Desulfurization of bibenzyl trisulfide by [CpMo(CO)3]2: Formation and isolation of thiolato-bridged dimolybdenum complexes of [CpMo(CO)2(SBz)]2, [CpMo(CO)(SBz)]2S and [CpMo(SBz)S]2 (Cp = (η5-C5H5), Bz = PhCH2-). Crystal structures of two polymorphs of [CpMo(SBz)S]2

Article abstract of DOI:10.1016/j.ica.2007.02.021

The reaction of [CpMo(CO)₃]₂ (1) with a molar equivalent of Bz₂S₃ at 60 °C for 3.5 h has led to the isolation of [CpMo(CO)₂(SBz)]₂ (2), [CpMo(CO)(SBz)]₂S (3) and [CpMo(SBz)S]₂ (4) in 16.9%, 3.1% and 61.1% yields, respectively, as main products. Thermolytic studies showed that 2 underwent stepwise decarbonylation to give 3 and 4. All the three products of 2, 3 and 4 were thiolato-bridged dimolybdenum complexes with bond orders of zero, one and two for 2, 3 and 4, respectively. In addition, both 3 and 4 have one and two S atoms bridged in a μ-η²-mode, respectively. The structures of 2 and 3 have been reported previously. The totally decarbonylated 4 was isolated as polymorphs, 4a and 4b, which have been characterized by elemental, spectral analyses and structurally determined.

Full text of DOI:10.1016/j.ica.2007.02.021

Inorganica Chimica Acta 360 (2007) 3113–3118
www.elsevier.com/locate/ica
Note
Desulfurization of bibenzyl trisulfide by [CpMo(CO)3]2: Formation
and isolation of thiolato-bridged dimolybdenum complexes
of [CpMo(CO)2(SBz)]2, [CpMo(CO)(SBz)]2S and
[CpMo(SBz)S]2 (Cp = (g5-C5H5), Bz = PhCH2–). Crystal
structures of two polymorphs of [CpMo(SBz)S]2
*
Richard C.S. Wong , Mei Lee Ooi, Guan Huat Tan, Seik Weng Ng
Department of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
Received 27 July 2006; received in revised form 12 February 2007; accepted 15 February 2007
Available online 21 February 2007
Abstract
The reaction of [CpMo(CO)3]2 (1) with a molar equivalent of Bz2S3 at 60 ꢀC for 3.5 h has led to the isolation of [CpMo(CO)2(SBz)]2
(2), [CpMo(CO)(SBz)]2S (3) and [CpMo(SBz)S]2 (4) in 16.9%, 3.1% and 61.1% yields, respectively, as main products. Thermolytic studies
showed that 2 underwent stepwise decarbonylation to give 3 and 4. All the three products of 2, 3 and 4 were thiolato-bridged dimolyb-
denum complexes with bond orders of zero, one and two for 2, 3 and 4, respectively. In addition, both 3 and 4 have one and two S atoms
bridged in a l–g2-mode, respectively. The structures of 2 and 3 have been reported previously. The totally decarbonylated 4 was isolated
as polymorphs, 4a and 4b, which have been characterized by elemental, spectral analyses and structurally determined.
ꢁ 2007 Elsevier B.V. All rights reserved.
Keywords: Dimolybdenum complexes; Bibenzyl trisulfide; Polymorphs; Thermolytic studies; Desulfurization
1. Introduction
a variety of addition [12,13] and substitution [14,15] type
reactions. Sulfur donor ligands such as thiolato (SRꢀ)
[16,17], thioether (SR2) [18] and hydrosulfido (SHꢀ) [19]
especially have been known to serve as bridging and stabi-
lizing ligands for many of these transition metal complexes.
Among the earliest examples of such thiolato-bridged
cyclopentadienyl complexes were [CpM(CO)2(l-SR)]2
(M = Mo, R = Me [20], Ph [21], But, p-tolyl [22] and
M = Cr, R = Ph [23]), which feature a centered M2S2 ring
but without any metal–metal bonds. All of these complexes
underwent decarbonylation readily on heating to give dou-
bly bonded [CpM(CO)(l-SR)]2. In a preliminary paper, we
reported the facile reaction of [CpCr(CO)3]2 towards Bz2S3
which proceeded at ambient temperature leading to thio-
late-bridged metal complexes as main products [24]. As
part of our ongoing investigation, we wish to report herein
a comparative study of the reactivity of [CpMo(CO)3]2
towards Bz2S3.
