Synthesis, characterization, and X-ray diffraction studies of Co(II), Ni(II), and Cu(II) Tellurite (TeO3M2-) complexes with nicotinic acid

Article abstract of DOI:10.1080/15533170903492648

A series of complexes of the type Hx [M²⁺(NA) _nTeO₃].YH₂O [Where M(II) = Co(II), Ni(II) and Cu(II), X = 2, n = 3 and Y = 6 for Co(II) and Ni(II); X = l, n = 2 and Y = 3 for Cu(II); NA = Nicotinic acid] have been synthesized, and characterization of the ligand, as well as complexes, has been done on the basis of elemental analysis, conductivity, magnetic susceptibility measurements, spectral studies. Thermogravimetric analysis and XRD studies, various ligand field parameters like Dq, B., etc. have been evaluated for Co(II) and Ni(II) complexes, which suggests an octahedral geometry for the complexes and square planar structure for Cu(II) complex. x-ray diffraction studies have been undertaken to determined lattice parameters viz. crystal system, crystal lattice edge, etc. Copyright Taylor & Francis Group, LLC.

Full text of DOI:10.1080/15533170903492648

Synthesis and Reactivity in Inorganic, Metal-Organic, and Nano-Metal Chemistry, 40:5–11, 2010
Copyright © Taylor & Francis Group, LLC
ISSN: 1553-3174 print / 1553-3182 online
DOI: 10.1080/15533170903492648
Synthesis, Characterization, and X-ray Diffraction Studies
of Co(II), Ni(II), and Cu(II) Tellurite (TeO23−) Complexes
with Nicotinic Acid
Chitra Gupta
Department of Chemistry, Bundelkhand University, Jhansi (U.P.), India
EXPERIMENTAL
A series of complexes of the type Hx [M2+(NA)nTeO3].YH2O
Materials
[Where M(II) = Co(II), Ni(II) and Cu(II), X = 2, n = 3 and Y
The starting materials, cobalt tellurite (CoTeO3·H2O), nickel
= 6 for Co(II) and Ni(II); X = l, n = 2 and Y = 3 for Cu(II);
NA = Nicotinic acid] have been synthesized, and characterization
of the ligand, as well as complexes, has been done on the basis
of elemental analysis, conductivity, magnetic susceptibility mea-
surements, spectral studies. Thermogravimetric analysis and XRD
studies, various ligand field parameters like Dq, B,β, etc. have been
evaluated for Co(II) and Ni(II) complexes, which suggests an oc-
tahedral geometry for the complexes and square planar structure
for Cu(II) complex. x-ray diffraction studies have been undertaken
to determined lattice parameters viz. crystal system, crystal lattice
edge, etc.
tellurite (NiTeO3·2H2O) and copper tellurite (CuTeO3·H2O)
were prepared by the reported methods.[4−5]
Preparation of the Complexes
The Hx[M(NA)nTeO3]·YH2O complexes were isolated by
refluxing metal(II) tellurite (Co(II) = 0.25 g, 10 mmol ; Ni(II) =
0.27g,10mmol; Cu(II) = 0. 25g, 10mmol) and was dissolvedin
water (∼100 mL), and the ligand nicotinic acid solution (0.37g,
30 mmol ) was dissolved in hot distilled water (∼100 mL ) in
1:3 (for Co(II), Ni (II) and 1:2 (for Cu(II) the metal ligand molar
ratio. The resulting mixture was refluxed on a water bath for 12–
15 hours at room temperature (28 3◦C) untill the complexes
separated out. The formation of the complexation was marked by
a change in color and precipitation. The precipitate so obtained
was filtrered, washed with diethyl either and dried in a vacuum
over P4O10 before analysis.
