Synthesis and characterization of Zn(II), Cd(II), and Hg(II) alkyl-aryl dithiocarbamate: X-ray crystal structure of [(C6H5N(et) CS2)Hg(C6H5N(butyl)CS2)]

Article abstract of DOI:10.1080/15533171003766717

Zn(II), Cd(II), and Hg(II) complexes of alkyl-aryl dithiocarbamate formulated as ZnL¹L¹ (1), CdL¹L¹ (2), and HgL1L2(3) have been synthesized and characterized. X-ray crystallographic analysis shows that the Hg(II) complex, [(C₆H ₆N(et)CS₆)Hg(C₆H₆N(butyl)CS ₆)] is four coordinate with distorted tetrahedral geometry. Distortions from the regular tetrahedral geometry are attributed to the restricted bite angles of the dithiocarbamate ligand. The spectroscopic analyses confirmed the proposed four coordinate geometry for the complexes in which the metal ions are coordinated to two molecules of the ligands through the S-atoms. X-ray analysis of the mercury complex revealed a compositional disorder between the alkyl groups at certain carbon positions. Copyright Taylor & Francis Group, LLC.

Full text of DOI:10.1080/15533171003766717

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Synthesis and Characterization of Zn(II), Cd(II),
and Hg(II) Alkyl-aryl Dithiocarbamate: X-ray Crystal
Structure of [(C6H5N(et)CS2)Hg(C6H5N(butyl)CS2)]
Damian C. Onwudiwe a & Peter A. Ajibade a
a Department of Chemistry , University of Fort Hare , Alice, South Africa
Published online: 10 May 2010.
To cite this article: Damian C. Onwudiwe & Peter A. Ajibade (2010) Synthesis and Characterization of Zn(II), Cd(II), and
Hg(II) Alkyl-aryl Dithiocarbamate: X-ray Crystal Structure of [(C6H5N(et)CS2)Hg(C6H5N(butyl)CS2)], Synthesis and Reactivity
in Inorganic, Metal-Organic, and Nano-Metal Chemistry, 40:4, 279-284
To link to this article: http://dx.doi.org/10.1080/15533171003766717
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Synthesis and Reactivity in Inorganic, Metal-Organic, and Nano-Metal Chemistry, 40:279–284, 2010
Copyright © Taylor & Francis Group, LLC
ISSN: 1553-3174 print / 1553-3182 online
DOI: 10.1080/15533171003766717
Synthesis and Characterization of Zn(II), Cd(II), and Hg(II)
Alkyl-aryl Dithiocarbamate: X-ray Crystal Structure of
[(C6H5N(et)CS2)Hg(C6H5N(butyl)CS2)]
Damian C. Onwudiwe and Peter A. Ajibade
Department of Chemistry, University of Fort Hare, Alice, South Africa
wide variety of dithiocarbamate metal complexes.[12] The com-
Zn(II), Cd(II), and Hg(II) complexes of alkyl-aryl dithio-
carbamate formulated as ZnL1L2 (1), CdL1L2 (2), and
HgL1L2(3) have been synthesized and characterized. X-ray
crystallographic analysis shows that the Hg(II) complex,
[(C6H5N(et)CS2)Hg(C6H5N(butyl)CS2)] is four coordinate with
distorted tetrahedral geometry. Distortions from the regular tetra-
hedral geometry are attributed to the restricted bite angles of
the dithiocarbamate ligand. The spectroscopic analyses confirmed
the proposed four coordinate geometry for the complexes in which
the metal ions are coordinated to two molecules of the ligands
through the S-atoms. X-ray analysis of the mercury complex re-
vealed a compositional disorder between the alkyl groups at certain
carbon positions.
mon four member cyclic structure appears not to suffer ring-
strain. It has also been established that metal dithiocarbamate
complexes are capable of adopting both mono- and binuclear
types of molecular structures depending on the experimental
conditions.[13] While the complexes that exist in their monomer
forms are square-planar, the dimeric types exist as non-planar
in the configuration of the coordination around the central atom
adopting distorted tetrahedral or square pyramidal or trigonal-
bipyramidal as obtained in Zn (II),[14−17] Cd (II) [18,19] and Hg
(II).[20] Herein, we report the synthesis and characterization of
the group 12 complexes of alkyl-aryl dithiocarbamates.