Despite several decades of research work on the chemis-
try of transition metal thiolate compounds, the area still
offer interesting new findings and prospects. Basically, the
important features of these compounds lay in their wealth
of bonding, structural and reactivity properties [1,2]. Tran-
sition metal thiolate complexes have generated a lot of
interest due to their importance in catalytic processes such
as desulfurization [3–7] and involvement in a large number
of biological systems [8–11]. Much attention has been
focused especially on the triply bonded complexes [(g5-
Cp)M(CO)2]2 (M = Cr, Mo, W), which have displayed
interesting chemistry due to the high reactivity and versatil-
ity of the metal–metal triple bond which are able to exhibit
*
Corresponding author. Tel.: +60 379674260; fax: +60 379674193.
E-mail address: richard@um.edu.my (R.C.S. Wong).
0020-1693/$ - see front matter ꢁ 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.ica.2007.02.021

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R.C.S. Wong et al. / Inorganica Chimica Acta 360 (2007) 3113–3118
2. Experimental
2.1. General procedures
808m, 698s cmꢀ1 (nujol). Anal. Calc. for
C24H24Mo2S4: C, 45.6; H, 3.8; Mo, 30.4; S, 20.3.
Found: C, 45.6; H, 3.4; Mo, 30.7; S, 19.8%.
(iii) A brownish pink fraction in a 2:1 toluene/ether mix-
ture (25 mL) which gave fine dark pink crystalline
solids of [CpMo(SBz)(S)]2 (4b) (102 mg, 0.161 mmol,
All experiments were carried out under nitrogen using
Schlenk techniques and further manipulation of complexes
were performed inside a dry-box equipped with a HE-493
dri-train under argon atmosphere. 1H and 13C NMR spectra
were measured on a JEOL Lambda FT 400 MHz spectrom-
eter, and chemical shifts referenced to residual C6H6 in ben-
zene-d6. IR spectra in Nujol mulls were measured in the
range 4000–400 cmꢀ1 by means of a Perkin–Elmer 2000
FTIR spectrophotometer. Elemental analyses were per-
formed by the Chemical, Molecular and Materials Analysis
Centre (CMMAC), National University of Singapore.
[CpMo(CO)3]2 was synthesized using Mo(CO)6 pur-
chased from Fluka Ltd. according to Manning’s method
[25]. Bz2S3 was purchased from Sigma–Aldrich Chemical
Company and was used without any purification. Silica
gel (Merck Kieselgel 60, 35–70 mesh) and Celite (Fluka
AG) were dried at 140 ꢀC overnight before chromato-
graphic use. All solvents were distilled with sodium and
benzophenone under nitrogen prior to use.
1
40.3% yield) when concentrate to dryness. H NMR
(C6D6): (C6H5) 7.72–6.89 (m, 10H); (C5H5) 5.84 (s,
5H); (CH2) 2.78 (s, 2H). 13C NMR (C6D6): (CH2)
41.57; (C5H5) 97.95; (S–CH2–C6H5) 129.37, 130.32,
142.05. IR: v at 1667m, 1599w, 1317w, 1276m,
1011w, 800m, 698s cmꢀ1 (nujol).
(iv) A pinkish brown fraction in ether (7 mL) which upon
concentration to dryness under vacuo gave pinkish
brown crystalline solids of [CpMo(CO)(SBz)]2S (3)
[27] (8 mg, 0.012 mmol, 2.9% yield). 1H NMR
(C6D6): (C6H5) 7.42–7.01 (m, 10H); (C5H5) 4.83 (s,
5H); (CH2) 4.02 (s, 2H). 13C NMR (C6D6): (CH2)
49.37; (C5H5) 90.38, 90.71, 91.03, 91.24, 91.56; (S–
CH2–C6H5) 128.74, 143.10; (CO) 244.10. IR: v(CO)
at 1925vs, 1869s, 1846sh cmꢀ1
;
other bands,
1061vw, 1031vw, 1011vw, 813m, 760m, 700m cmꢀ1
(nujol). Anal. Calc. for C26H24Mo2O2S2: C, 47.6; H,
3.7; Mo, 29.3; S, 14.6. Found: C, 47.5; H, 3.8; Mo,
30.2; S, 14.9%. A dark brown band remained un-
eluted on the top of the column.