Keywords Co(II), Ni(II), and Cu(II) complexes, nicotinic acid lig-
and, analytical, physical studies, IR, TGA and XRD data
INTRODUCTION
Since tellurium(VI) ion has a small size, high positive charge
and stability to appear in tetrahedral and octahedral geome-
try with oxygen, it is the main characteristic of heteropoly
adenda. As such, it can act as a good stabilizing agent to sta-
bilize oxidation states of many transition metal ions. In pre-
vious papers[1−3] we reported the synthesis, characterization,
antimicrobial screening and anti-inflammatory activity of var-
ious complexes having tellurite (TeO23−) anion with organic
ligands (1,l0-phenanthroline, 2,2’-bipyridyl, 1,2-diaminoethane
and 1,3-diaminopropane). The aim of the present investigation
is to study the coordination behavior and structure of the Co(II),
Ni(II) complexes in tetragonal and Cu(II) complexes in cubic
crystal in presence of a TeO23− anion, with nicotinic acid ligand,
the results of which have been reported in the paper.
Characterization of the Complexes
The percentage of each metal in the studied complexes
was determined by reported methods[6].·C,H and N analy-
sis data of the complexes was obtained from Bhabha Atomic
Research Centre Mumbai, India. The molar conductance of
the prepared complexes was measured at 30◦C in aqueous
solutions (10−3M) using an Elico India conductivity bridge
model CM 185. Room temperature magnetic susceptibilities
were determined on an Unico Gouy’s balance model No.
MP 1053, using Hg[Co(NCS)4] as standard. Electronic spec-
tra were recorded on a Chemito 2500 UV-VIS recording
spectrophtometer in aqueous medium. The IR spectra were
recorded on a Bruker IFS 66 V FTIR spectrometer using
KBr pellets at Centre for Advance Technology, Indore, In-
dore. The results of the thermogravimetric analysis and X-ray
diffraction studies on the research samples were furnished to
the author performed by Regional Sophisticated Instrumen-
tation Centre, Nagpur, India. The weight loss was measured
Received 12 October 2009; accepted 12 November 2009.
The author is thankful to Prof. K. S. Pitre, Department of Chemistry,
Dr. H. S. Gour University, Sagar (M.P.) for stimulating discussion and
encouragement.
Address correspondence to Chitra Gupta, Mahakoshal General Store,
(above), Katra Bazar, Sagar (M.P.), 470002, India. E-mail: chitragupta
sgr@rediffmail.com
5

6
C. GUPTA
TABLE 1
Physical characteristics, analytical, molar conductance and magnetic susceptibility data of Hx[M2+(NA)nTeO3]·YH2O complexes
Elemental analysis % found [calculated]
Formula
Melting point/
S.
Empirical
formula
weight Yield decomposition
[color] (%) temperature (◦C)
Molar
conductance B.M.
µeff.
no. Complexes
C
H
N
Metal
Te
(1) H2[Co (C6H4O2N)3TeO3]· 6H2O C18H26N3CoO15Te 711.53 67%
312a
315a
306a
30.857 4.129 6.029 8.015 17.543 Insoluble 4.87
[30.343] [3.792] [5.90] [8.278] [17.924]
30.425 3.821 6.015 8.352 18.238 Insoluble 3.58
[30.352] [3.794] [5.902] [8.248] [17.930]
26.585 2.875 5.205 11.535 23.545 Insoluble 2.17
[26.698] [2.966] [5.191] [11.780] [23.657]
[Pink]
(2) H2[Ni (C6H4O2N)3 TeO3]· 6H2O C18H26N3NiO15Te 711.63 72%
[Skyblue]
(3) H[Cu (C6H4O2N)2 TeO3]· 3H2O C12H15N2CuO10Te 539.36 64%
[Green]
a
Melts with decomposition.
from room temperature up to 900◦C at a heating rate of trons. The µeff.values for Ni(II) complexes are well within the
10◦C/min.
range expected for six coordinated Ni(II) complexes.[8] The
magnetic moment of the Ni(II) complex under study is 3.58
B.M., which is in the expected range for the spin-only value
for the two unpaired electrons in an octahedral or distorted
octahedral geometry.[9] The magnetic moment of the studied
Cu(II) complex is 2.17 B.M., which is slightly higher than the
spin-only value of one unpaired e1ectron for squar- plannar
RESULTS AND DISCUSSION
Cobalt (II), nickel (II) and copper (II) complexes are pink,
skyblue and green in color, respectively. The elemental analysis,
magnetic moment and conductance data have been tabulated in
Table 1.
