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Journal List > Acta Crystallogr Sect E Struct Rep Online > v.64(Pt 5); May 1, 2008

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Acta Crystallogr Sect E Struct Rep Online. 2008 May 1; 64(Pt 5): m695.
Published online 2008 April 23. doi: 10.1107/S1600536808010751.
PMCID: PMC2961228
Copyright © Wong et al. 2008
(μ-4-Methyl­benzene­thiol­ato-κ2 S:S)bis­[carbon­yl(η5-cyclo­penta­dien­yl)molybdenum(II)]
Richard Chee Seng Wong,a Mei Lee Ooi,a and Seik Weng Nga*
aDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
Correspondence e-mail: seikweng/at/um.edu.my
Received April 7, 2008; Accepted April 18, 2008.
This is an open-access article distributed under the terms of the Creative Commons Attribution Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
Abstract
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 [triangle]). The 4-methyl-substituted compound was characterized spectroscopically, see: Benson et al. (1980 [triangle]).
Click on image to enlarge
An external file that holds a picture, illustration, etc. Object name is e-64-0m695-scheme1.jpg Object name is e-64-0m695-scheme1.jpg
Crystal data
  • [Mo2(C5H5)2(C7H7S)2(CO)2]
  • M r = 624.45
  • Monoclinic, An external file that holds a picture, illustration, etc. Object name is e-64-0m695-efi1.jpg
  • 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 [triangle]) T min = 0.758, T max = 0.928
  • 14384 measured reflections
  • 5374 independent reflections
  • 3915 reflections with I > 2σ(I)
  • R int = 0.048
Refinement
  • R[F 2 > 2σ(F 2)] = 0.043
  • wR(F 2) = 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
Data collection: APEX2 (Bruker, 2007 [triangle]); cell refinement: SAINT (Bruker, 2007 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: X-SEED (Barbour, 2001 [triangle]); software used to prepare material for publication: publCIF (Westrip, 2008 [triangle]).
​
Table 1
Table 1
Selected bond lengths (Å)
Supplementary Material
Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808010751/ci2579sup1.cif
Click here to view.(31K, cif)
Structure factors: contains datablocks I. DOI: 10.1107/S1600536808010751/ci2579Isup2.hkl
Click here to view.(263K, hkl)
Additional supplementary materials: crystallographic information; 3D view; checkCIF report
Acknowledgments
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.
supplementary crystallographic information
Comment
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.
Experimental
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
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.
Figures
Fig. 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 (more ...)
Crystal data
[Mo2(C5H5)2(C7H7S)2(CO)2]F000 = 1248
Mr = 624.45Dx = 1.772 Mg m−3
Monoclinic, P21/nMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 2210 reflections
a = 13.245 (2) Åθ = 2.3–24.8º
b = 10.135 (1) ŵ = 1.27 mm−1
c = 18.042 (2) ÅT = 100 (2) K
β = 104.901 (2)ºCube, green–brown