2.2. Reaction of [CpMo(CO)3]2 (1) with Bz2S3
To a reddish purple solution of [CpMo(CO)3]2 (200 mg,
0.41 mmol) in toluene (ca.20 mL) was added Bz2S3
(114 mg, 0.41 mmol). The reaction mixture was stirred
under nitrogen at 60 ꢀC for 3.5 h. The resultant reddish
brown solution was filtered through a disk of Celite
(1 · 1.5 cm) and concentrated to ca. 2–3 mL, and then
loaded onto a silica gel column (10 · 1.5 cm) which was
prepared in n-hexane. The following fractions were eluted:
2.3. Thermolysis of [CpMo(CO)2(SBz)]2 (2)
A stirred reddish brown solution of 2 (100 mg,
0.147mmol) in toluene (15 mL) was maintained at 60 ꢀC
for ca. 14.5 h. The resultant dark yellowish brown solution
was filtered through Celite (1 cm disk), concentrated (ca.
2 mL) and then loaded onto
a silica gel column
(i) A reddish brown fraction in a 2:1 n-hexane/toluene
mixture (90 mL) which upon concentration to dryness
under vacuo gave dark brown crystalline solids of
[CpMo(CO)2(SBz)]2 (2) [26] (46 mg, 0.067 mmol,
16.3% yield). 1H NMR (C6D6): (C6H5) 7.72–7.03 (m,
10H); (C5H5) 4.61 (s, 5H); (CH2) 3.69 (s, 2H). 13C
NMR (C6D6): (CH2) 38.85; (C5H5) 96.67, 96.72,
96.76, 96.79, (S–CH2–C6H5) 127.72, 128.73, 130.32,
141.15; (CO) 256.67. IR: v(CO) at 1944vs, 1918sh,
1849vs, 1831sh cmꢀ1; other bands, 1067vw, 1029vw,
1009w, 842w, 808m, 700m cmꢀ1 (nujol). Anal. Calc.
for C28H24Mo2O4S2: C, 49.4; H, 3.5; Mo, 28.2; S, 9.4.
Found: C, 49.5; H, 3.6; Mo, 28.5; S, 9.3%.
(1.5 · 10 cm) prepared in n-hexane. Two fractions were
eluted:
(i) A deep pink fraction in a 2:1 toluene/ether mixture
(20 mL) which when concentrated to dryness gave
deep pink crystalline solids of [CpMo(SBz)(S)]2 (4)
(15 mg, 0.024 mmol, 16.3% yield).
(ii) A pinkish brown fraction in ether (15 mL) which
when concentrated to dryness gave dark reddish
brown crystalline solids of 3 (25 mg, 0.038 mmol,
25.9% yield).
(ii) A pink fraction in a 4:1 toluene/ether mixture
(30 mL) which upon concentration to dryness under
vacuo gave fine dark pink crystalline solids of
[CpMo(SBz)(S)]2 (4a) (53 mg, 0.084 mmol, 21.0%
yield). 1H NMR (C6D6): (C6H5) 7.72–7.01 (m,
10H); (C5H5) 5.89 (s, 5H); (CH2) 2.72 (s, 2H). 13C
NMR (C6D6): (CH2) 38.8; (C5H5) 98.07, 98.14,
98.19, 98.22; (S–CH2–C6H5) 129.62, 129.79, 142.26.
IR: v at 1667m, 1599w, 1317w, 1277m, 1008w,
2.4. Thermolysis of [CpMo(CO)(SBz)]2S (3)
A pinkish brown solution of 3 (100 mg, 0.152 mmol) in
toluene (15 mL) was maintained at 110 ꢀC for 18 h. The
resultant dark yellowish brown solution was filtered
through Celite (1 cm disk), concentrated (ca. 2 mL) and
then loaded onto a silica gel column (1.5 · 10 cm) prepared
in n-hexane–toluene (1:1). Only one fraction was eluted as a
pink solution in 2:1 toluene/ether mixture (35 mL) which

R.C.S. Wong et al. / Inorganica Chimica Acta 360 (2007) 3113–3118
3115
when concentrated to dryness gave deep pink crystalline
solids of [CpMo(SBz)(S)]2 (4) (24 mg, 0.038 mmol, 25.0%
yield). A dark brown layer remained uneluted at the top
rim of the column.