On the basis of the above data, the molecular for-
mula of the complexes have been worked out to be
Hx[M2+(NA)nTeO3]·YH2O [Where M(II) = Co(II), Ni(II) and
Cu(II); x = 2, n = 3 and Y = 6 for Co(II) & Ni(II) but x = l, n =
2 and Y = 3 for Cu(II) complexes, NA = C6H5O2N (Nicotinic
acid)], respectively.
environment[10]
.
Electronic Spectra
The Electronic spectral data of the complexes under study
has been tabulated in Table 2.
The studied Co(II) complex is a typical of an octahedral sym-
metry exhibiting two absorption bands at 19804 cm−1 (ν2) and
24322 cm−1 (ν3) transitions, respectively.[11] These bands are
Conductance Measurements
All the complexes have high melting points and are soluble
in DMF and DMSO. They are insoluble in common organic
solvent, water, and are nonelectrolytes.
4
4
assigned to 4Tlg(F) → A2g(F) and 4T1g(F) → Tlg(P) transition,
respectively. The ligand field parameters such as Dq, B, β have
been calculated[12] from the assigned band position of ν2 and ν3
in Table 2. These spectral data suggest octahedral geometry to
the complex.
Magnetic Properties
The effective magnetic moment (µeff.) (Table 1) for Co(II)
Electronic spectra of Ni(II) complex under study exhibits two
complex is 4.87 B.M., respectively. The magnetic moment of broad bands in the range 16393 cm−1 and 26315 cm−1 attributed
complexes are in good agreement with reported octahedral to the ligand field bands ν2 and ν3 corresponding to the tran-
4
4
3
3
complexes[7] of Co(II) corresponding to three unpaired elec- sitions A2g(F) → Tlg(F)and A2g(F) → Tlg(P), respectively.
TABLE 2
Electronic spectral data and ligand field parameters (in cm−1) of Hx[M2+ (NA)n TeO3]. YH2O complex
Ligand field’s parameters (in cm−1
)
Band maxima
ν(in cm−1
S. no.
(1)
Complex
)
Transition
Dq
B
β
4
H2[Co (C6H4O2N)3 TeO3]. 6H2O
19804 (ν2)
24322 (ν3)
16393 (ν2)
26315 (ν3)
9806
4T1g(F) → A2g(F)
1058
1097
0.9794
0.721
4
4T1g(F) → T1g(P)
4
(2)
(3)
H2[Ni (C6H4O2N)3 TeO3]. 6H2O
H[Cu (C6H4O2N)2 TeO3]. 3H2O
4A2g(F) → T1g(F)
1034
778.78
—
3
3A2g(F) → T1g(P)
2
15383 (ν1)
2B1g → A1g
1538.3
—

STUDIES OF COMPLEXES WITH NICOTINIC ACID
7
FIG. 1. Infrared spectra of (a) H2[Co(NA)3 TeO3]. 6H2O,(b) H2[Ni(NA)3 TeO3]. 6H2O and (c) H[Cu(NA)2 TeO3]. 3H2O.
TABLE 3
Principle infrared spectral bands (cm−1) of Hx[M2+ (NA)n TeO3]. YH2O complexes
-COOH group
Unionized & Ionized &
TeO23−
νM−O ν1 ν3 νM−N
S.
C-H
O-H uncoordinated coordinated
uncoordinated
νC=O νC−O -COOH
No.
Complexes
νOH
stretching stretching
-COOH
-COO−
(1) H2[Co (C6H4O2N)3 TeO3].6H2O 3900-3600br 2940m
2360ws
2353w
-
1690s
1589vs 1568br 1328vs
760v
764m
764m
495v 648s 760w 531ms
485v 701vs 764w 532s
494v 717s 760w 586s
975vs
(2) H2[Ni (C6H4O2N)3 TeO3]. 6H2O 3900-3585br 2925w
1704w
1694s
1695ms
1589w
1595m
1568s 1328m
1569s 1313w
975ws
(3) H[Cu (C6H4O2N)2 TeO3]. 3H2O 3900-3400br 3042s
975ws

8
C. GUPTA
TABLE 4
Thermogravimetric data of Hx[M2+ (NA)n TeO3]. YH2O complex
Total weight loss (%) steps found
(calculated) with temperature ranges (◦C)
Lattice water
molecule
Ligand
molecule
Total weight loss
(%) found (calculated)
