Synthesis, crystal structure, and spectral analysis of antimony thiourea tetra chloride

Article abstract of DOI:10.1080/15533174.2010.522548

The synthesis of antimony thiourea tetra chloride (ATTC) single crystals by solution technique at room temperature is reported. The complex crystallizes in the orthorhombic space group Pnma with four formula units ofSb[CS(NH ₂)₂]₂Cl₃·Cl in the unit cell. The structure has been solved by direct methods and refined to a final-R value of 0.0393. The synthesized crystals are characterized by FT-IR, UV-visible and TGA-DTA techniques. Copyright Taylor & Francis Group, LLC.

Full text of DOI:10.1080/15533174.2010.522548

Synthesis and Reactivity in Inorganic, Metal-Organic, and Nano-Metal Chemistry, 40:812–820, 2010
Copyright © Taylor & Francis Group, LLC
ISSN: 1553-3174 print / 1553-3182 online
DOI: 10.1080/15533174.2010.522548
Synthesis, Crystal Structure, and Spectral Analysis of
Antimony Thiourea Tetra Chloride
K. Mahesha Upadhya and N. K. Udayashankar
Department of Physics, National Institute of Technology Karnataka, Surathkal, P. O. Srinivasnagar,
Karnataka, India
filtered to get antimony chloride solution. This solution is thor-
oughly mixed with 9 g of thiourea dissolved in 300 ml of dis-
tilled water, filtered and kept at room temperature to get yellow
coloured ATTC crystals. As-grown ATTC crystals are shown in
Figure 7.
The synthesis of antimony thiourea tetra chloride (ATTC) single
crystals by solution technique at room temperature is reported. The
complex crystallizes in the orthorhombic space group Pnma with
four formula units of Sb[CS(NH2)2]2Cl3.Cl in the unit cell. The
structure has been solved by direct methods and refined to a final-
R value of 0.0393. The synthesized crystals are characterized by
FT-IR, UV-visible and TGA-DTA techniques.
The single crystal XRD data of ATTC have been collected
by Bruker SMART using MoKα radiation. The structure was
solved by the direct method and refined by the full matrix
least–square technique using the SHELXL program. Powder
X–ray diffraction studies were carried out using Rigaku X –
Keywords antimony complex, crystal structure, synthesis, thermo-
gravimetric
˚
ray diffractometer with CuKα radiation (λ = 1.540562 A) over
the range 10◦–50◦ at a scanning rate of 2◦/min. The optical ab-
sorption spectrum was recorded in the range of 178.75 nm to
876.15 nm using Ocean Optics, Inc. SD2000 fiber optic spec-
trometer at the room temperature. The FTIR spectrum was
recorded in the range of 500–4000 cm−1 using Nicolet Avatar
330 FT-IR spectrometer by KBr pellet technique. The TG/DTA
analysis of dried powder of single crystals of ATTC is carried
out in nitrogen atmosphere at a heating rate of 10 K/min using
the Thermo-Gravimetric/Differential Thermal Analyzer EXS-
TAR6000 TG/DTA 6300.
INTRODUCTION
Single crystals of some inorganic complexes of thiourea are
gaining importance in recent years because of their unique opti-
cal properties.[1−3] The thiourea molecule is an interesting inor-
ganic matrix modifier due to its large dipole moment[4] and its
ability to form an extensive network of hydrogen bonds. These
metal-organic materials have the potential for combining the
chemical flexibility of organics with the physical ruggedness of
inorganics. Also, the complexes of some main group elements,[5]
such as antimony, can possess a certain biological function.[6–8]
To synthesize complexes of antimony will be interesting not
only for main group element chemistry, but also bioinorganic
chemistry.[9] The present investigation is aimed at the synthe-
sis, structure and spectral analysis of antimony thiourea tetra
chloride single crystals.
RESULTS AND DISCUSSION
ATTC crystals were prepared according to the following re-
action scheme:
CS(NH )
Sb2O3 + HCl → SbCl3
2 2 Sb[CS(NH2)2]2Cl4
−→
Structural determination shows that the title compound crys-
tallizes in the orthorhombic space group Pnma. The MER-
CURY 2.2 drawing of the asymmetric unit of this compound
is shown in Figure 1. The carbon-sulphur bond distance lies
between that of C=S (1.60 A) and C-S (1.81 A) distances
supporting the existence of planar resonance configuration of
thiourea.[2,4] The crystal packing along a-axis is shown in Fig-
ure 2. Interactions like N2. . . Cl3, N1. . . Cl1 were found, which
can be considered as hydrogen bonds, were responsible for the
crystal packing. The crystal data, data collection, refinement
details, atomic coordinates, anisotropic atomic displacement
EXPERIMENTAL
For 100 ml concentrated hydrochloric acid, 9 g of anti-
mony oxide was mixed and the mixture was stirred well and
˚
˚
Received 11 July 2010; accepted 26 July 2010.
Address correspondence to K. Mahesha Upadhya, Depart-
ment of Physics, National Institute of Technology Karnataka,
Surathkal, P.O. Srinivasnagar, Karnataka, India 575025. E-mail:
mahesh.upadhya@yahoo.com
812

