B. Blumich, Chem. Phys. Lett., 2001,348,
263.
1742
E. Johansson, J. Svensson, S. Mansson, J.S. Petersson, L.E. Olsson, K. Golman and F.
Stahlberg, J . Magn. Reson., 2002,159,68. A. Wong-Foy, S. Saxena, A.J. Moule, H.M.L. Bitter, J.A. Seeley, R. McDermott, J. Clarke and A. Pines, J. Magn. Reson., 2002,157,235. 1744 G. Duhamel, P. Choquet, E. Grillon and J.-L. Leviel, C . R. Chim., 2001,4, 789;Anon, C . R . G. Chim., 2002,5,209; Duhamel, P. Choquet, E. Grillon, L. Lamalle, J.-L. Leviel, A. Ziegler and A. Constantinesco, Magn. Res. Med., 2001,46,208. 1745 M. Gerken and G.J. Schrobilgen, Inorg. Chem., 2002,41,198. 1746 D.L. Bryce and R.E. Wasylishen, Inorg. Chem., 2002,41,3091.
1743
119
11 Appendix
This Appendix contains a list of papers in which the use of nuclei other than 'H, I3C,19F, 31P been described. The nuclei are ordered by increasing atomic and has number and mass.
2H 3H 3He 'Li 7Li
9Be 1B IIB
14N 15N
170
"Ne *a "
2 7 ~ 1
29Si
6,44,94,164,231,530,645,657,659,676,832,1055,1083,1106 and 1693. 232 and 530. 21 and 1730-1734. 27,28,30,33,39,447,841,843 and 912. 26,29, 31, 32, 34, 35,41,47,48, 50-53, 55-63,65-68,70-75,95,98, 138, 141,150, 185,305,399,404,405,444,602,634-636,642,643,646-650, 732,843,912,1222,1475,1497 and 1532. 81 and 85-87. 1245,1337 and 1406. 21,47,57,98, 111, 117, 125-127, 134, 137, 169,221,240-245,256,259, 267, 273, 278, 291, 301, 307, 309, 365, 482, 595, 600,902, 926, 927, 991, 1037-1042, 1230, 1232-1244, 1246-1 303, 1305-1326, 1328-1 397, 1399-1405,1407-1410,1425,1432,1476,1512,1534 and 1557. 68, 112, 142, 191, 326,400,656, 752,832, 1347, 1556, 1662, 1687, 1688, 1706,1720 and 1721. 3, 18,40,79,117,120,122,131,140, 145,148,153,176,189,209,279,284, 290, 292, 325, 339, 366, 370, 371, 379, 382, 403, 413,415, 423, 425, 432, 453, 604, 680, 752, 764, 797, 798, 806, 887, 888, 969, 1023, 1024, 1030, 1041, 1103, 1108, 1110, 1140, 1141, 1238, 1357, 1386, 1400, 1444, 1447, 1482,1528,1548,1557,1595,1658 and 1667. 42,85, 152, 153, 170,219,626, 657,676, 678,688,693,696,705,706,712, 727, 752, 777, 781, 818, 821, 822, 828, 832, 1092, 1177, 1183, 1186, 1189-1192, 1194,1196,1205,1552, 1691 and 1693. 21. 4,37,43,44,74,448,635,637,638,640,641,643,648,649,653-658,668, 822,1079,1115 and 1201. 21,110, 114,190,210,275,412,588,620,812,813,816,818,822,853,904, 1051, 1231, 1414, 1415, 1417, 1422, 1423, 1427, 1428, 1430-1434, 1438, 1439,1441,1443-1446,1450,1453-1461 and 1464. 2, 29, 35-37,49, 50, 52, 54-57,60, 61, 63, 69, 75, 76, 88,95,97, 100, 113, 115-119, 121, 123, 124, 129, 130, 132, 134, 135, 139, 141,149, 222,239, 246-254,266,269,274,277,296-300,308,311,313,350,353,356-362, 372, 374, 399, 418, 421, 430, 602, 605, 609, 610, 612, 824, 826, 905, 926, 961,965,967,979,1046,1048-1050,1122, 1304,1337,1354-1359,1372, 1382, 1393, 1396, 1402, 1414-1416, 1418, 1420, 1421, 1424, 1426, 1429, 1434, 1437, 1451, 1452, 1465, 1466, 1471-1483, 1485, 1490-1511, 1515-1522, 1524, 1525, 1528-1543, 1554, 1555, 1557, 1558, 1561-1565, 1574-1580,1585, 1586, 1592,1593, 1596, 1598,1600-1604,1606-1612, 1621, 1623-1627, 1629, 1636, 1642-1644, 1647-1653, 1659-1665 and 1672-1676.
120
33s
35c1
37c1
39K 41Ca 43Ca 41sc 45sc 48sc
51v
1719. 19,651,658,833 and 1726-1728. 1726. 643 and 658. 80. 78. 80 and 89. 99 and 101. 90. 133, 143-147, 151, 153-163, 187, 197,212,696-699,704,709,712,932 and 933. 215,216,219 and 223. 228,258,264,272 and 285. 314,316,317,324 and 682. 408. 21. 823,1419,1435,1436,1447 and 1462. 1486. 1687. 64,65, 177,226,280,283,323,373,389,390,394,400,409,410,414,566, 622,839,867,1060,1061,1164,1331,1437,1507,1540,1556,1575,1621, 1639, 1654, 1686, 1690, 1694-1696, 1698, 1699, 1701-1705, 1711-1714, 1718 and 1721-1723. 658 and 1726. 1726. 24,46 and 915. 92,96,102 and 670. 107. 934. 170,174,178,180,181,191-193,702 and 705. 225. 229 and 293. 294,295,302,310,312,322,368,544,752,977,979 and 1331. 400,403,411 and 413. 400 and 407. 427,432 and 437. 13,418,424,426-428,432-439,594,804 and 809. 172. 174,1487,1553 and 1582. 3, 20, 113, 173, 174, 182, 216, 255, 259,268,270, 271, 275,276,295, 297, 307,340,344,406,573,828,829,906-908,934,1052-1054,1327,1346, 1356, 1357, 1361, 1366, 1383, 1422, 1442, 1467-1469, 1484, 1488, 1489, 1497-1502,1510, 1512-1514, 1516,1523, 1526, 1527,1544-1551,1557, 1559,1560,1566-1573,1575, 1583, 1584, 1587-1591,1594-1596,1605, 1613-1620, 1622, 1628, 1630-1641, 1645, 1646, 1655-1657, 1666-1670 and 1677-1680.
121
1687. 66,213,280,281,283,395,400,622,1062,1463,1507,1540,1581,1587, 1639,1689,1690,1704,1706-1710,1715-1717 and 1723-1725. 24,1735-1744 and 1746. 1745. 38,77 and 643. 640,672 and 686. 94,95 and 103. 2,169, 171,179,186,188,194-209,211,212,708,712,715 and 945. 234 and 236. 20, 282, 327, 334, 335, 337, 338, 340-343, 345-349, 351, 352, 354, 355, 357,359,361, 363,364,368,373, 375-381,383-396,553,554,566, 575, 580,766,767,769,771,774,884,1025 and 1026. 20,355,386,416-421,429,438,439 and 808. 128,335,1440,1448 and 1449. 3,13,20,174,175,380,831,1470,1597,1621,1667 and 1671. 93.