Keywords metal complexes, crystal structure, dithiocarbamates,
EXPERIMENTAL
synthesis, spectroscopy
Materials and Physical Measurements
All chemicals and reagent were used as received. Anhydrous
CdCl2, ZnCl2, HgCl2 and CS2 were purchased from Aldrich
Chemicals. N-ethyl and N-butyl anilines (Merck) were used
INTRODUCTION
Group 12 metal ions exhibit strong coordinating affinity to
dithiocarbamate ligands to form stable complexes and their
chemistry are dominated by +2 oxidation state.[1,2] They have
diverse applications such as additives to commercial pavement
asphalt,[3] in analytical determinations,[4] and as potent biolog-
ical pesticides and/or pharmaceuticals[5] and recently their use
in catalysis[6] and materials science[7] is receiving consider-
able attention. They have been found as useful precursors for
the deposition of II/VI compound semiconductor materials be-
cause of their reasonable volatility and less carbon deposition
as impurity.[8−10] Initial studies on these complexes were di-
rected at understanding the structural chemistry of their metal
complexes.[11] These structural studies have been extended to a
1
without redistilling. H and 13C NMR spectra were recorded
on 400 MHz and 101 MHz Bruker NMR spectrophotometers,
respectively. Chemical shifts are given in ppm (δ scale) relative
to tetramethylsilane (for 1H and 13C nuclei). Elemental analyses
were performed on Fisons elemental analyzer. Infrared spectra
were recorded on a Perkin–Elmer 2000 FT-IR spectrometer as
KBr disc.
Synthesis of the Ligands
The ligands ammonium N-ethyl-N-phenyldithiocarbamate
(L1) and ammonium N-butyl-N-phenyldithiocarbamate (L2)
were prepared according to reported procedures[21] with slight
modifications. In a typical synthesis, 0.15 mol of the respective
aniline (N-ethyl and N-butyl aniline) was mixed with 20 mL
conc. aqueous ammonia in ice and the mixture was allowed to
stand for 10 mins. To this mixture was added 4.5 mL (0.15 mol)
of ice cold carbon disulfide and stirred vigorously for 6–7 h.
The yellowish solid (orange solid in the case of N-butyl aniline)
product was filtered by suction and rinsed 3 times with cold
ethanol. The products are air and thermally unstable. Attempts
Received 20 January 2010; accepted 10 February 2010.
The authors gratefully acknowledge the contributions of Dr. Ilia
A. Guzei and Lara C. Spencer, University of Wisconsin-Madison and
financial support of GMRDC, University of Fort Hare, South Africa.
Address correspondence to P. A. Ajibade, Department of Chemistry,
University of Fort Hare, Private Bag X1314, Alice 5700, South Africa.
E-mail: pajibade@ufh.ac.za
279

280
D. C. ONWUDIWE AND P. A. AJIBADE
to obtain elemental analyses were hindered by rapid decompo-
sition.
Crystal Structure Determination
A yellow crystal of complex 3 was selected under oil at
ambient conditions and attached to the tip of a micro mount.
The crystal was mounted in a stream of cold nitrogen at 100(2)
K and centered in the X-ray beam. The crystal evaluation and
data collection were performed on a Bruker SMART APEXII
Synthesis of [(C6H5N(et)CS2)Zn(C6H5N(bu)CS2)] (1)
To a well stirred solution of an equimolar (1.25 mmol) con-
centration of ligands L1 (0.267 g) and L2 (0.302 g) in 40 mL
of water was added ZnCl2 (1.25 mmol, 0.170 g) in 20 mL of
the same solvent to obtain an immediate precipitation. The re-
action mixture was then stirred for 1 h at room temperature.
The white product was filtered, washed with water and dried in
vacuo. Yield: 1.10 g, (91%), m. p 140–142◦C. Anal. calc. for
C20H24N2S4Zn (486.04): C, 49.42; H, 4.98; N, 5.76; S, 26.38.
Found: C, 49.40; H, 4.85; N, 5.39; S, 26.35. IR, υ (cm−1):
1456 (C=N), 1157 (C2-N), 959 (C=S). 1H NMR (CDCl3)δ =
7.44–7.33 (m, C6H5-N(et)), 7.24–7.22 (m, C6H5-N(bu)), 4.21
(q, CH2-N(et)), 4.10 (t, CH2-N(bu)), 0.90 (t, CH3-(bu)), 1.20 (q,
CH3-(et)).13C NMR (CDCl3)δ 206.74, 206.49 (CS2), 144.31,
144.09 (C6H5-N (et)), 129.56, 128.63, 126.71 (C6H5-N (bu)),
58.83, 53.96, 29.21, 19.83 (CH2), 13.70 (CH3-(et)), 12.38 (CH3-
(bu)).