SYNTHESIS, STRUCTURE, SPECTRAL ANALYSIS OF ATTC
813
TABLE 1
Crystal data, data collection, and refinement details
Empirical formula
Formula weight
C2 H8 Cl4 N4 S2 Sb
415.82
Crystal system, space group
Cell parameters
Orthorhombic, Pnma
a = 13.8015(12)A α = 90◦
˚
b = 14.7064(13)A β = 90◦
˚
c = 6.0048(5)A
γ = 90◦
˚
Number of formula units (Z)
Volume
Calculated density
Radiation, wavelength
θrange for data collection
Experimental crystal size
Temperature
Absorption coefficient (µ)
Absorption corrections (Tmin, Tmax
∗F (000)
4
3
˚
1218.80(18)A
2.266Mgm−3
˚
MoKα, λ = 0.71073 A
2.77◦ to 28.22◦
0.26 mm × 0.22 mm × 0.20 mm
298 K
3.447 mm−1
)
0.424, 0.502 (calculated); 0.468, 0.546 (reported)
796.0
Measured /Independent reflections
Observed reflections
12958/1526
1520 [I > 2σ (I)]
Restraints /No. of parameters refined
Index ranges
4/76
−18 ≤ h ≤ 18, −19 ≤ k ≤ 18, and −7 ≤ 1 ≤ 7
†R
0.0393 [(F2 > 2σ (F2)]
w
1/ [σ2(F2o)+ (0.0252P)2 + 3.5625P] where P= [(F02)+2(F2c)]/3
Weighted R factor (wR)
Goodness-of-fit on F2
Measurement
Structure drawing
Refinement
0.1142
1.208
Bruker SMART
Mercury 1.4.2 using CIF
SHELXL9710
∗F (000) is the structure factor evaluated in the zeroth-order case h = k = l = 0.
†R (residual disagreement) factor is a measure of agreement between the amplitudes of the structure factors calculated from a crystallographic
model and those from the original x-ray diffraction data.
‡w is the weights used in least squares refinement to represent the relative influence an observation should have on the results.
FIG. 1. Asymmetric unit of Sb[CS(NH2)2]2Cl4. Thermal ellipsoids are shown at 50% probability.

