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To cite this article: A. K. Saxena (1998) A Method for the Preparation of the
cis-Bis(Glycinato)Copper(II) Monohydrate Complex in the Solid State, Synthesis
and Reactivity in Inorganic and Metal-Organic Chemistry, 28:10, 1653-1663, DOI:
10.1080/00945719809349420
To link to this article: http://dx.doi.org/10.1080/00945719809349420
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A. K. Saxena
Department of Physics and Astrophysics
University of Delhi
Delhi-110007
India
ABSTRACT
A
method has
been
described
cis
form
X-ray
diffraction
analyser.
The
blue
complex
INTRODUCTION
During Ley's
In
1653
Copyright 0 1998 by Marcel Dekker. Inc.
www.dckker.com
SAXENA
1654
Bis(glycinato)copper(II),
to
formulate
his
concept
of
inner
discovered
modifications
and
bluish
[ NH,CH,COO
that
the
was
first
compound
exists
in
two
glistening
] ,Cu. 2H20.
These
two
in
trans-
have
planer
scales
forms
H,O,
configurations.
Ley
and
Wiegner'
and
later
Grinberg
and
Gol'braikh'
cis and
1961 T ~ m i t a ~
confirmed
'~
the
the
basis
of
his
X-ray
In
diffraction
and
IR
studies,
respectively.
Finally,
three
isolated.
were
Out
crystalline
of
assigned
these,
the
forms
of
the
complex
were
trans
structures
and
t'he
third
cis
structure.
The
cis
11
distilled
water
and
(0.02 mole)
adding
cupric
Later
hydroxide
20
mL
in
200 mL
of
an
filtered
and
of
aqueous
The
washed
1655
cis-btr(GLYCMATO)COPPER(II)MONOHYDRATE
c i s = blue needles
trans
Fig. 1.
violet scales
from
This
alkali-free
cupric
hydroxide
was
mole).
water
bath
60C
for
30
min.
and
filtered.
On
the
50%
They reported
SAXENA
1656
This corresponds to
+ 3H,O + CO,
2Cu(NH,CH,COO),.H20
The
gas
only,
showing
that
the
mobility
of
the
other
This,
the mobility
of
will
occur
because
of
the
mobility
of
the
moleculesi2.
The pure complex was obtained by dissolving the product in
water, filtering and crystallizing it, after quickly washing
the crystals with ice-cold distilled water several times.
The
process
was
repeated
two
or
three
times.
The
products
subjected
to
X-ray
powder
obtained
obtained by
were
The
the
by
this method
was
identical
Analytical
to
that
results
cis-bis(GLYCINATO)COPPER(II)
MONOHYDRATE
are given in Table 11.
IR spectra
1657
by the wet method and the present method were also found to
be identical (Table 111).
EXPERIMENTAL
Materials
Basic
copper
carbonate
(May and
Baker),
acetic acid
Synthesis
Basic copper carbonate (0.2391 g, 1 mmole) and
glycine
and the
in an
open vessel
to
water
60'
room
temperature
it
was
filtered.
The
filtrate was
for crystallization.
The
further gave
1.3
(29%) of
the
complex.
The total product (2.8 g) was again dissolved in 100 mL warm
water
and
concentrated,
repeating
the
crystallization
SAXENA
1658
TABLE I
X-ray Powder Diffraction Data
Compound
Basic Copper
Carbonate
[ CuCO,. Cu ( O H )
d = h/2sin J
Peak
( A = 1.5441838)
2e0
Remarks
Definite
structure
,. H,O ]
11.74
12.68
24.05
25.58
31.22
32.04
33.44
33.58
36.58
39.64
43.44
7.531
6.975
3.698
3.479
2.862
2.791
2.677
2.666
2.455
2.271
2.081
7.5380
6.9812
3.7018
3.4824
2.8649
2.7935
2.6796
2.6688
2.4565
2.2737
2.0832
Definite
structure
12.02
12.30
14.00
14.62
21.82
29.24
35.68
38.92
7.356
7.189
6.320
6.058
4.069
3.051
2.514
2.312
7.3630
7.1960
6.3258
6.0589
4.0732
3.0543
2.5164
2.3140
Definite
structure
9.760
10.100
10.340
9.054
8.750
8.548
9.0623
8.8453
8.5552
1659
TABLE I
Continued
Compound
d = A/2sin 8
( A = 1.5441838)
29
15.260
15.420
16.200
17.500
20.940
24.480
25.400
27.920
33.100
46.540
5.801
5.741
5.467
5.063
4.238
3.633
3.504
3.193
2.704
1.950
Peak
5.8674
5.7463
5.5324
5.1854
4.2423
3.6363
3.5012
3.1956
2.7064
1.9514
Remarks
Definite
structure
Definite
structure
H,O
9.780
9.960
10.300
10.540
15.220
15.340
17.440
17.700
20.160
20.280
20.920
25.400
25.520
27.880
33.360
46.620
-~
9.036
8.873
8.581
8.386
5.816
5.771
5.081
5.007
4.401
4.375
4.243
3.504
3.487
3.197
2.704
1.946
9.0438
8,8807
8.5883
8.3933
5.8214
5.7761
6,1340
6.0261
4.4047
4.3789
4.2463
3.5066
3.4904
3.2001
2.7661
1.9482
1.9
g (42.5%).
The
copper in the
1660
SAXENA
In
u)
In
15
pl
N
Y
u)
00
pl
In
m
r(
u)
15
l-i
I4
pl
l-i
cl
m
4
In
0
15
l-i
0
N
--
v)
In
u)
u)
CI
CI
u)
0
0
X
tiI:
b
cis-bi.s(GLYCINATO)COPPER(II) MONOHYDRATE
1661
TABLE I11
IR Spectral Data of The Complex (cm-')
DRY METHOD
WET METHOD
3300
3200
2970
1680
1620
1580
1430
1380
1330
1270
1115
1050
1030
950
920
740
670
560
3300
3200
3000
1679
1610
1590
1420
1390
1320
1270
1140
1060
1035
940
910
145
655
575
Instrumentation
X-ray powder diffraction patterns were obtained on a Philips
Compact X-ray Diffraction Analyser model with the following
operating conditions: P.W. 1840/04/11 at 40kV, 25 ma, and a
slit width of 0.2 nun, copper-LFF tube, angular range 3.0' to
65. Oo,
range 1 to IxlO',
spectra
were
spectrophotometer
subjected
recorded
as
KBr
on
temperature.
discs.
to microanalyses at
200-91527
The
Shimadzu
complexes
the Chemistry
The IR
were
Department,
SAXENA
1662
ACKNOWLEDGEMENT
My thanks to the Chemistry Department of the University of
Dar Es Salaam, Tanzania, for research facilities.
THe paper
Jersey,
USA,
who
Microchemical Journal.
was
the
founding
Editor
of
the
work.
REFERENCES
10, 954
1.
H. Ley, Z. Elektrochem.,
2.
3.
(1904).
3,
257 (1841);
11, 373
(1890).
11, 585
4.
5.
6.
7.
K. Tomita
and
SOC.
Japan.,
I. Nitta, Bull.
34,
(1905).
280 (1961).
286 (1961).
8.
T. Yasui
and
SOC.
Japan.,
2,
604 (1966).
9.
cis-bis(GLYCINATO)COPPER(II)MONOHYDRATE
10.
1663
163,
96 (1927).
11.
12.
13.
z,
Referee I: G . J. Meyer
Referee 11: E. J. Valente