˚
diffractometer with Cu Kα (λ = 1.54178 A) radiation and the
diffractometer to crystal distance of 4.03 cm. These highly
redundant datasets were corrected for Lorentz and polariza-
tion effects. The absorption correction was based on fitting a
function to the empirical transmission surface as sampled by
multiple equivalent measurements.[22] A successful solution by
the direct methods provided most non-hydrogen atoms from the
E-map. The remaining non-hydrogen atoms were located in an
alternating series of least-squares cycles and difference Fourier
maps. All non-hydrogen atoms were refined with anisotropic
displacement coefficients. All hydrogen atoms were included in
the structure factor calculation at idealized positions and were
allowed to ride on the neighboring atoms with relative isotropic
displacement coefficients.
RESULTS AND DISCUSSION
Synthesis of [(C6H5N(et)CS2)Cd(C6H5N(bu)CS2)] (2)
This complex was prepared by the procedure described for
1 using CdCl2 (1.25 mmol, 0.228 g). Cadmium complex was
obtained as white solid. Yield: 1.23 g (92 %), m. p 234–236
◦C. Anal. calc. for C20H24N2S4Cd (533.07): C, 45.06; H, 4.54;
N, 5.26; S, 24.06. Found: C, 44.78; H, 4.46; N, 5.26; S, 24.54.
IR, υ (cm−1): 1491(C=N), 1276 (C2-N), 939 (C=S). 1H NMR
(CDCl3)δ = 7.40–7.30 (m, C6H5-N(et)), 7.27–7.24 (m, C6H5-
N(bu)), 4.27–4.22 (q, CH2-N(et)), 4.16 (t, CH2-N(bu)), 0.88 (t,
CH3-(bu)), 1.28 (q, CH3-(et)).13C NMR (CDCl3)δ = 207.21,
206.97 (CS2), 146.09, 145.79 (C6H5-N (et)), 129.41, 128.25,
126.68 (C6H5-N (bu)), 60.73, 55.75, 29.22, 19.92 (CH2), 13.76
(CH3-(et)), 12.44 (CH3-(bu)).
Syntheses
Reactions of the metal salts MCl2 (M = Zn, Cd, Hg) with
equimolar concentrations of the ligandsgave the corresponding
complexes formulated as ZnL1L2, CdL1L2, and HgL1L2 re-
spectively in good yield. Although the ligands are not stable
at room temperature, the complexes obtained are very stable.
Formation of complexes with mixed ligands is a common phe-
nomenon whenever two or more ligands are present in solution.
Many factors have been established that control the processes of
formation, and determine the composition and stability of mixed
ligand complexes. Factors such as the electronic structure of the
central atom and its coordination number, the donor nature of
the ligands and the mutual effect of ligands in a mixed ligand
complex, the geometric structure of the complex and the coor-
dination equilibria in solutions of mixed ligand complexes have
been studied.[23] Generally, mixed ligand complexes are more
stable than simple complexes and should be preferred over sim-
ple complexes.[24] The synthesis of the three complexes using
ligands with varying alkyl substituent’s can be represented as
shown in equation 1.
Synthesis of [(C6H5N(et)CS2)Hg(C6H5N(bu)CS2)] (3)
This complex was prepared by the procedure described for
1 using HgCl2 (1.25 mmol, 0.339 g). Mercury complex was
obtained as pale green solid. Yield: 1.31 g (85 %) m. p = 172–
174◦C. Anal. calc. for C20H24N2S4Hg (621.25): C, 38.67; H,
3.89; N, 4.51; S, 20.64. Found: C, 38.73; H, 3.86; N, 4.90; S,
20.29. IR, υ (cm−1): 1455 (C=N), 1281 (C2-N), 981 (C=S). 1H
NMR (CDCl3)δ = 7.42–7.32 (m, C6H5-N(et)), 7.28–7.24 (m,
C6H5-N(bu)), 4.17 (q, CH2-N(et)), 4.06 (t, CH2-N(bu)), 0.88
(t, CH3-(bu)), 1.27 (q, CH3-(et)).13C NMR (CDCl3)δ 206.73,
206.44 (CS2), 145.59, 145.35 (C6H5-N (et)), 129.58, 128.70,
MCl2 + NH4L1 + NH4L2 → ML1L2 + 2NH4Cl
[1]
M = Zn, Cd and Hg
Although we cannot completely rule out the possibility of
126.47 (C6H5-N (bu)), 60.62, 55.68, 29.11, 19.86 (CH2), 13.72 the formation of simple complexes with each of the respective
(CH3-(et)), 12.25 (CH3-(bu)). Selected Crystals suitable for X- ligands in solution, given rise to M(L1)2 and M(L2)2, as shown
ray analysis were obtained by the slow evaporation of a solvent in equation 2 and 3, the concentration (equimolar), comparable
mixture of dichloromethane and methanol (3:1) at room tem- donor nature of the ligands, and the drive towards compound
perature.