2.5. NMR tube reactions
2.5.1. Cothermolysis of [CpMo(CO)2(SBz)]2 (2) with
Bz2S3
A reddish brown solution of 2 (20 mg, 0.029 mmol) in
C6D6 (0.6 mL) placed in a 5 mm NMR tube was heated
with an equivalent of Bz2S3 (8 mg, 0.029 mmol) at 60 ꢀC
1
for 9.5 h. Its H NMR spectrum showed that the resultant
yellowish brown solution consists of [CpMo(CO)(SBz)]2S
(3) (31% yield) and [CpMo(SBz)(S)]2 (4) (49% yield)
together with some uncharacterized dark brown
precipitates.
Fig. 1. ORTEP plot of the monoclinic modification of [(g5-
C5H5)Mo(S)(SCH2C6H5)]2 (4a); the molecule lies on a center-of-inversion
in the crystal structure.
2.5.2. Cothermolysis of [CpMo(CO)(SBz)]2S (3) with
Bz2S3
A pinkish brown solution of 3 (20 mg, 0.030 mmol) in
d8-toluene (0.6 mL) in a 5 mm NMR tube was heated with
an equivalent of Bz2S3 (8 mg, 0.030 mmol) at 110 ꢀC for
15 h. Its 1H NMR spectrum showed that the resultant solu-
tion consists of [CpMo(SBz)(S)]2 (4) (47% yield) together
with some uncharacterized dark brown precipitates.
(CO)2(SBz)]2
(2),
[CpMo(CO)(SBz)]2S
(3)
and
[CpMo(SBz)(S)]2 (4) in 16.3%, 2.9% and 61.3% yields,
respectively. Thermolysis of [CpMo(CO)2(SBz)]2 (2) at
60 ꢀC for 14.5 h has resulted in the isolation of 3 and 4 in
25.9% and 16.3% yields, respectively. Prolonged thermoly-
sis of 3 at an elevated temperature of 110 ꢀC for 18 h
resulted in the isolation of [CpMo(SBz)(S)]2 (4) in 25.0%
yield. NMR tube reaction study of 2 under similar thermo-
3. Results and discussion
3.1. Synthetic pathways
The reaction of [CpMo(CO)3]2 (1) with an equimolar of
Bz2S3 at 60 ꢀC for 3.5 h has led to the isolation of [CpMo
OC
CO
CO
CO
CO
Mo
Mo
Mo
Mo
OC
OC
OC
60 oC
OC
CO
1a
1
Bz2S3
CH2
CH2
S
60 oC
OC
CO
CO
S
OC
CO
S
OC
Mo
Mo
Mo
Mo
S
S
CH2
CH2
110 oC
CH2
S
S
2
3
Mo
+
Mo
S
S
CH2
4
Scheme 1. Proposed synthetic pathway for the reaction of [CpMo(CO)3]2 (1) with Bz2S3.

3116
R.C.S. Wong et al. / Inorganica Chimica Acta 360 (2007) 3113–3118
ized by NMR spectroscopy. As with the Cr analogue,
[CpMo(CO)3]2 (1) also demonstrates the ability to desulfur-
ize trisulfides to disulfides and monosulfides in an effective
manner.
3.2. Structural study
The reported structures of 2 and 3 [26,27] feature a cis
arrangement of the carbonyl ligands similar to the chro-
mium analogue [CpCr(CO)2(SBz)]2. Both have the same
type of non-planar Mo2S2 ring system. The decarbonylated
[CpMo(CO)(SBz)]2S (3) differs from 2 with an extra sulfide
linkage in addition to the two benzylthiolate linkages. The
˚
Mo(1)ꢁ ꢁ ꢁMo(2) separation of 3.836 (3) A of 2 is much
longer than the normal Mo–Mo single bond found in
˚
related dinuclear complex 1 (3.235 A) [31,32] indicates the
absence of metal–metal bond between them.
Fig. 2. ORTEP plot of the orthorhombic modification of [(g5-
C5H5)Mo(S)(SCH2C6H5)]2 (4b); the molecule lies on a center-of-inversion
in the crystal structure.