S. no.
Complex
(1)
(2)
(3)
H2[Co(NA)3 TeO3].6H2O
15.0(15.171)
(77–142)
15.25(15.176)
(77–142)
9.85(10.011)
(77–137)
52.5(51.882)
(377–537)
52.34(51.899)
(177–567)
46.15(45.650)
(187–462)
67.500(67.053)
67.59(67.075)
56.000(55.661)
H2[Ni(NA)3 TeO3].6H2O
H[Cu(NA)2 TeO3].3H2O
Various ligand field parameters like Dq (1034 cm−l) Racah
A broad asymmetric band in the region 15383 cm−1 is ob-
inter electronic repulsion parameter B (778.78 cm−l) and the served in the electronic spectrum of the studied Cu(II) complex.
nepthelauxetic ratio β (0.721) have been ca1culated.[13,14] The The broadness of the band may be due to John-Teller distrac-
spectrum suggested an octahedral geometry[11] to the Ni(II) tion. Duff et al.,[15] suggested that the absorption bands in this re-
complex.
gion are due to tetragonally distroted squar plannar environment
TABLE 5(a)
TABLE 5(b)
The X-ray powder diffraction data for H2[Ni(NA)3 TeO3].
6H2O complex
The X-ray powder diffraction data for H2[Co(NA)3 TeO3].
6H2O complex
˚
˚
˚
˚
S. no.
h
k
l
dObS(A)
dca1(A)
Iobs
1.5
100
24.2
97.9
50
29.1
44.9
17.5
35.6
51.4
50
20.7
33.2
41.5
52.2
16.7
19.3
6.1
S. no.
h
k
l
dObs(A)
dcal(A)
Iobs
79.66
(1)
(2)
(3)
(4)
(5)
(6)
(7)
(8)
(9)
(10)
(11)
(12)
(13)
(14)
(15)
(16)
(17)
(18)
(19)
(20)
(21)
(22)
(23)
(24)
(25)
0
1
0
1
2
1
2
3
1
3
1
3
2
2
0
0
5
4
2
7
6
3
6
8
7
0
1
0
1
0
1
2
0
0
0
1
1
1
1
0
0
2
0
2
0
5
2
5
2
1
1
0
2
1
0
3
1
0
4
2
4
2
4
4
5
6
4
7
8
1
1
9
2
0
0
15.793
8.261
7.477
6.55
14.907
8.263
7.454
7.227
5.843
4.259
3.982
3.895
3.55
3.452
3.397
3.311
3.034
3.034
2.981
2.484
1.875
1.721
1.699
1.659
1.489
1.475
1.467
1.417
1.376
(1)
(2)
(3)
(4)
(5)
(6)
(7)
(8)
(9)
(10)
(11)
(12)
(13)
(14)
(15)
(16)
(17)
(18)
(19)
(20)
(21)
(22)
(23)
(24)
(25)
2
2
2
2
3
2
4
3
4
3
2
4
5
2
3
5
5
5
1
7
4
7
7
7
7
0
1
1
2
1
0
0
2
1
3
0
3
0
2
3
2
1
3
1
0
1
1
7
8
1
0
0
1
0
0
3
0
2
1
2
4
0
1
4
3
1
2
2
6
1
7
6
1
4
9
8.259
7.406
6.496
6.007
5.300
4.227
4.164
3.942
3.865
3.44
3.405
3.319
3.225
3.108
3.044
3.010
2.987
2.655
2.408
2.338
1.876
1.704
1.665
1.491
1.375
8.263
7.392
6.614
5.843
5.226
4.24
17.5
65.8
56.9
10.7
27.5
16.8
30.6
15.5
56.3
96.7
24.2
12.4
13.9
19.6
26.7
6.03
4.244
3.962
3.885
3.504
3.45
3.408
3.348
3.042
3.018
2.99
2.494
1.878
1.726
1.703
1.665
1.494
1.481
1.472
1.421
1.37
4.132
3.898
3.869
3.448
3.381
3.305
3.226
3.129
3.059
3.005
2.969
2.648
2.417
2.331
1.872
1.698
1.659
1.483
1.346
100
17.5
16.1
3
46.8
12.4
17.8
8.7
5.1
7.7
4.8
4.6
100
1.6
4.05
2.24

STUDIES OF COMPLEXES WITH NICOTINIC ACID
9
TABLE 5(c)
The X-ray powder diffraction data for H[Cu(NA)2
TeO3].3H2O complex
around Cu(II) ion. However, the recent studies on electronic
2
2
spectra of Cu(II) complex indicate that the B1g → A1g is
close in energy and often give rise to a single broad absorp-
tion envelop.[16]
˚
˚
S.no.