of higher stability make equation 2 and 3 highly negligible and

ZN(II), CD(II), AND HG(II) ALKYL-ARYL DITHIOCARBAMATE
281
TABLE 1
on the magnetic equivalence of the phenyl rings. Apparently,
two signals appeared as multiplets around 7.44– 7.30 ppm and
7.28–7.22 ppm, corresponding to the aromatic protons in dif-
ferent magnetic environments. Peaks due to the methyl protons
were observed in two distinctly different environments. The
triplets around 0.99 ppm are ascribed to the CH3 protons of
the butyl group, the up field signals are due to more shielding
effect experienced through the nuclei of the carbon chain, while
the peaks observed around 1.20–1.30 ppm are assigned to the
CH3 of the ethyl group. The N–CH2 protons are nonequivalent
and appear as quartets (around 4.20 ppm) and triplets (around
4.10 ppm) for the ethyl and butyl group, respectively. These
peaks appear to be affected by the central metal atom as the
sequence Cd > Zn > Hg was observed. The methylene protons
N–(CH2)2 were detected around 1.70 and 1.40 ppm in the three
complexes.
Selected IR spectra of ligands and complexes
υ(C=N) υ(C2-N) υ(C=S) υ(NH4)+ σ(NH4)+
PhN(et)
CSSNH4 L1
1456
1261
982
3422
1601
PhN(bu)
1456
1254
929
3423
1601
CSSNH4 L2
Zn L1L2
Cd L1L2
Hg L1L1
1491
1491
1489
1283
1276
1278
957
939
948
–
–
–
–
equation 4 more feasible.
MCl2 + 2NH4L1 → M(L1)2 + 2NH4Cl2
MCl2 + 2NH4L2 → M(L2)2 + 2NH4Cl
ML12 + ML22 → 2ML1L2
[2]
In the 13C NMR spectra, two different signals were observed
in the aromatic regions, which are indicative of the different
environments of the phenyl groups in the complexes. The first
signal of less intensity appears as two peaks around 145.00
and 144.00 ppm, while the second, with the highest intensity
in the spectra, was observed as three peaks between 129.50
to 126.50 ppm, and is assigned to the phenyl ring of the N-
butyl group due to the shielding effect expected to increase
with increased inductive effect thereby increasing the electron
density around the phenyl carbon atoms.[31] The compounds
exhibits four signals for the methylene carbons between 60.70
and 19.83 ppm while the terminal carbons (-CH3) were found to
resonate around 13.70 and 12.30 ppm. The highest methylene
carbon peak is assigned to the N-(CH2) of the ethyl being more
deshielded than the N-(CH2) of the butyl group. The terminal
carbons of the alkyls in the complexes can be distinguished from
each other. –CH3 of the butyl appears at a lower energy (12.30
ppm) than the –CH3 of the ethyl group being more shielded
from thioureide π-system.
The CS2 resonances for the compounds are observed at
206.74, 206.49; 207.21, 206.97 and 206.73, 206.44 ppm for
complexes 1, 2 and 3, respectively, with very weak intensity
characteristics of the quaternary carbon signals.[32] The down-
field shift of NCS2 carbon signal for these complexes from the
chemical shift value of the alkyldithiocarbamate (usually around
202.30 ppm)[33] is due to electron withdrawing resonance effect
of phenyl. The shift is consistent with reduced electronic cloud
over the entire MS2CN region.
