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(μ-4-Methyl­benzene­thiol­ato-κ2S:S)bis­­[carbon­yl(η5-cyclo­penta­dien­yl)molybdenum(II)]

aDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
*Correspondence e-mail: seikweng@um.edu.my

(Received 7 April 2008; accepted 18 April 2008; online 23 April 2008)

The asymmetric unit of the title compound, [Mo2(C5H5)2(C7H7S)2(CO)2], consists of two half-mol­ecules, each molecule lying on a centre of symmetry. The thiol­ate groups function as bridges between the MoII atoms, which adopt a quasi-octa­hedral geometry. In the octa­hedral environment the two ligating S atoms are in a cis arrangement.

Related literature

For related literature on unsubstituted [MoCp(CO)(μ-SC6H5)]2, see: Song et al. (1997[Song, L.-C., Wang, J.-Q., Hu, Q.-M., Wang, R.-J. & Mak, T. C. W. (1997). Inorg. Chim. Acta, 256, 129-135.]). The 4-methyl-substituted compound was characterized spectroscopically, see: Benson et al. (1980[Benson, I. B., Killops, S. D., Know, S. A. R. & Welch, A. J. (1980). J. Chem. Soc. Chem. Commun. pp. 1137-1139.]).

[Scheme 1]

Experimental

Crystal data
  • [Mo2(C5H5)2(C7H7S)2(CO)2]

  • Mr = 624.45

  • Monoclinic, P 21 /n

  • a = 13.245 (2) Å

  • b = 10.135 (1) Å

  • c = 18.042 (2) Å

  • β = 104.901 (2)°

  • V = 2340.4 (5) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 1.27 mm−1

  • T = 100 (2) K

  • 0.06 × 0.06 × 0.06 mm

Data collection
  • Bruker APEXII diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.758, Tmax = 0.928

  • 14384 measured reflections

  • 5374 independent reflections

  • 3915 reflections with I > 2σ(I)

  • Rint = 0.048

Refinement
  • R[F2 > 2σ(F2)] = 0.043

  • wR(F2) = 0.104

  • S = 1.03

  • 5374 reflections

  • 291 parameters

  • H-atom parameters constrained

  • Δρmax = 2.60 e Å−3

  • Δρmin = −1.77 e Å−3

Table 1
Selected bond lengths (Å)

Mo1—S1 2.424 (1)
Mo1—S1i 2.425 (1)
Mo2—S2 2.430 (1)
Mo2—S2ii 2.419 (1)
Symmetry codes: (i) -x+1, -y, -z+1; (ii) -x, -y+1, -z+1.

Data collection: APEX2 (Bruker, 2007[Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2007[Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: X-SEED (Barbour, 2001[Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.]); software used to prepare material for publication: publCIF (Westrip, 2008[Westrip, S. P. (2008). publCIF. In preparation.]).

Supporting information


Comment top

The title compound was characterized spectroscopically in a study on [MoCp(CO)(µ-SAr]2 type of compounds. The compound was synthesized by treating MoClCp(CO)3 with 4-tolyl mercaptan (Benson et al., 1980). We have obtained the title compound (Fig. 1) as the unexpected product in the reaction of [(η5-C5H5)Mo(CO)2]2 with deuterated o-P(PhSCD3)3. Under the conditions of the reaction, the ortho-SD3 groups of the phosphine have been rearranged to the para position. The rearrangement is then followed by an exchange of the deuterium atoms by hydrogen atoms; the absence of deuterium in the compound is confirmed by 1H NMR spectroscopic analysis.

Related literature top

For related literature on unsubstituted [MoCp(CO)(µ-SC6H5)]2, see: Song et al. (1997). The 4-methyl-substituted compound was characterized spectroscopically (see Benson et al., 1980).

Experimental top

A reddish-brown suspension of [(η5-C5H5)Mo(CO)2]2 (100 mg, 0.23 mmol) and an equivalent quantity of the deuterated phosphine, o-P(PhSCD3)3 (94 mg, 0.23 mol), was heated at 383 K for 14.5 h under argon. The mixture was filtered and then absorbed onto Celite (1.5 g). The slurry was evacuated to dryness and loaded onto a silica gel column (9.5 cm x 2.0 cm) in n-hexane. The title compound was eluted with n-hexane-toluene (1:4, 50 ml) as a greenish-brown fraction (60.0 mg, 0.096 mmol, 40% yield). The dichroic compound was recrystallized from an n-hexane-toluene mixture and crystals were isolated after 2 d.

Refinement top

H-atoms were placed in calculated positions (C—H = 0.95–1.00 Å) and were included in the refinement in the riding-model approximation, with Uiso(H) = 1.2–1.5Ueq(C). The final difference Fourier map had a peak at 0.80 Å and a deep hole at 0.68 Å from Mo2.