h
k
l
dobs(A)
dcal(A)
Iobs
35.7
Infrared Spectra
The Infrared spectra of the complexes under study are de-
picted in Figure 1.
(1)
(2)
(3)
(4)
(5)
(6)
(7)
(8)
(9)
(10)
(11)
(12)
(13)
(14)
(15)
(16)
(17)
(18)
(19)
(20)
(21)
(22)
(23)
(24)
(25)
(26)
(27)
(28)
2
2
2
3
4
5
4
5
4
5
6
5
5
6
7
6
6
7
7
9
8
8
9
8
8
5
9
8
2
2
2
2
2
1
3
2
4
3
0
4
4
2
2
5
4
5
5
3
5
7
6
7
6
9
9
8
0
1
2
1
1
0
2
1
0
0
0
0
1
2
0
2
4
0
4
2
4
0
2
4
6
6
3
7
6.936
6.479
5.835
5.306
4.422
3.899
3.75
7.008
6.607
5.722
5.298
4.325
3.887
3.681
3.619
3.504
3.399
3.303
3.095
3.058
2.988
2.723
2.458
2.403
2.304
2.089
2.045
1.934
1.865
1.802
1.745
1.7
7.4
11.8
8.4
12.2
12.6
11
Structurally important IR signals of the complexes under
study have been reported in Table 3.
A strong band at 3900–3400br and 975 cm−1 were obtained
in the case of simple complexes, which indicated the presence
of water molecules inside the coordination sphere.[17,18] The
3.624
3.525
3.419
3.301
3.089
3.058
3.003
2.747
2.465
2.402
2.31
100
32.9
32.3
11.4
19.2
22.4
53
24.1
5.9
11
7.1
2.6
15.3
11.4
23.5
5.6
2.094
2.037
1.938
1.883
1.807
1.756
1. 705
1.668
1.522
1.498
4.5
4.8
12.2
4.5
5.9
1.664
1.516
1.49
FIG. 2. Thermogravimetric curves of (a) H2[Co(NA)3 TeO3]. 6H2O, (b)
H2[Ni(NA)3 TeO3]. 6H2O and (c) H[Cu(NA)2 TeO3]. 3H2O.
FIG. 3. X-ray diffraction powder patterns of (a) H2[Co(NA)3 TeO3] 6H2O,
(b) H2[Ni(NA)3 TeO3] 6H2O and (c) H[Cu(NA)2 TeO3] 3H2O.

10
C. GUPTA
O
O
O
O
Te
O
H
O
O
C
Te
H
O
O
C
N
O
N
M
C
O
O
Cu
C
O
O
N
H
.3H2O
OOC
FIG. 4(b). Structural formula of H[Cu2+(C6H4O2N)2TeO3].3H2O.
the NA (nicotinic acid) complexes are hydrated; so is in these
complexes[20,21] the tellurite ions contain the infinite chain of
approximately D3hsymmetry.[21] As such, the NA complexes
show two bands at ∼ 648 cm−1 (ν1) and ∼760 cm−1 (ν3). The
M-N stretcheing band appear[22] in the region ∼530 cm−l.
N
N
Thermogravimetric Analysis
The thermograms (Figure 2) and the thermogravimetric data
in Table 4 show the decomposition of complexes in two steps.