814
K. M. UPADHYA AND N. K. UDAYASHANKAR
TABLE 2
Atomic coordinates, anisotropic ADPs, and equivalent isotropic ADP for each atom
2
˚
Atomic coordinates
Anisotropic ADPs (A )
†
2
˚
Atoms
x
y
z
U11
U22
U33
U12
U13
U23
Uequiv (A )
Sb
0.2874 0.7500
0.2360 0.7500
0.1496 0.6211
0.4965 0.7500
0.4087 0.6222
0.0768
0.4583
0.0170
0.7614
0.2029
0.0150 0.0142 0.0087
0.0251 0.0178 0.0091
0.0000
0.0000
0.0008
0.0029
−0.0012
0.0190
−0.0045
−0.0011
0.0005
—
0.0000
0.0000
0.0006
0.0000
−0.0028
−0.0024
−0.0007
—
0.0126
0.0173
0.0171
0.1103
0.0183
0.0164
0.0213
0.0320
0.0320
0.0216
0.0320
0.0320
Cl1
Cl2
Cl3
S
C
N1
0.0196 0.0180 0.0136 −0.0031
0.1200 0.0990 0.1120
0.0221 0.0192 0.0136
0.0190 0.0164 0.0139
0.0320 0.0175 0.0145
0.0000
0.0048
0.0045
0.0012
—
0.3851 0.5497 −0.0203
0.3585 0.4652
0.0197
0.152
−0.083
H1A∗
H1B∗
N2
0.352
0.353
0.444
0.427
—
—
—
—
—
—
—
—
0.0003
—
—
0.3935 0.5794 −0.2271
0.0330 0.0192 0.0126 −0.0008
−0.0010
H2A∗
H2B∗
0.381
0.411
0.544
0.631
−0.320
−0.236
—
—
—
—
—
—
—
—
—
—
—
∗†Isotropic ADP
Uequivis defined as one third of the trace of the orthogonalized Uij tensor whose elements have dimension (length)2 and are associated with the
mean-square displacements of the atom considered in the corresponding directions.
Symmetry codes: (i) x, y, z (ii) 0.5 −x, −y, 0.5 + z (iii) −x, 0.5 +y, −z (iv) 0.5 +x, 0.5 −y, 0.5 −z (v) −x, −y, −z (vi) 0.5 +x, y, 0.5 −z (vii)
x, 0.5 −y, z (viii) 0.5 −x, 0.5 +y, 0.5 +z.
parameters (ADP), and corresponding/equivalent isotropic
The powder X-ray diffraction pattern is shown in Figure
atomic displacement parameter (Uequiv) for each atom, bond 3(b). 2θ and d values of peaks in this XRD pattern are given
lengths, bond angles, torsions and potential hydrogen bonds in in Table 5. The indexed hkl values with corresponding 2θ
the title compound are given in Tables 1-4. The XRD pattern and d values obtained from the structural details using CIF
derived from the structural details using crystallographic infor- are also listed in Table 5. The d values corresponding to
mation file (CIF) is given in Figure 3(a). CCDC 779849 contains various 2θ values obtained by the powder XRD analysis
the supplementary crystallographic data for this structure. These are in accordance with the d values obtained by the single
data can be obtained from The Cambridge Crystallographic Data crystal XRD data. From Figure 3, one can see that each of
Centre via www.ccdc.cam.ac.uk/data request/cif.
the experimental diffraction peaks has a corresponding peak
FIG. 2. Projection of the structure of Sb[CS(NH2)2]2Cl4along the a axis. The hydrogen bonds are denoted by dotted red lines.

SYNTHESIS, STRUCTURE, SPECTRAL ANALYSIS OF ATTC
815
FIG. 3. (a) XRD pattern derived from the structural details using Mercury 2.2; (b) Powder XRD pattern of ATTC.
in the simulated pattern. This indicates that the product is istered due to its excellent optical behavior until the wave-
pure.[11]
length from 400 nm to 876 nm. Absence of absorption in
the region between 400 and 876 nm is an advantage as it is
the key requirement for materials having NLO properties.[12]
UV-Visible Spectra
UV-Visible spectrum of title compound, which was dis- The visible region of the spectrum exhibits a high intense
solved in 1:1 mixture of N, N-dimethylformamide and tetrahy- transition at 298 nm corresponds to the optical band gap of
drofuran, is shown in Figure 4. The absorbance is not reg- 4.164 eV.