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2008).

Figures top
[Figure 1] Fig. 1. Displacement ellipsoid plot (Barbour, 2001) of the two independent dimeric [Mo(C5H5)(CO)(C7H7S)]2 molecules, drawn at the 70% probability level. H atoms are drawn as spheres of arbitrary radii. For molecules with Mo1 and Mo2, the unlabeled atoms are related to the labeled ones by (1 - x, -y, 1 - z) and (-x, 1 - y, 1 - z), respectively.
(µ-4-Methylbenzenethiolato-κ2S:S)bis[carbonyl(η5- cyclopentadienyl)molybdenum(II)] top
Crystal data top
[Mo2(C5H5)2(C7H7S)2(CO)2]F(000) = 1248
Mr = 624.45Dx = 1.772 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 2210 reflections
a = 13.245 (2) Åθ = 2.3–24.8°
b = 10.135 (1) ŵ = 1.27 mm1
c = 18.042 (2) ÅT = 100 K
β = 104.901 (2)°Cube, green–brown
V = 2340.4 (5) Å30.06 × 0.06 × 0.06 mm
Z = 4
Data collection top
Bruker APEXII
diffractometer
5374 independent reflections
Radiation source: fine-focus sealed tube3915 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.048
ϕ and ω scansθmax = 27.5°, θmin = 1.7°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1716
Tmin = 0.758, Tmax = 0.928k = 713
14384 measured reflectionsl = 2323
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.043Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.104H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0453P)2 + 1.5589P]
where P = (Fo2 + 2Fc2)/3
5374 reflections(Δ/σ)max = 0.001
291 parametersΔρmax = 2.60 e Å3
0 restraintsΔρmin = 1.78 e Å3
Crystal data top
[Mo2(C5H5)2(C7H7S)2(CO)2]V = 2340.4 (5) Å3
Mr = 624.45Z = 4
Monoclinic, P21/nMo Kα radiation
a = 13.245 (2) ŵ = 1.27 mm1
b = 10.135 (1) ÅT = 100 K
c = 18.042 (2) Å0.06 × 0.06 × 0.06 mm
β = 104.901 (2)°
Data collection top
Bruker APEXII
diffractometer
5374 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
3915 reflections with I > 2σ(I)
Tmin = 0.758, Tmax = 0.928Rint = 0.048
14384 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0430 restraints
wR(F2) = 0.104H-atom parameters constrained
S = 1.03Δρmax = 2.60 e Å3
5374 reflectionsΔρmin = 1.78 e Å3
291 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mo10.53951 (3)0.10457 (4)0.53870 (2)0.01595 (11)
Mo20.01435 (3)0.62084 (4)0.47776 (2)0.02086 (11)
S10.49151 (8)0.09871 (11)0.39974 (6)0.0174 (2)
S20.00847 (9)0.55650 (11)0.61079 (6)0.0195 (2)
O10.7457 (2)0.0389 (3)0.53895 (18)0.0277 (8)
O20.2474 (2)0.5238 (4)0.4399 (2)0.0345 (9)
C10.4768 (4)0.2943 (4)0.5899 (3)0.0261 (11)
H10.40260.31180.59010.031*
C20.5256 (4)0.3337 (4)0.5324 (3)0.0262 (11)
H20.49220.38620.48560.031*
C30.6331 (4)0.2982 (4)0.5566 (3)0.0235 (10)
H30.68860.32370.53090.028*
C40.6493 (3)0.2359 (4)0.6296 (2)0.0209 (10)
H40.71830.20860.66360.025*