[3]
[4]
IR Spectra
The relevant infrared bands of the ligands and complexes
are presented in Table 1. The IR spectra of the free ligands and
the metal complexes were compared and assigned after careful
comparison. Three regions in the infra red spectra of diagnos-
tic values are the thioureide vibrations, the C S and the M S
bands. The absorptions in the region of 1456 cm−1 in the ligands
L1 and L2; and at 1480–1490 cm−1 region in all the complexes is
associated primarily with the thioureide vibrations υ(CN). The
mode of this vibration in relation to CN stretching frequency
band conformed to the fact that the bond assumes a double-bond
character.[25] Higher frequencies observed for this vibration in
alkyldithiocarbamates results are due to an increase in the dou-
ble bond character of the C–N bond.[26] In accordance with the
arrangement of sulphur atoms around the central metal atom,
the energy of the υ(CN) band falls roughly into groups. Chatt
et al.[27] grouped the order of decreasing frequency as planar >
tetrahedral > octahedral > distorted octahedral > pyramidal.
Variation of alkyl substituents produce both electronic and kine-
matic effects, and determine the vibration of the thioureide band.
In the asymmetric N- alkyl, the symmetric C–S modes have been
found to be profoundly affected.[28] This peak is observed here
as an isolated band near 950 cm−1. This indicates a monodentate
bonding in all the complexes. The peak observed in this region
is a diagnostic criterion, which distinguishes monodentate from
bidentate.[29] Two strong absorptions in the region of 760 cm1
and 695 cm−1 common to all the complexes are diagnostic of
monosubstituted aromatic rings.[30] The third diagnostics bands
are the bands associated with MflS vibrations and are observed
Structure Description for
[(C6H5N(et)CS2)Hg(C6H5N(butyl)CS2)]
The molecular structure of the complex with atom number-
ing scheme is shown in Figure 1. The crystal data and structure
refinement are presented in Table 2, and selected bond lengths
and angles are presented in Table 3. The structure of the complex
in the region of 300–400 cm−1
.
1H-NMR and 13C-NMR Spectra
Generally, the 1H NMR spectra of all the complexes showed consists of monoclinic P21/n space group. The molecular struc-
the effect of the difference in alkyl group of the nitrogen atoms ture of the compound revealed that the Hg atom is tetrahedrally

282
D. C. ONWUDIWE AND P. A. AJIBADE
coordinated to two dithiocarbamate ligands acting as a biden-
tate chelating ligand. The coordination geometry around the Hg
atom is a distorted tetrahedral geometry. The distortion from a
regular tetrahedral geometry may be due to the small bite of the
dithiocarbamate ligand chelate angles [34], S(4) Hg(1) S(3)
[68.94(3)] and S(1) Hg(1) S(2) [68.22 (4)]. This leads to a de-
viation of the angles around the Hg ion from the ideal 109◦. The
other two angles around the Hg apart from the chelate angles
are in the range 102.62(4)–112.19(4)◦. The C N bond length
FIG. 1. Molecular structures of [(C6H5N(et)CS2)]Hg(C6H5N(butyl)CS2)].
TABLE 2
Crystal data and structure refinement for
[(C6H5N(et)CS2)]Hg(C6H5N(butyl)CS2)]
˚
is the same [1.326 (6) A] in the two dithiocarbamate ligands.
It is considerably shorter than would be expected for a typical
Compound
HgL1L2 (3)
˚
single C N bond (1.47 A) but closer to that of C N double
˚
bond (1.28 A). This showed that the Hg S bond have high co-
Empirical formula
Formula weight
Temperature, K
Wavelength, A
Crystal system
Space group
C20H24HgN2S4
624.24
valent character typical of third row transition metal complex.
The Hg S bond lengths in each dithiocarbamate consist of one
short bond and one long bond. The packing diagram (Figure 2)
of the complex consists of four monomeric units packed in two
at adjacent corner of the unit cell. In the molecular structure
of the complex, there is compositional disorder at the positions
of C(8) and C(19) between a butyl group and an ethyl group.