816
K. M. UPADHYA AND N. K. UDAYASHANKAR
TABLE 3
˚
Bond lengths (A), bond angles (degree), and torsions (degree)
in ATTC
˚
˚
1.743(5)A
1.318(6)A
Sb-Cl1
Sb-Cl2
Sb-S
N1-H1A
2.398(2)A
S-C
N1-C
N2-C
N1-H1B
N2-H2B
˚
˚
2.709(1)A
˚
˚
1.321(6)A
2.628(1)A
˚
˚
0.86(5) A
0.84(6) A
˚
˚
N2-H2A
0.78(6) A
0.80(5) A
Cl1-Sb-Cl2
Cl2-Sb- S
Cl2a-Sb-S
Sb-S-C
85.33(5)◦
89.13(4)◦
170.28(4)◦
95.6(2)◦
120.3(3)◦
123(4)◦
Cl1-Sb-S
Cl2-Sb-Cl2a
S-Sb-S
85.03(5)◦
88.81(3)◦
91.31(4)◦
119.2(3)◦
120.5(4)◦
122(4)◦
114(4)◦
131(6)◦
48.5(2)◦
141.2(2)◦
54.4(4)◦
−173(5)◦
8(5)◦
S-C-N1
S-C-N2
N1-C-N2
C-N1-H1B
C-N2-H2B
H2A-N2-H2B
Cl2-Sb-S-C
S- Sb-S-C
Sb-S-C-N2
S-C-N1-H1B
N2-C-N1-H1B
S-C-N2-H2B
C-N1-H1A
C-N2-H2A
H1A-N1-H1B
Cl1-Sb- S-C
Cl2a-Sb- S- C
Sb-S-C-N1
S-C-N1-H1A
N2-C-N1-H1A
S-C-N2-H2A
N1-C-N2-H2A
116(5)◦
FIG. 4. UV-visible spectrum of the title compound.
115(6)◦
133.9(2)◦
126.3(3)◦
−125.3(4)◦
0(5)◦
Thermogravimetric/Differential Thermal Analysis
Figure 6 shows the TGA and DTA thermogram of ATTC.
During the process from 40◦C to 189.1◦C, it loses weight by
the liberation of hydrogen chloride molecules and corresponds
to an endothermic peak at 97◦C. Here the experimental mass
loss (8.77%) is very close to the theoretical one (8.76%) and no
phase transformation is observed.
−180(5)◦
−179(5)◦
1(5)◦
1(5)◦
N1-C-N2-H2B −179(5)◦
From 189.1◦C to 300◦C, the weight loss is due to the loss
of Cl2 and CSNHNH2(thiocarbazoyl group) from the complex
corresponding to an endothermic peak at 247.3◦C. At 300◦C,
the experimental mass loss (42.3%) is close to the theoreti-
cal one (43.9%). Now the composition of the product will be
Sb[CS(NH2)2]Cl. If this composition is reasonable, the the-
oretical content of Sb in Sb[CS(NH2)2]Cl will be 52.2%. A
check experiment was conducted by heating the powder of sin-
gle crystals of ATTC placed in an alumina crucible using muffle
furnace. After the furnace temperature rose to 300◦C, the sam-
ple was kept in the furnace for 10 min. The mass loss (42%)
of the sample is close to the theoretical mass loss (43.9%).
The atomic absorption spectroscopy using GBC 932 Plus of the
heated sample indicates that the relative content of Sb (53.45%)
is close to the theoretical content of Sb in Sb[CS(NH2)2]Cl.
The FTIR spectrum of this decomposition product is shown in
Figure 5(b). The absorption at 3326.4 cm−1 is due to N-H band
stretching.
FT-Infrared Spectra
The recorded FTIR spectrum of ATTC is as shown in Figure
5(a). Few peaks were found to be shifted slightly when com-
pared with the spectrum of thiourea[13,14] due to the following
reason. The structure of ATTC reveals that antimony bonds with
sulphur as all metals except Ti form complexes via sulphur (Ti
forms bond via nitrogen).[15] Hence the C-S stretching frequency
should decrease and that of C-N should increase on complex for-
mation. The absorption at 1618 cm−1due to NH2 deformation
mode is not affected indicating the absence of nitrogen metal
bond. Absorption at 1086 cm−1 due to NH2 rocking mode is
not affected by the formation of metal sulphur bond alone. Thus
the metal-sulphur bond is assumed to be responsible for the
shifting of the vibration at 1412 cm−1 and 730 cm−1 to a lower
frequency.[15] Comparison of vibrations of thiourea with ATTC
crystal is shown in the Table 6.
From 300◦C to 546.9◦C, CSNHNH2 (thiocarbazoyl group),
HCl will be eliminated from the complex leading to the
endothermic peak at 439.1◦C in DTA curve. At 546.9◦C, the
experimental and theoretical mass losses are 69.1% and 70.7%,
respectively. A check experiment was performed by heating
the powder of single crystals of ATTC to 547◦C and it was
kept at that temperature for 02 min. The mass loss (68.1%) of
the sample is very close to the theoretical mass loss (70.7%).
The atomic absorption spectroscopy of the heated sample
indicates that the relative content of Sb in it is 98.1%. This
shows that the product at 547◦C is metal antimony which
TABLE 4
Potential hydrogen bonds in ATTC
Donor — H . . . . D – H H . . . A D . . . A D – H . . . A
˚
˚
˚
Acceptor
(A)
(A)
(A)
(degree)
N2–H2B ..Cl3
N1–H1B ..Cl1
N1–H1B ..Cl2
N1–H1A ..Cl2
0.798
0.838
0.838
0.858
2.111
2.889
5.100
5.749
2.884
3.443
5.893
6.594
163.32
125.43
159.88
169.11

SYNTHESIS, STRUCTURE, SPECTRAL ANALYSIS OF ATTC
817
FIG. 5. FTIR spectra of (a) ATTC, (b) decomposition product after heating at 300◦C, and (c) decomposition product after heating at 547◦C.