C50.5531 (4)0.2342 (4)0.6494 (2)0.0223 (10)
H50.54200.20220.69910.027*
C60.6654 (4)0.0091 (4)0.5356 (2)0.0212 (10)
C70.6066 (3)0.1070 (5)0.3651 (2)0.0188 (9)
C80.6512 (4)0.0029 (5)0.3415 (3)0.0253 (10)
H80.62450.08820.34710.030*
C90.7354 (4)0.0111 (5)0.3093 (3)0.0261 (11)
H90.76480.06530.29260.031*
C100.7776 (4)0.1338 (5)0.3010 (3)0.0247 (10)
C110.7337 (4)0.2431 (5)0.3263 (3)0.0272 (11)
H110.76250.32790.32260.033*
C120.6477 (3)0.2307 (5)0.3573 (2)0.0213 (10)
H120.61730.30720.37300.026*
C130.8678 (4)0.1468 (6)0.2643 (3)0.0355 (13)
H13A0.90590.22870.28170.053*
H13B0.84100.14860.20840.053*
H13C0.91500.07140.27920.053*
C140.0611 (4)0.7759 (5)0.4160 (3)0.0269 (11)
H140.11350.75840.38600.032*
C150.0495 (4)0.7844 (5)0.3857 (3)0.0258 (11)
H150.08810.77260.33070.031*
C160.0927 (4)0.8291 (5)0.4449 (3)0.0279 (11)
H160.16790.85100.43950.033*
C170.0100 (4)0.8469 (4)0.5119 (3)0.0302 (12)
H170.01720.88270.56190.036*
C180.0835 (4)0.8158 (5)0.4944 (3)0.0276 (11)
H180.15490.82740.52950.033*
C190.1602 (4)0.5542 (5)0.4557 (3)0.0279 (11)
C200.1100 (3)0.5593 (4)0.6420 (2)0.0178 (9)
C210.1885 (3)0.6503 (4)0.6146 (3)0.0225 (10)
H210.18270.71130.57590.027*
C220.2757 (4)0.6521 (5)0.6437 (3)0.0232 (10)
H220.32930.71480.62420.028*
C230.2869 (3)0.5659 (5)0.6999 (3)0.0217 (10)
C240.2062 (3)0.4753 (4)0.7287 (2)0.0206 (10)
H240.21180.41520.76780.025*
C250.1182 (3)0.4732 (4)0.7002 (2)0.0199 (9)
H250.06330.41260.72060.024*
C260.3837 (4)0.5654 (5)0.7300 (3)0.0282 (11)
H26A0.40870.65610.73180.042*
H26B0.36660.52760.78180.042*
H26C0.43830.51240.69610.042*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.0185 (2)0.01103 (19)0.01885 (19)0.00035 (15)0.00568 (15)0.00125 (15)
Mo20.0320 (2)0.01180 (19)0.0223 (2)0.00178 (17)0.01341 (17)0.00156 (16)
S10.0177 (5)0.0141 (5)0.0211 (5)0.0004 (4)0.0062 (4)0.0003 (4)
S20.0217 (6)0.0178 (6)0.0203 (5)0.0011 (4)0.0077 (4)0.0015 (4)
O10.0218 (18)0.0253 (19)0.039 (2)0.0060 (15)0.0126 (15)0.0047 (15)
O20.0170 (18)0.042 (2)0.043 (2)0.0054 (16)0.0061 (15)0.0146 (18)
C10.031 (3)0.014 (2)0.035 (3)0.004 (2)0.011 (2)0.011 (2)
C20.042 (3)0.011 (2)0.025 (2)0.000 (2)0.007 (2)0.0026 (19)
C30.031 (3)0.015 (2)0.023 (2)0.008 (2)0.005 (2)0.0039 (18)
C40.023 (2)0.016 (2)0.021 (2)0.0067 (19)0.0008 (18)0.0057 (18)
C50.033 (3)0.014 (2)0.021 (2)0.0059 (19)0.009 (2)0.0046 (18)
C60.030 (3)0.013 (2)0.020 (2)0.005 (2)0.006 (2)0.0012 (18)
C70.017 (2)0.022 (2)0.018 (2)0.0009 (19)0.0057 (17)0.0018 (19)
C80.027 (3)0.019 (2)0.032 (3)0.001 (2)0.012 (2)0.001 (2)
C90.024 (3)0.028 (3)0.028 (3)0.001 (2)0.009 (2)0.003 (2)
C100.025 (2)0.030 (3)0.020 (2)0.008 (2)0.0079 (19)0.003 (2)
C110.033 (3)0.027 (3)0.022 (2)0.010 (2)0.010 (2)0.001 (2)
C120.029 (2)0.017 (2)0.018 (2)0.0010 (19)0.0062 (19)0.0025 (18)