The infrared spectra in Table 3 for the synthesized complexes
showed a broad band at ∼3600 cm−1, which may be assigned
as due to overlapping of the νOH of the lattice water, and the
first step weight loss at 77–142◦C indicates the loss of loosely
bound water of crystallization. According to Nikalaev et al.[23]
and Singh et al.,[24] water eliminated below 77–142◦C can be
considered as lattice water present in the complex. The second
step in the thermogram shows the loss of ligand molecules of the
complex, which occurs between 177–567◦C, the metal oxides
are formed in both cases.
H2
.6H2O
FIG. 4(a). Structural formula of H2[M2+(C6H4O2N)3TeO3].6H2O for
M2+ = Co(II)/Ni(II).
characteristic bands because of unionized (uncoordinated) and
ionized (coordinated) - COOH group[19] were obtained in the
range of 1690–1704 cm−1 and 1590 5 cm−1; 1590 5 cm−1
showing the presence of coordinated carboxyl group. An ad-
ditional band of 760 cm−1 in the spectra of complexes was
due to the presence of uncoordinated -COOH group,[19] M-O
stretching bands appeared at ∼495 cm−1. The bands due to
tellurite (TeO23−) ion appeared at ∼648–764 cm−1. Generally,
The decomposition pattern may be summed up as:
Loss of total
Water molecule
Hx[M2+(NA)nTeO3].YH2O
−−−→
77−142
Loss of total
Ligand molecule
Hx[M2+(NA)nTeO3]
−−−→
M2+TeO3[M2+/TeO2]
177−567◦C
TABLE 6
Crystal parameters and other characteristics of Hx[M2+(NA)nTeO3].YH2O complexes
Crystal lattice edge
Cell
volume A
Density found
(calculated) (g cm−3
)
Crystal
system
3
˚
˚
˚
˚
S. no.
Complexes
a (A)
b (A)
c (A)
n
(1)
(2)
(3)
H2[Co (C6H4O2N)3 TeO3].6H2O 11.686 11.686 14.907
H2[Ni (C6H4O2N)3TeO3].6H2O 16.526 16.526 14.824
H[Cu (C6H4O2N)2 TeO3].3H2O 19.823 19.823 19.823
2035.638
4048.593
7789.470
4
8
12
2.30 (2.32)
2.30 (2.31)
1.37 (1.38)
Tetragonal
Tetragonal
Cubic

STUDIES OF COMPLEXES WITH NICOTINIC ACID
11
where M(II) = Co(II), Ni(II) and Cu(II); NA = Nicotinic
2. Gupta, C., and Gautam, R.K. Bioinorganic studies on Co(II), Ni (II) and
Cu(II) tellurite complexes with 2, 2ꢀ- Bipyridyl ligand. Indian J. Chem.
2002. 41 (A), 763–766.
acid
3. Gupta, C., Gautam, R.K., and Pitre, K.S. Chemical and structural studies
of some transition metal tellurite compleness with 1, 3- diaminopropane.
Synthesis and Reactivity in Inorganic and Metal Organic Chem. 2004, 34
(6), 1105–1122.
4. Mellor, J.W. A Comprehensive Treatise of Inorganic and Theoretical Chem-
istry, 11th Ed. Longman: London, 1947, 802.
5. Vallance, R.H., Twiss, D.F., and Russell, A.R. A Text-book of Inorganic
Chemistry, 1st Ed. Chorles Griffin and Co. Ltd.: London, 1931, 383.
6. Vogel, A.I. A Text Book of Quantitative Inorganic Analysis, 4th Ed. Long-
man: London, 1961, 302, 324, 497, 527, 531.
7. Figgis, B.N., and Lewis, J. Prog. Inorg. Chem. 1964, (6) 37.
8. Cotton, F.A., and Wilkinson, G. Advanced Inorganic Chemistry, 3rd Ed.
Wiley Eastern: New Delhi, 1976, 894.