56.0(8) % of the time an ethyl group is present at the C8 position
and a butyl group is present at the C(19) position. 44.0(8) % of
the time a butyl group is present at the C(8) position and an ethyl
group is present at the C(19) position. Butyl groups cannot be
present simultaneously at positions C(8) and C(19) due to steric
limitations in the packing structure. The butyl and ethyl carbon
atoms were refined with restraints and constraints. The final
difference Fourier map contained four peaks of electron density
100(2) K
1.54178 A
˚
˚
Monoclinic
P21/n
Unit cell dimensions
˚
a (A)
10.7421(4)
16.2250(7)
13.6232(6)
105.247(2)
90
2290.82(16)
4
1.801
˚
b (A)
˚
c (A)
β(◦)
γ (◦)
Volume (A )
3
˚
Z
Dcalc Mg/m3
Absorption coefficient (mm−1)
F(000)
15.512
1208
Crystal size (mm3)
0.16 × 0.15 ×
TABLE 3
0.06
◦
Theta range (◦)
Limiting indices
4.33 to 72.13
12<=h<=13,
19<=k<=19,
16<=1<=15
34025
˚
Selected bond lengths (A) and bond angles ( ) for
[(C6H5N(et)CS2)]Hg(C6H5N(butyl)CS2)]
Bond length
Bond angles
Reflections collected
Independent reflection
Hg(1) S(1) 2.3838(11) S(1) Hg(1) S(4) 172.90 (4)
Hg(1) S(4) 2.3915(11) S(1) Hg(1) S(3) 118.11 (4)
Hg(1) S(3) 2.8429(12) S(4) Hg(1) S(3) 68.94 (3)
Hg(1) S(2) 2.8837(13) S(1) Hg(1) S(2) 68.22 (4)
4396 [R(int) =
0.0291]
Refinement method
Full-matrix
least-squares on
F2
99.7 %
4396/28/243
1.069
R1 = 0.0312,
wR2 = 0.0784
R1 = 0312, wR2
= 0.0799
1.223 and 0.491
S(1) C(1)
S(2) C(1)
1.752(5) S(4) Hg(1) S(2) 112.19 (4)
1.690(5) S(3) Hg(1) S(2) 102.62 (4)
Completeness to θ = 67.00◦
Data/restraints/parameters/
Goodness-of-fit on F2
S(3) C(12) 1.706(4) C(1) S(1) Hg(1) 93.17 (15)
N(1) C(12) 1.744(5) C(1) S(2) Hg(1) 78.42 (16)
N(1) C(1) 1.326(6) C(12) S(3) Hg(1) 78.18 (160
N(1) C(2) 1.455(6) C(1) N(1) C(2) 91.68 (15)
N(2) C(8) 1.461(7) C(1) N(1) C(2) 121.8 (4)
N(2) C(12) 1.326(6) C(1) N(1) C(8) 122.8 (4)
N(2) C(13) 1.448(6) C(2) N(1) C(8) 115.3 (4)
N(2) C(19) 1.493(6) C(12) N(2) C(13) 121.9 (4)
Final R indices [I>2sigma(I)]
R indices (all data)
−3
˚
Largest diff. Peak and hole e. A

ZN(II), CD(II), AND HG(II) ALKYL-ARYL DITHIOCARBAMATE
283
FIG. 2. Packing diagram of [(C6H5N(et)CS2)Hg(C6H5N(butyl)CS2)].
3
˚
(max ca. 1.223 e/A ) near atom Hg(1) which are considered
noise.
2. Deeming, A.J., Forth, C.S., and Hogarth, G. Synthesis and crystal struc-
ture of [Ru8(µ5-S)2(µ4-S)(µ3-S)(µ-CNMe2)2(µ-CO)(CO)15] formed via
the double sulphur–carbon bond cleavage of dithiocarbamate ligands. J.
Organomet. Chem., 2007, 692, 4000–4004.
CONCLUSIONS
3. Gossage, R.A., and Jenkins, H.A. The crystal structure of bis-(µ−N-ethyl-
N−phenyldithiocarbamato-S, S’)-bis[(N-ethyl-Nphenyldithiocarbamato-
κ2S, Sꢀ)zinc(II)]. Acta Chim. Slov., 2009, 56, 329–333.
Zn(II), Cd(II), and Hg(II) complexes of ethyl-phenyl and
butyl-phenyl dithiocarbamates have been synthesized and char-
acterized by elemental analyses, IR, and NMR spectra. The
X-ray crystallographic analysis of the Hg complex revealed a
compositional disorder between the butyl and ethyl group at cer-
tain carbon position. All the complexes are four coordinate with
direct M S bond. Their potential as single source precursor for
MS semiconductor nanoparticles has been investigated.
4. Beer, P.D., and Hayes, E.J. Transition metal and organometallic anion com-
plexation agents. Coord. Chem. Rev., 2003, 240, 167–189.
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SUPPLEMENTARY MATERIAL
CCDC-737050 contain the supplementary crystallographic
data for this paper. These data can be obtained free of charge
at www.ccdc.cam.ac.uk/conts/retrieving.html or from the
Cambridge Crystallographic Data Centre, 12 Union Road,
Cambridge, CB2 1EZ, UK; fax: (+44)-1223-336-033 or email:
deposit@ccdc.cam.ac.uk].
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