C130.037 (3)0.040 (3)0.035 (3)0.011 (2)0.019 (2)0.009 (2)
C140.035 (3)0.017 (2)0.032 (3)0.000 (2)0.016 (2)0.008 (2)
C150.038 (3)0.015 (2)0.028 (3)0.005 (2)0.013 (2)0.0070 (19)
C160.030 (3)0.016 (2)0.042 (3)0.004 (2)0.017 (2)0.005 (2)
C170.062 (4)0.008 (2)0.030 (3)0.002 (2)0.027 (3)0.0018 (19)
C180.039 (3)0.015 (2)0.030 (3)0.006 (2)0.010 (2)0.004 (2)
C190.036 (3)0.023 (3)0.028 (3)0.003 (2)0.015 (2)0.003 (2)
C200.019 (2)0.015 (2)0.019 (2)0.0018 (17)0.0052 (18)0.0048 (17)
C210.030 (3)0.017 (2)0.023 (2)0.0026 (19)0.011 (2)0.0028 (18)
C220.028 (2)0.018 (2)0.024 (2)0.005 (2)0.0067 (19)0.0032 (19)
C230.024 (2)0.019 (2)0.023 (2)0.0015 (19)0.0082 (19)0.0089 (19)
C240.028 (2)0.014 (2)0.021 (2)0.0013 (19)0.0070 (19)0.0002 (18)
C250.022 (2)0.016 (2)0.021 (2)0.0028 (18)0.0041 (18)0.0015 (18)
C260.025 (3)0.026 (3)0.035 (3)0.000 (2)0.010 (2)0.002 (2)
Geometric parameters (Å, º) top
Mo1—C61.941 (5)C8—C91.390 (6)
Mo1—C32.299 (4)C8—H80.95
Mo1—C42.312 (4)C9—C101.388 (7)
Mo1—C22.330 (5)C9—H90.95
Mo1—C52.359 (4)C10—C111.381 (7)
Mo1—C12.374 (4)C10—C131.513 (6)
Mo1—S12.424 (1)C11—C121.398 (6)
Mo1—S1i2.425 (1)C11—H110.95
Mo1—Mo1i2.6052 (8)C12—H120.95
Mo2—C191.988 (5)C13—H13A0.98
Mo2—C142.298 (5)C13—H13B0.98
Mo2—C152.308 (4)C13—H13C0.98
Mo2—C182.340 (5)C14—C151.428 (7)
Mo2—C162.359 (5)C14—C181.428 (7)
Mo2—C172.370 (5)C14—H141.00
Mo2—S22.430 (1)C15—C161.410 (6)
Mo2—S2ii2.419 (1)C15—H151.00
Mo2—Mo2ii2.5751 (8)C16—C171.419 (7)
S1—C71.792 (4)C16—H161.00
S1—Mo1i2.4252 (12)C17—C181.391 (7)
S2—C201.799 (4)C17—H171.00
S2—Mo2ii2.4192 (12)C18—H181.00
O1—C61.157 (5)C20—C211.382 (6)
O2—C191.159 (6)C20—C251.391 (6)
C1—C51.409 (6)C21—C221.387 (6)
C1—C21.414 (7)C21—H210.95
C1—H11.00C22—C231.376 (6)
C2—C31.423 (6)C22—H220.95
C2—H21.00C23—C241.403 (6)
C3—C41.426 (6)C23—C261.516 (6)
C3—H31.00C24—C251.390 (6)
C4—C51.410 (6)C24—H240.95
C4—H41.00C25—H250.95
C5—H51.00C26—H26A0.98
C7—C81.380 (6)C26—H26B0.98
C7—C121.388 (6)C26—H26C0.98
C6—Mo1—C389.65 (18)C4—C3—H3126.1
C6—Mo1—C485.36 (17)Mo1—C3—H3126.1
C3—Mo1—C436.02 (15)C5—C4—C3107.9 (4)
C6—Mo1—C2123.59 (18)C5—C4—Mo174.2 (2)
C3—Mo1—C235.81 (16)C3—C4—Mo171.5 (2)
C4—Mo1—C259.25 (16)C5—C4—H4125.8
C6—Mo1—C5115.04 (17)C3—C4—H4125.8
C3—Mo1—C558.96 (16)Mo1—C4—H4125.8
C4—Mo1—C535.11 (15)C1—C5—C4108.6 (4)
C2—Mo1—C558.27 (16)C1—C5—Mo173.3 (2)
C6—Mo1—C1143.52 (17)C4—C5—Mo170.6 (2)
C3—Mo1—C158.91 (17)C1—C5—H5125.6
C4—Mo1—C158.47 (16)C4—C5—H5125.6
C2—Mo1—C134.99 (16)Mo1—C5—H5125.6
C5—Mo1—C134.63 (16)O1—C6—Mo1173.3 (4)
C6—Mo1—S187.53 (13)C8—C7—C12119.1 (4)
C3—Mo1—S198.92 (11)C8—C7—S1122.7 (4)
C4—Mo1—S1134.23 (11)C12—C7—S1118.0 (3)
C2—Mo1—S188.70 (12)C7—C8—C9120.0 (4)
C5—Mo1—S1146.32 (12)C7—C8—H8120.0
C1—Mo1—S1113.43 (12)C9—C8—H8120.0