V = 2340.4 (5) Å30.06 × 0.06 × 0.06 mm
Z = 4
Data collection
Bruker APEXII diffractometer5374 independent reflections
Radiation source: fine-focus sealed tube3915 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.048
T = 100(2) Kθmax = 27.5º
[var phi] and ω scansθmin = 1.7º
Absorption correction: multi-scan(SADABS; Sheldrick, 1996)h = −17→16
Tmin = 0.758, Tmax = 0.928k = −7→13
14384 measured reflectionsl = −23→23
Refinement
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.043H-atom parameters constrained
wR(F2) = 0.104  w = 1/[σ2(Fo2) + (0.0453P)2 + 1.5589P] where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.001
5374 reflectionsΔρmax = 2.60 e Å−3
291 parametersΔρmin = −1.77 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)
xyzUiso*/Ueq
Mo10.53951 (3)0.10457 (4)0.53870 (2)0.01595 (11)
Mo2−0.01435 (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)
O2−0.2474 (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)
H80.6245−0.08820.34710.030*
C90.7354 (4)0.0111 (5)0.3093 (3)0.0261 (11)
H90.7648−0.06530.29260.031*
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*
C15−0.0495 (4)0.7844 (5)0.3857 (3)0.0258 (11)
H15−0.08810.77260.33070.031*
C16−0.0927 (4)0.8291 (5)0.4449 (3)0.0279 (11)
H16−0.16790.85100.43950.033*
C17−0.0100 (4)0.8469 (4)0.5119 (3)0.0302 (12)
H17−0.01720.88270.56190.036*
C180.0835 (4)0.8158 (5)0.4944 (3)0.0276 (11)
H180.15490.82740.52950.033*
C19−0.1602 (4)0.5542 (5)0.4557 (3)0.0279 (11)
C20−0.1100 (3)0.5593 (4)0.6420 (2)0.0178 (9)
C21−0.1885 (3)0.6503 (4)0.6146 (3)0.0225 (10)
H21−0.18270.71130.57590.027*
C22−0.2757 (4)0.6521 (5)0.6437 (3)0.0232 (10)
H22−0.32930.71480.62420.028*
C23−0.2869 (3)0.5659 (5)0.6999 (3)0.0217 (10)
C24−0.2062 (3)0.4753 (4)0.7287 (2)0.0206 (10)
H24−0.21180.41520.76780.025*
C25−0.1182 (3)0.4732 (4)0.7002 (2)0.0199 (9)
H25−0.06330.41260.72060.024*
C26−0.3837 (4)0.5654 (5)0.7300 (3)0.0282 (11)
H26A−0.40870.65610.73180.042*
H26B−0.36660.52760.78180.042*
H26C−0.43830.51240.69610.042*
Atomic displacement parameters (Å2)
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, °)
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—C7−33.3 (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—C12−84.4 (3)
C5—Mo1—S1—C7101.1 (3)Mo1i—S1—C7—C12−155.8 (3)
C1—Mo1—S1—C7115.9 (2)C12—C7—C8—C9−0.8 (7)
S1i—Mo1—S1—C7−111.75 (17)S1—C7—C8—C9174.7 (3)
Mo1i—Mo1—S1—C7−111.75 (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—C13−178.8 (4)
C4—Mo1—S1—Mo1i159.57 (16)C9—C10—C11—C12−1.8 (7)
C2—Mo1—S1—Mo1i−157.81 (13)C13—C10—C11—C12177.4 (4)
C5—Mo1—S1—Mo1i−147.2 (2)C8—C7—C12—C11−0.5 (6)
C1—Mo1—S1—Mo1i−132.37 (13)S1—C7—C12—C11−176.3 (3)
S1i—Mo1—S1—Mo1i0.0C10—C11—C12—C71.9 (7)
C19—Mo2—S2—C20−28.4 (2)C19—Mo2—C14—C1511.2 (4)
C14—Mo2—S2—C20125.5 (2)C18—Mo2—C14—C15−114.5 (4)
C15—Mo2—S2—C2069.6 (3)C16—Mo2—C14—C15−37.4 (3)
C18—Mo2—S2—C20114.6 (2)C17—Mo2—C14—C15−78.4 (3)
C16—Mo2—S2—C2055.3 (2)S2ii—Mo2—C14—C1591.5 (3)
C17—Mo2—S2—C2081.3 (2)S2—Mo2—C14—C15−133.1 (2)