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NMR Mann

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1

NMR Spectroscopy in the Liquid and Gas Phase

Spectroscopic Properties of Inorganic and Organometallic Compounds

1 : N M R Spectroscopy in the Liquid and Gas Phase

Spectroscopic Properties of Inorganic and Organometallic Compounds

1: N M R Spectroscopy in the Liquid and Gas Phase

Spectroscopic Properties o Inorganic and Organometallic Compounds f

1 : N M R Spectroscopy in the Liquid and Gas Phase

''' 'I4 '' '' '' '

Spectroscopic Properties of Inorganic and Organometallic Compounds

136 137 138 139

140 141 142

I: N M R Spectroscopy in the Liquid and Gas Phase

Spectroscopic Properties of Inorganic and Organometallic Compounds

C6H4(NSiMe3)2}Mo(=NPh)(H2)(PMe3)2] estimated from 'J('H2H) and has been

168 169 170

I: N M R Spectroscopy in the Liquid and Gas Phase

Spectroscopic Properties of Inorganic and Organometallic Compounds

192 193 194 19s 196 197

200 201 202 203

204 205 206 207

211 212 213 214

1 : N M R Spectroscopy in the L q i and Gas Phase iud

Se-seqse Se SeSi (OC),Re':#:'Re(C0)3

Spectroscopic Properties of Inorganic and Organometallic Compounds

247 248 249 250 251 252 253 254 255

1 : N M R Spectroscopy in the Liquid and Gas Phase

Spectroscopic Properties of Inorganic and Organometallic Compounds

I : N M R Spectroscopy in the Liquid and Gas Phase

Spectroscopic Properties of Inorganic and Organometallic Compounds

306 307 308 309 310 3 11 312

313 314 315

316 311 318 319

1: N M R Spectroscopy in the Liquid and Gas Phase

Spectroscopic Properties of Inorganic and Organometallic Compounds

1 : N M R Spectroscopy in the Liquid and Gas Phase

361 362 363 364

365 366 361 368

Spectroscopic Properties of Inorganic and Organometallic Compounds

370 371 372

I : N M R Spectroscopy in the Liquid and G a s Phase

(125Te, 195Pt),395 Pt" complexes with bile acids, (19sPt).396 and

402 403 404

405 406 407

Spectroscopic Properties o Inorganic and Organometallic Compounds f

409 410 4 11 412

418 419 420

1: N M R Spectroscopy in the Liquid and Gas Phase

Spectroscopic Properties of Inorganic and Organometallic Compounds

1: N M R Spectroscopy in the Liquid and Gas Phase

penantiomerisation processes have been monitored for [MhL6l4-, L

451 458 459

Spectroscopic Properties o Inorganic and Organometallic Compounds f

463 464 465

466 46 7 468 469

1 : N M R Spectroscopy in the L q i and Gas Phase iud

473 474 475

476 47 7 478 479

Spectroscopic Properties o Inorganic and Organometallic Compounds f

investigate the nature of the fluxionality of [Ta(NMe2h{S02(NB~t)2}].48

1: N M R Spectroscopy in the Liquid and Gas Phase

3.1 .I 4 Rhenium. The

Spectroscopic Properties o Inorganic and Organometallic Compounds f