C6—Mo1—S1i80.65 (13)C10—C9—C8121.7 (5)
C3—Mo1—S1i144.04 (11)C10—C9—H9119.2
C4—Mo1—S1i108.29 (11)C8—C9—H9119.2
C2—Mo1—S1i148.06 (12)C11—C10—C9117.9 (4)
C5—Mo1—S1i94.04 (11)C11—C10—C13121.4 (4)
C1—Mo1—S1i113.10 (12)C9—C10—C13120.7 (4)
S1—Mo1—S1i115.00 (3)C10—C11—C12121.0 (5)
C6—Mo1—Mo1i78.96 (13)C10—C11—H11119.5
C3—Mo1—Mo1i153.86 (12)C12—C11—H11119.5
C4—Mo1—Mo1i160.22 (12)C7—C12—C11120.2 (4)
C2—Mo1—Mo1i140.25 (12)C7—C12—H12119.9
C5—Mo1—Mo1i147.12 (11)C11—C12—H12119.9
C1—Mo1—Mo1i137.32 (12)C10—C13—H13A109.5
S1—Mo1—Mo1i57.53 (3)C10—C13—H13B109.5
S1i—Mo1—Mo1i57.47 (3)H13A—C13—H13B109.5
C19—Mo2—C14131.04 (19)C10—C13—H13C109.5
C19—Mo2—C1595.41 (19)H13A—C13—H13C109.5
C14—Mo2—C1536.11 (16)H13B—C13—H13C109.5
C19—Mo2—C18142.23 (19)C15—C14—C18107.1 (4)
C14—Mo2—C1835.85 (16)C15—C14—Mo272.3 (3)
C15—Mo2—C1859.24 (17)C18—C14—Mo273.7 (3)
C19—Mo2—C1684.92 (19)C15—C14—H14126.2
C14—Mo2—C1658.97 (17)C18—C14—H14126.2
C15—Mo2—C1635.15 (16)Mo2—C14—H14126.2
C18—Mo2—C1658.02 (17)C16—C15—C14107.8 (4)
C19—Mo2—C17109.75 (19)C16—C15—Mo274.4 (3)
C14—Mo2—C1758.68 (17)C14—C15—Mo271.6 (3)
C15—Mo2—C1758.62 (16)C16—C15—H15125.9
C18—Mo2—C1734.35 (17)C14—C15—H15125.9
C16—Mo2—C1734.91 (17)Mo2—C15—H15125.9
C19—Mo2—S2ii79.05 (14)C15—C16—C17108.1 (4)
C14—Mo2—S2ii95.51 (13)C15—C16—Mo270.4 (3)
C15—Mo2—S2ii95.34 (12)C17—C16—Mo272.9 (3)
C18—Mo2—S2ii126.98 (12)C15—C16—H16125.9
C16—Mo2—S2ii125.83 (13)C17—C16—H16125.9
C17—Mo2—S2ii152.53 (11)Mo2—C16—H16125.9
C19—Mo2—S288.51 (14)C18—C17—C16108.4 (4)
C14—Mo2—S2134.69 (13)C18—C17—Mo271.7 (3)
C15—Mo2—S2148.71 (12)C16—C17—Mo272.2 (3)
C18—Mo2—S2100.11 (12)C18—C17—H17125.7
C16—Mo2—S2115.04 (12)C16—C17—H17125.7
C17—Mo2—S290.83 (12)Mo2—C17—H17125.7
S2ii—Mo2—S2115.85 (3)C17—C18—C14108.5 (4)
C19—Mo2—Mo2ii78.29 (15)C17—C18—Mo274.0 (3)
C14—Mo2—Mo2ii138.92 (12)C14—C18—Mo270.5 (3)
C15—Mo2—Mo2ii153.36 (12)C17—C18—H18125.6
C18—Mo2—Mo2ii136.94 (13)C14—C18—H18125.6
C16—Mo2—Mo2ii161.67 (12)Mo2—C18—H18125.6
C17—Mo2—Mo2ii147.90 (12)O2—C19—Mo2175.0 (4)
S2ii—Mo2—Mo2ii58.12 (3)C21—C20—C25119.4 (4)
S2—Mo2—Mo2ii57.72 (3)C21—C20—S2122.3 (3)
C7—S1—Mo1109.82 (14)C25—C20—S2118.0 (3)
C7—S1—Mo1i117.34 (15)C20—C21—C22119.8 (4)
Mo1—S1—Mo1i65.00 (3)C20—C21—H21120.1
C20—S2—Mo2ii113.39 (14)C22—C21—H21120.1
C20—S2—Mo2114.07 (14)C23—C22—C21121.9 (4)
Mo2ii—S2—Mo264.15 (3)C23—C22—H22119.0
C5—C1—C2107.9 (4)C21—C22—H22119.0
C5—C1—Mo172.1 (3)C22—C23—C24118.2 (4)
C2—C1—Mo170.8 (3)C22—C23—C26121.8 (4)
C5—C1—H1126.0C24—C23—C26120.0 (4)
C2—C1—H1126.0C25—C24—C23120.3 (4)
Mo1—C1—H1126.0C25—C24—H24119.8
C1—C2—C3108.2 (4)C23—C24—H24119.8
C1—C2—Mo174.2 (3)C24—C25—C20120.3 (4)
C3—C2—Mo170.9 (3)C24—C25—H25119.8
C1—C2—H2125.7C20—C25—H25119.8
C3—C2—H2125.7C23—C26—H26A109.5
Mo1—C2—H2125.7C23—C26—H26B109.5