[CpMo(SBz)S]2 (4) can be obtained as two polymor-
phous species. Complex 4a crystallizes in the space group
Pcba of the orthorhombic system and 4b in the space group
P21/c of the monoclinic system. The ORTEP plots of 4a
and 4b are presented in Figs. 1 and 2 respectively and
define the atomic numbering scheme. Both compounds
consist of a Mo2S4 framework with the geometry of the
Mo atom described as pseudo-pentagonal bipyramidal
and feature a nearly square-planar arrangement of the four
sulfur atoms, perpendicular to the Mo–Mo bond and
almost parallel to the two (g5-C5H5) planes. Their phenyl
groups attached to the thiolato bridges are in an equato-
rial-axial configuration being trans to each other. The qua-
lytic condition, but in the presence of Bz2S3, gave higher
yields of 3 (31%) and 4 (49%). Likewise, thermolysis of 3
in the presence of Bz2S3 also resulted in higher yield of 4
(47%).
A major consequence of reactions involving organic
disulfides (RSSR) is the susceptibility of their S–S linkage
to be cleaved by nucleophilic, electrophilic or radical pro-
cesses [28a,28b,28c]. The closely related organic trisulfides
(RSSSR) having two adjacent sulfur–sulfur bonds as in
Bz2S3 is expected to undergo similar desulfurization pro-
cess as well. According to Harpp et al. [29], the central sul-
fur atom being bonded to two soft sulfur atoms, would be a
softer acceptor than a terminal sulfur atom that is bonded
to a carbon atom hence the desulfurization process is tar-
geted towards the central sulfur. For this reaction, it is pos-
tulated that the coordination of the thiobenzyl moiety from
the desulfurized Bz2S3 has led to the formation of the thio-
late-bridged dimer [CpMo(CO)2(SBz)]2 (2) which was
observed previously in a similar reaction with the Cr ana-
logue [24]. Initial isolation of 2 which underwent stepwise
decarbonylation to yield [CpMo(CO)(SBz)]2S (3) and
finally to the completely decarbonylated [CpMo(SBz)(S)]2
(4) after prolonged thermolysis indicates that 2 is a primary
product (Scheme 1). The partial decarbonylation of 2
results in the loss of two carbonyl ligands but proceeds with
a formal insertion of an S(0) atom (presumably from the
desulfurized Bz2S3) across the singly-bonded Mo center
to form the Mo–(l2–S)–Mo bridged complex 3. Finally, 3
succumbed to complete decarbonylation, coupled with
concomitant sulfur insertions ultimately gave rise to the
mixed quadruply thiolato-bridged complex 4. A different
synthetic route reported by Franz et al. [30] involves a
two-step exchange of both the l2-SH groups from
[CpMo(l-S)(l-SH)]2 with benzylthiol to give the final dib-
enzyl substituted cluster similar to 4 which was character-
druply thiolato-bridged complex belongs to
a well
characterized group of structures which contain a Mo2(l-
S)4 residue such as CpꢂMo2ðl-SCH3Þ ðl-SÞ (Cp* = g5-
2
2
2
pentamethylcyclopentadienyl) [33], Cp2Mo2(l2-SCH3)4
[34], Cp0 Mo2ðl2-SCH3Þ ðl2-SÞ (Cp0 = g5-methylcyclo-
2
2
pentadienyl) [35] and Cp002Mo2ðl2-SCH3Þ (Cp0 = g5-ethyl-
2
4
tetramethylcyclopentadienyl) [36]. In all these complexes,
the formal +4 oxidation state of the Mo atoms would
require the existence of a double bond between them, in
accordance to the demands of the 18 e-rule. Both 4a and
˚
4b with Mo–Mo bond lengths of 2.579(7) and 2.581(5) A
Table 1
Comparison of Mo–Mo bonds and Mo–S bonds in complexes 1–4
Complex Mo–Mo