818
K. M. UPADHYA AND N. K. UDAYASHANKAR
FIG. 6. TGA and DTA thermogram of ATTC.
FIG. 7. Photograph of synthesized ATTC single crystals.

SYNTHESIS, STRUCTURE, SPECTRAL ANALYSIS OF ATTC
819
TABLE 5
Powder XRD diffraction data for grown ATTC crystals
Data obtained from powder XRD
Data obtained from structural details
∗
˚
˚
Peak no.
2θ
d1 (A)
2θ
h k l
d2 (A)
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
10.2688
12.6614
14.0604
15.8499
17.1253
28.1813
29.6249
30.2714
31.3494
32.6007
34.2877
35.2497
36.2540
37.2973
38.9650
43.1385
45.8989
47.7607
49.5624
8.61418
6.99119
6.29861
5.59125
5.17763
3.16648
3.01538
2.95244
2.85333
2.74661
2.61525
2.54604
2.47779
2.41084
2.31142
2.09697
1.97708
1.90427
1.83918
12.043
12.826
14.196
15.957
17.196
28.543
29.717
30.500
31.283
32.522
34.543
35.130
36.239
37.804
38.978
43.413
45.761
47.652
49.543
0 2 0
2 0 0
2 1 0
0 1 1
1 1 1
4 2 0
0 0 2
3 3 1
2 4 1
2 0 2
1 5 1
4 3 1
3 5 0
3 2 2
2 6 0
6 3 0
1 0 3
2 1 3
0 8 0
7.3532
6.90075
6.24718
5.55924
5.15663
3.12359
3.0024
2.9286
2.85468
2.75311
2.59434
2.55368
2.4781
2.37909
2.3097
2.08239
1.98088
1.90615
1.8383
∗Here
1
d2 = ꢀ
ꢁ
ꢂ
2
2
2
2
2
h
a
k
l
+
+
2
b
c
˚
˚
˚
where a = 13.8015 A, b = 14.7064 A, c = 6.0048 A.
TABLE 7
Thermal decomposition data of ATTC crystal
will be volatilized with temperature. The FTIR spectrum
of this decomposition product is shown in Figure 5(c). The
presence of water modes is due to the absorption of moisture
by the product.[16] The thermal decomposition data is given in
Table 7.
Mass loss (%)
Sb (%)
Reaction
DTA (◦C)
97 (endo)
Wexp
8.77
Wtheor Wexp Wtheor
Sb[CS(NH2)2]2CI4
↓ −HCl
29.282
8.76
↓ (40.0◦C – 189.1◦C)
↓
TABLE 6
Assignment of IR band frequencies (cm−1) in ATTC crystal
SbC2S2N4H7Cl3
32.096
↓ −Cl2, – CSNHNH2 247.3(endo) 33.57 35.117
Thiourea
ATTC
Assignment∗
↓ (189.1◦C – 300◦C)
↓
300
41.996a
3280
1618
1471
1412
1086
730
3284.7
1616.7
1521.4
1388.7
1187.0
707.5
ν(N-H)
δ(NH2)
νas(C-N)
νs(C-S)
ρ(NH2)
νs(C-S)
Sb[CS(NH2)2]Cl
53.45b 52.182
↓ −HCl, - CSNHNH2 439.1(endo) 26.731 26.833
↓ (300◦C - 546.9◦C)
↓ Sb
547
68.078a
98.11b
100
aThe percentage mass loss of the sample measured in the check experi-
ment;
∗δ – Deformation; ν – Band Stretching; ρ – Rocking; s – Symmetric;
as – Asymmetric.
bThe relative content of Sb in the intermediate measured in the check
experiment.

820
K. M. UPADHYA AND N. K. UDAYASHANKAR
and their effect on Leishmania-infected macrophages. Biochem. J., 1993,
CONCLUSIONS
289, 155–160.
Single crystals of antimony thiourea tetra chloride (ATTC)
were synthesized by solution technique at room temperature.
From the single crystal X- ray diffraction pattern, the lattice
parameters, molecular structure, molecular weight and volume
are found. The presence of functional group of the synthesized
complex and the metal-sulphur bond was confirmed by FTIR
spectral study. From the absorption spectrum of ATTC it was
found that the ATTC has good transmittance between 400 – 876
nm and its optical band gap is also calculated. The TG/DTA
analysis revealed no phase transformation of the crystal before
and after melting.
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