C2—C3—C4107.3 (4)H26A—C26—H26B109.5
C2—C3—Mo173.3 (3)C23—C26—H26C109.5
C4—C3—Mo172.5 (2)H26A—C26—H26C109.5
C2—C3—H3126.1H26B—C26—H26C109.5
C6—Mo1—S1—C733.3 (2)Mo1i—Mo1—C5—C4144.4 (2)
C3—Mo1—S1—C756.0 (2)Mo1—S1—C7—C8100.0 (4)
C4—Mo1—S1—C747.8 (2)Mo1i—S1—C7—C828.6 (4)
C2—Mo1—S1—C790.4 (2)Mo1—S1—C7—C1284.4 (3)
C5—Mo1—S1—C7101.1 (3)Mo1i—S1—C7—C12155.8 (3)
C1—Mo1—S1—C7115.9 (2)C12—C7—C8—C90.8 (7)
S1i—Mo1—S1—C7111.75 (17)S1—C7—C8—C9174.7 (3)
Mo1i—Mo1—S1—C7111.75 (17)C7—C8—C9—C100.8 (7)
C6—Mo1—S1—Mo1i78.49 (13)C8—C9—C10—C110.5 (7)
C3—Mo1—S1—Mo1i167.74 (12)C8—C9—C10—C13178.8 (4)
C4—Mo1—S1—Mo1i159.57 (16)C9—C10—C11—C121.8 (7)
C2—Mo1—S1—Mo1i157.81 (13)C13—C10—C11—C12177.4 (4)
C5—Mo1—S1—Mo1i147.2 (2)C8—C7—C12—C110.5 (6)
C1—Mo1—S1—Mo1i132.37 (13)S1—C7—C12—C11176.3 (3)
S1i—Mo1—S1—Mo1i0.0C10—C11—C12—C71.9 (7)
C19—Mo2—S2—C2028.4 (2)C19—Mo2—C14—C1511.2 (4)
C14—Mo2—S2—C20125.5 (2)C18—Mo2—C14—C15114.5 (4)
C15—Mo2—S2—C2069.6 (3)C16—Mo2—C14—C1537.4 (3)
C18—Mo2—S2—C20114.6 (2)C17—Mo2—C14—C1578.4 (3)
C16—Mo2—S2—C2055.3 (2)S2ii—Mo2—C14—C1591.5 (3)
C17—Mo2—S2—C2081.3 (2)S2—Mo2—C14—C15133.1 (2)
S2ii—Mo2—S2—C20105.47 (16)Mo2ii—Mo2—C14—C15137.3 (2)
Mo2ii—Mo2—S2—C20105.47 (16)C19—Mo2—C14—C18125.8 (3)
C19—Mo2—S2—Mo2ii77.08 (14)C15—Mo2—C14—C18114.5 (4)
C14—Mo2—S2—Mo2ii129.00 (17)C16—Mo2—C14—C1877.1 (3)
C15—Mo2—S2—Mo2ii175.1 (2)C17—Mo2—C14—C1836.1 (3)
C18—Mo2—S2—Mo2ii139.93 (13)S2ii—Mo2—C14—C18153.9 (3)
C16—Mo2—S2—Mo2ii160.76 (14)S2—Mo2—C14—C1818.6 (4)
C17—Mo2—S2—Mo2ii173.19 (13)Mo2ii—Mo2—C14—C18108.1 (3)
S2ii—Mo2—S2—Mo2ii0.0C18—C14—C15—C160.2 (5)
C6—Mo1—C1—C545.1 (4)Mo2—C14—C15—C1666.2 (3)
C3—Mo1—C1—C579.2 (3)C18—C14—C15—Mo266.0 (3)
C4—Mo1—C1—C536.8 (3)C19—Mo2—C15—C1673.2 (3)
C2—Mo1—C1—C5117.1 (4)C14—Mo2—C15—C16115.3 (4)
S1—Mo1—C1—C5165.6 (2)C18—Mo2—C15—C1677.0 (3)
S1i—Mo1—C1—C561.1 (3)C17—Mo2—C15—C1636.7 (3)
Mo1i—Mo1—C1—C5127.6 (2)S2ii—Mo2—C15—C16152.7 (3)
C6—Mo1—C1—C272.0 (4)S2—Mo2—C15—C1622.9 (4)
C3—Mo1—C1—C237.8 (3)Mo2ii—Mo2—C15—C16147.8 (3)
C4—Mo1—C1—C280.2 (3)C19—Mo2—C15—C14171.5 (3)
C5—Mo1—C1—C2117.1 (4)C18—Mo2—C15—C1438.3 (3)
S1—Mo1—C1—C248.5 (3)C16—Mo2—C15—C14115.3 (4)
S1i—Mo1—C1—C2178.2 (2)C17—Mo2—C15—C1478.6 (3)
Mo1i—Mo1—C1—C2115.4 (3)S2ii—Mo2—C15—C1492.0 (3)
C5—C1—C2—C30.3 (5)S2—Mo2—C15—C1492.4 (3)
Mo1—C1—C2—C363.2 (3)Mo2ii—Mo2—C15—C1496.9 (4)
C5—C1—C2—Mo163.0 (3)C14—C15—C16—C170.6 (5)
C6—Mo1—C2—C1137.3 (3)Mo2—C15—C16—C1763.6 (3)
C3—Mo1—C2—C1116.2 (4)C14—C15—C16—Mo264.3 (3)
C4—Mo1—C2—C177.8 (3)C19—Mo2—C16—C15106.9 (3)
C5—Mo1—C2—C136.5 (3)C14—Mo2—C16—C1538.4 (3)
S1—Mo1—C2—C1136.6 (3)C18—Mo2—C16—C1580.7 (3)
S1i—Mo1—C2—C13.1 (4)C17—Mo2—C16—C15117.0 (4)
Mo1i—Mo1—C2—C1106.7 (3)S2ii—Mo2—C16—C1534.3 (3)
C6—Mo1—C2—C321.1 (3)S2—Mo2—C16—C15167.1 (3)