9. Calvin, M., and Barkelew, C.H. J. Am. Chem. Soc. 1946, (68), 2267.
10. Nyholm, R.S. Chem. Rev. 1953, (53), 262.
11. Lever, A.B.P. Inorganic Electronic Spectroscopy, 2nd Ed. Elsevier:
Amsterdam, 1984.
12. Ballhansen, C.J. 1962 Introduction to Ligand Field Theory, McGraw-Hill:
New York, 1962; Figgis, B.N. Introduction to Ligand Fields, Wiley Inter
science: New York, 1967.
13. Rastogi, D.K., Shrma, K.C., Dua, S.K., and Teotia, M.P., J Inorg Nucl
Chem, 1975, (37) 685.
X-ray Diffraction Studies
The X-ray powder diffraction patterns in Figure 3 of the com-
plexes have been indexed for peaks having relative intensities
by standard methods,[25,26] keeping in mind the characteristics
of various symmetry systems, untill a good fit was obtained
between the observed and calculated d-values. The unit cell
parameters were calculated form the indexed data. It is also
clear from the data that Co(Il) and Ni(II) complexes possesses
tetragonal symmetry, where as Cu(II) complex possess cubic
symmetry, respectively. The Miller indices (h k l) along with
observed and calculated d-values and the relative intensities are
reported in the Tables 5a, 5b, 5c within the limits of experimen-
tal errors, the calculated and observed valued of d-values are in
good agreement.
X-ray diffraction studies have been carried out with a view
to find out the type of crystal system; lattice parameters, cell
volume and crystalline size of the complexes are given in Table
6.
14. Drago, R.S. Physical Methods in Inorganic Chemistry, Reinhold: New York,
1965, 410.
15. Duff, E.J., Hughes, M.N., and Rutt, K.J. J Chem. Soc. 1969, 2126.
16. Satyanarayana, D., and Manapatra, B.K., Indian J. Chem. 1975, (13), 414.
17. Feeman, F.B., Lee, D.S., and Adde, L.R. Infrared Spectra and Character-
istic Frequencies 700-300 cm−1, 1968, 98.
18. Adams, D.M., and Squire, A. J. Chem. Soc. 1970, (A) 1808.
19. Bellamy, L.J. The Infrared Spectra of Complex Molecules, 2nd Ed. Wiley:
New York, 1958, 279.
20. Nakamoto, K. Infrared and Raman Spectra of Inorganic and Coordination
Compounds, 5th Ed. John Wiley-Interscience: New York, 1983.
21. Siebert, H. J. Inorg. Allg. Chem. 1955, (275) 225.
22. Powell, D.S., and Sheppard, N. J Chem. Soc. 1956, 3108.
23. Nikalaev, A.V., Logvinenko, V.A., and Myachina, L.I. On thermal Analysis,
New York: Academic Press, 1969, (12) 779.
CONCLUSIONS
From the above discussion, it could be concluded that the
nicotinic acid behaves as a mono and bidentate ligand through
nitrogen and oxygen atom of -COO group. The complexes of
Co(II) and Ni(II) were of octrahedral geometry and that of Cu(II)
of square planar geometry where as X-ray data revealed that the
Cobalt(II) and Nickel(II) complexes of ‘NA’ (Nicoinic Acid)
possessed tetragonal symmetry and Copper(II) complex pos-
sessed cubic symmetry, as such the following general structures
to the complexes may be assigned.
24. Singh, B., Maurya, P.L., Agarwala, B.V., and Dey, A.K. Coordination
polymers of terephthalaldehyde bis (semicarbazone) with some bipositive
cations. J. Indian Chem. Soc., 1982, 59 (10), 1130–1132.
25. Peiser, H.S., Rookshy, H.P., Wilson, A.J.C. X-ray Diffraction by Polycrys-
talline Materials, London: The Institute of Physics, 1956, 344.
26. Woolfson, M.M. An Introduction to X-ray Crystallograph. Cambridge Uni-
versity Press: Cambridge, 1980, 125.
REFERENCES
1. Gupta, C., and Gautam, R.K. Synthesis and characterization on some
[Co2+(amine)3]TeO3. nH2O complexes. Rev. Inorg. Chem. 2000, 20 (3),
241–253.

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