Mo–S(sulfido)
(A)
Mo–S(thiolato)
(A)
Ref
˚
˚
˚
(A)
1
2
3.235
–
–
–
–
[31,32]
[26]
2.512 (7)
2.521 (7)
2.460 (2)
2.452 (2)
2.465 (1)
2.478 (1)
2.479 (1)
2.476 (1)
3
2.802
2.437 (2)
[27]
4a
4b
2.579 (7)
2.581 (5)
2.341 (1)
2.355 (1)
2.352 (1)
2.344 (1)
this work
this work

R.C.S. Wong et al. / Inorganica Chimica Acta 360 (2007) 3113–3118
3117
Table 2
X-ray crystal data and structure refinement for 4a and 4b
Identification code
4a
4b
Empirical formula
Formula weight
Temperature (K)
C24H24Mo2S2
632.55
223(2)
C24H24Mo2S2
632.55
223(2)
˚
Wavelength (A)
0.71073
0.71073
Crystal system, space group
Unit cell dimensions
monoclinic, P21/c
orthorhombic, Pcba
˚
a (A)
12.084(1)
8.052(1)
˚
b (A)
7.834(1)
12.563(1)
90
98.542(1)
90
1176.1(2)
2, 1.786
1.432
12.328(1)
23.838(1)
90
90
90
2366.3(1)
4, 1.776
1.423
˚
c (A)
a (ꢀ)
b (ꢀ)
c (ꢀ)
3
˚
V, Volume (A )
Z, Calculated density (Mg/m3)
Absorption coefficient (mmꢀ1
F(000)
)
632
1264
Crystal size (mm)
h Range for data collection (ꢀ)
Limiting indices
0.10 · 0.10 · 0.04
1.70–27.54
0.14 · 0.10 · 0.09
1.71–27.53
ꢀ9 6 h 6 10,
ꢀ16 6 k 6 14,
ꢀ24 6 l 6 30
15518/2722 [0.0543]
100
ꢀ15 6 h 6 13,
ꢀ10 6 k 6 10,
ꢀ16 6l 6 15
8009/2693 [0.0360]
100
full-matrix least-squares on F2
2693/0/136
1.063
Reflections collected/unique [Rint
Completeness to h = 27.54 (%)
Refinement method
Data/restraints/parameters
Goodness-of-fit on F2
]
full-matrix least-squares on F2
2722/0/136
1.103
Final R indices [I > 2r(I)]
R indices (all data)
Largest difference in peak and hole (e A
R1 = 0.0434, wR2 = 0.1036
R1 = 0.0559, wR2 = 0.1102
1.302 and ꢀ0.388
R1 = 0.036, wR2 = 0.0753
R1 = 0.0533, wR2 = 0.0816
0.506 and ꢀ0.364
ꢀ3
˚
)
compares very closely to CpꢂMo2ðl-SCH3Þ ðl-SÞ (2.573
[average 2.348(1) A] resulting in a more acute Mo1–S1–
Mo1i angle and a comparison of the measured Mo–Mo
and Mo–S bond lengths for complexes 1–4 is shown in
Table 1. It is likely that these observations arise due to
greater steric repulsions between the SBz group and an S
substituent (Tables 2,3).
˚
2
2
2
˚
0
˚
(1) A) and Cp2Mo2ðl2-SCH3Þ2ðl2-SÞ2 (2.582(1) A) bond
distances. The four S atoms are bonded in a l–g2-mode.
˚
The Mo–S(thiolato) bond distances [average 2.472(1) A]
are significantly longer than the Mo–S(sulfido) distances
Table 3
˚
Bond lengths (A) and angles (ꢀ) for 4a and 4b
Acknowledgements
4a
4b
˚
Bond lengths (A)
The author acknowledges with thanks financial support
from SAGA Grant 66-02-03-0044 from the Academy Of
Sciences Malaysia.
Mo1–C1
Mo1–C2
Mo1–C3
Mo1–C4
Mo1–C5
Mo1–S1
Mo1–S1i
Mo1–S2
Mo1–S2i
Mo1–Mo1i
2.339(4)
2.346(5)
2.348(5)
2.327(4)
2.315(4)
2.465(1)
2.478(1)
2.341(1)
2.355(1)
2.579(2)
2.325(3)
2.312(4)
2.334(4)
2.350(3)
2.351(3)
2.352(1)
2.344(1)
2.479(1)
2.476(1)
2.581(5)
Appendix A. Supplementary material
CCDC 293259, 615748 contains the supplementary crys-
tallographic data for 4a and 4b. These data can be obtained
free of charge via www.ccdc.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 e-mail: deposit@ccdc.cam.ac.uk. Supplemen-
tary data associated with this article can be found, in the
online version, at doi:10.1016/j.ica.2007.02.021.
Bond angles (ꢀ)
S1–Mo1–S1i
S1–Mo1–S2
S1–Mo1–S2i
S1i–Mo1–S2
S1i–Mo1–S2i
S2–Mo1–S2i
Mo1–S1–Mo1i
Mo1–S2–Mo1i
117.1(1)
77.3(1)
69.6(1)
69.6(1)
76.8(1)
113.4(1)
62.9(3)
66.6(3)
113.3(1)
69.7(1)
76.8(1)
76.9(1)
69.9(1)
117.2(1)
66.7(2)
62.8(2)
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