C4—Mo1—C2—C338.4 (3)Mo2ii—Mo2—C16—C15130.5 (4)
C5—Mo1—C2—C379.7 (3)C19—Mo2—C16—C17136.1 (3)
C1—Mo1—C2—C3116.2 (4)C14—Mo2—C16—C1778.6 (3)
S1—Mo1—C2—C3107.2 (3)C15—Mo2—C16—C17117.0 (4)
S1i—Mo1—C2—C3113.1 (3)C18—Mo2—C16—C1736.3 (3)
Mo1i—Mo1—C2—C3137.1 (2)S2ii—Mo2—C16—C17151.4 (2)
C1—C2—C3—C40.4 (5)S2—Mo2—C16—C1750.1 (3)
Mo1—C2—C3—C465.0 (3)Mo2ii—Mo2—C16—C17112.4 (4)
C1—C2—C3—Mo165.4 (3)C15—C16—C17—C180.9 (5)
C6—Mo1—C3—C2162.6 (3)Mo2—C16—C17—C1862.9 (3)
C4—Mo1—C3—C2114.9 (4)C15—C16—C17—Mo262.0 (3)
C5—Mo1—C3—C277.6 (3)C19—Mo2—C17—C18164.4 (3)
C1—Mo1—C3—C236.9 (3)C14—Mo2—C17—C1837.7 (3)
S1—Mo1—C3—C275.1 (3)C15—Mo2—C17—C1880.3 (3)
S1i—Mo1—C3—C2124.0 (2)C16—Mo2—C17—C18117.2 (4)
Mo1i—Mo1—C3—C299.1 (3)S2ii—Mo2—C17—C1859.8 (4)
C6—Mo1—C3—C482.6 (3)S2—Mo2—C17—C18106.9 (3)
C2—Mo1—C3—C4114.9 (4)Mo2ii—Mo2—C17—C1896.0 (3)
C5—Mo1—C3—C437.3 (3)C19—Mo2—C17—C1647.2 (3)
C1—Mo1—C3—C477.9 (3)C14—Mo2—C17—C1679.5 (3)
S1—Mo1—C3—C4170.0 (2)C15—Mo2—C17—C1636.9 (3)
S1i—Mo1—C3—C49.1 (4)C18—Mo2—C17—C16117.2 (4)
Mo1i—Mo1—C3—C4146.0 (2)S2ii—Mo2—C17—C1657.4 (4)
C2—C3—C4—C50.3 (5)S2—Mo2—C17—C16136.0 (3)
Mo1—C3—C4—C565.8 (3)Mo2ii—Mo2—C17—C16146.8 (2)
C2—C3—C4—Mo165.5 (3)C16—C17—C18—C140.8 (5)
C6—Mo1—C4—C5148.6 (3)Mo2—C17—C18—C1462.4 (3)
C3—Mo1—C4—C5115.6 (4)C16—C17—C18—Mo263.2 (3)
C2—Mo1—C4—C577.4 (3)C15—C14—C18—C170.4 (5)
C1—Mo1—C4—C536.3 (3)Mo2—C14—C18—C1764.7 (3)
S1—Mo1—C4—C5129.4 (2)C15—C14—C18—Mo265.1 (3)
S1i—Mo1—C4—C570.1 (3)C19—Mo2—C18—C1724.4 (4)
Mo1i—Mo1—C4—C5111.1 (4)C14—Mo2—C18—C17116.9 (4)
C6—Mo1—C4—C395.8 (3)C15—Mo2—C18—C1778.3 (3)
C2—Mo1—C4—C338.1 (3)C16—Mo2—C18—C1736.9 (3)
C5—Mo1—C4—C3115.6 (4)S2ii—Mo2—C18—C17150.1 (2)
C1—Mo1—C4—C379.3 (3)S2—Mo2—C18—C1776.4 (3)
S1—Mo1—C4—C313.8 (3)Mo2ii—Mo2—C18—C17129.3 (3)
S1i—Mo1—C4—C3174.4 (2)C19—Mo2—C18—C1492.5 (4)
Mo1i—Mo1—C4—C3133.3 (3)C15—Mo2—C18—C1438.6 (3)
C2—C1—C5—C40.1 (5)C16—Mo2—C18—C1480.0 (3)
Mo1—C1—C5—C462.2 (3)C17—Mo2—C18—C14116.9 (4)
C2—C1—C5—Mo162.1 (3)S2ii—Mo2—C18—C1433.2 (3)
C3—C4—C5—C10.2 (5)S2—Mo2—C18—C14166.7 (3)
Mo1—C4—C5—C163.9 (3)Mo2ii—Mo2—C18—C14113.8 (3)
C3—C4—C5—Mo164.0 (3)Mo2ii—S2—C20—C21104.6 (4)
C6—Mo1—C5—C1152.3 (3)Mo2—S2—C20—C2133.7 (4)
C3—Mo1—C5—C179.1 (3)Mo2ii—S2—C20—C2580.6 (3)
C4—Mo1—C5—C1117.3 (4)Mo2—S2—C20—C25151.6 (3)
C2—Mo1—C5—C136.9 (3)C25—C20—C21—C222.0 (7)
S1—Mo1—C5—C124.3 (4)S2—C20—C21—C22176.6 (3)
S1i—Mo1—C5—C1126.1 (3)C20—C21—C22—C230.3 (7)
Mo1i—Mo1—C5—C198.2 (3)C21—C22—C23—C240.9 (7)
C6—Mo1—C5—C435.0 (3)C21—C22—C23—C26178.2 (4)
C3—Mo1—C5—C438.2 (3)C22—C23—C24—C250.5 (6)
C2—Mo1—C5—C480.5 (3)C26—C23—C24—C25178.6 (4)
C1—Mo1—C5—C4117.3 (4)C23—C24—C25—C201.1 (7)
S1—Mo1—C5—C493.0 (3)C21—C20—C25—C242.3 (6)
S1i—Mo1—C5—C4116.5 (3)S2—C20—C25—C24177.2 (3)
Symmetry codes: (i) x+1, y, z+1; (ii) x, y+1, z+1.

Experimental details

Crystal data
Chemical formula[Mo2(C5H5)2(C7H7S)2(CO)2]
Mr624.45
Crystal system, space groupMonoclinic, P21/n
Temperature (K)100
a, b, c (Å)13.245 (2), 10.135 (1), 18.042 (2)
β (°) 104.901 (2)
V3)2340.4 (5)
Z4
Radiation typeMo Kα
µ (mm1)1.27
Crystal size (mm)0.06 × 0.06 × 0.06
Data collection
DiffractometerBruker APEXII
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.758, 0.928
No. of measured, independent and
observed [I > 2σ(I)] reflections
14384, 5374, 3915
Rint0.048
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.043, 0.104, 1.03
No. of reflections5374
No. of parameters291
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)2.60, 1.78

Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), publCIF (Westrip, 2008).

Selected bond lengths (Å) top
Mo1—S12.424 (1)Mo2—S22.430 (1)
Mo1—S1i2.425 (1)Mo2—S2ii2.419 (1)
Mo1—Mo1i2.6052 (8)Mo2—Mo2ii2.5751 (8)
Symmetry codes: (i) x+1, y, z+1; (ii) x, y+1, z+1.
 

Acknowledgements

The authors thank the Science Fund MOSTI (grant No. 03-01-03-SF0209) for funding this study, and the University of Malaya for the purchase of the diffractometer.

References

First citationBarbour, L. J. (2001). J. Supramol. Chem. 1, 189–191.  CrossRef CAS Google Scholar
First citationBenson, I. B., Killops, S. D., Know, S. A. R. & Welch, A. J. (1980). J. Chem. Soc. Chem. Commun. pp. 1137–1139.  CrossRef Web of Science Google Scholar
First citationBruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationSheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationSong, L.-C., Wang, J.-Q., Hu, Q.-M., Wang, R.-J. & Mak, T. C. W. (1997). Inorg. Chim. Acta, 256, 129–135.  CSD CrossRef CAS Web of Science Google Scholar
First citationWestrip, S. P. (2008). publCIF. In preparation.  Google Scholar

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