S2ii—Mo2—S2—C20−105.47 (16)Mo2ii—Mo2—C14—C15137.3 (2)
Mo2ii—Mo2—S2—C20−105.47 (16)C19—Mo2—C14—C18125.8 (3)
C19—Mo2—S2—Mo2ii77.08 (14)C15—Mo2—C14—C18114.5 (4)
C14—Mo2—S2—Mo2ii−129.00 (17)C16—Mo2—C14—C1877.1 (3)
C15—Mo2—S2—Mo2ii175.1 (2)C17—Mo2—C14—C1836.1 (3)
C18—Mo2—S2—Mo2ii−139.93 (13)S2ii—Mo2—C14—C18−153.9 (3)
C16—Mo2—S2—Mo2ii160.76 (14)S2—Mo2—C14—C18−18.6 (4)
C17—Mo2—S2—Mo2ii−173.19 (13)Mo2ii—Mo2—C14—C18−108.1 (3)
S2ii—Mo2—S2—Mo2ii0.0C18—C14—C15—C160.2 (5)
C6—Mo1—C1—C5−45.1 (4)Mo2—C14—C15—C1666.2 (3)
C3—Mo1—C1—C5−79.2 (3)C18—C14—C15—Mo2−66.0 (3)
C4—Mo1—C1—C5−36.8 (3)C19—Mo2—C15—C1673.2 (3)
C2—Mo1—C1—C5−117.1 (4)C14—Mo2—C15—C16−115.3 (4)
S1—Mo1—C1—C5−165.6 (2)C18—Mo2—C15—C16−77.0 (3)
S1i—Mo1—C1—C561.1 (3)C17—Mo2—C15—C16−36.7 (3)
Mo1i—Mo1—C1—C5127.6 (2)S2ii—Mo2—C15—C16152.7 (3)
C6—Mo1—C1—C272.0 (4)S2—Mo2—C15—C16−22.9 (4)
C3—Mo1—C1—C237.8 (3)Mo2ii—Mo2—C15—C16147.8 (3)
C4—Mo1—C1—C280.2 (3)C19—Mo2—C15—C14−171.5 (3)
C5—Mo1—C1—C2117.1 (4)C18—Mo2—C15—C1438.3 (3)
S1—Mo1—C1—C2−48.5 (3)C16—Mo2—C15—C14115.3 (4)
S1i—Mo1—C1—C2178.2 (2)C17—Mo2—C15—C1478.6 (3)
Mo1i—Mo1—C1—C2−115.4 (3)S2ii—Mo2—C15—C14−92.0 (3)
C5—C1—C2—C3−0.3 (5)S2—Mo2—C15—C1492.4 (3)
Mo1—C1—C2—C3−63.2 (3)Mo2ii—Mo2—C15—C14−96.9 (4)
C5—C1—C2—Mo163.0 (3)C14—C15—C16—C17−0.6 (5)
C6—Mo1—C2—C1−137.3 (3)Mo2—C15—C16—C1763.6 (3)
C3—Mo1—C2—C1−116.2 (4)C14—C15—C16—Mo2−64.3 (3)
C4—Mo1—C2—C1−77.8 (3)C19—Mo2—C16—C15−106.9 (3)
C5—Mo1—C2—C1−36.5 (3)C14—Mo2—C16—C1538.4 (3)
S1—Mo1—C2—C1136.6 (3)C18—Mo2—C16—C1580.7 (3)
S1i—Mo1—C2—C1−3.1 (4)C17—Mo2—C16—C15117.0 (4)
Mo1i—Mo1—C2—C1106.7 (3)S2ii—Mo2—C16—C15−34.3 (3)
C6—Mo1—C2—C3−21.1 (3)S2—Mo2—C16—C15167.1 (3)
C4—Mo1—C2—C338.4 (3)Mo2ii—Mo2—C16—C15−130.5 (4)
C5—Mo1—C2—C379.7 (3)C19—Mo2—C16—C17136.1 (3)
C1—Mo1—C2—C3116.2 (4)C14—Mo2—C16—C17−78.6 (3)
S1—Mo1—C2—C3−107.2 (3)C15—Mo2—C16—C17−117.0 (4)
S1i—Mo1—C2—C3113.1 (3)C18—Mo2—C16—C17−36.3 (3)
Mo1i—Mo1—C2—C3−137.1 (2)S2ii—Mo2—C16—C17−151.4 (2)
C1—C2—C3—C40.4 (5)S2—Mo2—C16—C1750.1 (3)
Mo1—C2—C3—C4−65.0 (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—C2−114.9 (4)C15—C16—C17—Mo2−62.0 (3)
C5—Mo1—C3—C2−77.6 (3)C19—Mo2—C17—C18−164.4 (3)
C1—Mo1—C3—C2−36.9 (3)C14—Mo2—C17—C18−37.7 (3)
S1—Mo1—C3—C275.1 (3)C15—Mo2—C17—C18−80.3 (3)
S1i—Mo1—C3—C2−124.0 (2)C16—Mo2—C17—C18−117.2 (4)
Mo1i—Mo1—C3—C299.1 (3)S2ii—Mo2—C17—C18−59.8 (4)
C6—Mo1—C3—C4−82.6 (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—C16−47.2 (3)
C1—Mo1—C3—C477.9 (3)C14—Mo2—C17—C1679.5 (3)
S1—Mo1—C3—C4−170.0 (2)C15—Mo2—C17—C1636.9 (3)
S1i—Mo1—C3—C4−9.1 (4)C18—Mo2—C17—C16117.2 (4)
Mo1i—Mo1—C3—C4−146.0 (2)S2ii—Mo2—C17—C1657.4 (4)
C2—C3—C4—C5−0.3 (5)S2—Mo2—C17—C16−136.0 (3)
Mo1—C3—C4—C5−65.8 (3)Mo2ii—Mo2—C17—C16−146.8 (2)
C2—C3—C4—Mo165.5 (3)C16—C17—C18—C14−0.8 (5)
C6—Mo1—C4—C5−148.6 (3)Mo2—C17—C18—C1462.4 (3)
C3—Mo1—C4—C5115.6 (4)C16—C17—C18—Mo2−63.2 (3)
C2—Mo1—C4—C577.4 (3)C15—C14—C18—C170.4 (5)
C1—Mo1—C4—C536.3 (3)Mo2—C14—C18—C17−64.7 (3)
S1—Mo1—C4—C5129.4 (2)C15—C14—C18—Mo265.1 (3)
S1i—Mo1—C4—C5−70.1 (3)C19—Mo2—C18—C1724.4 (4)
Mo1i—Mo1—C4—C5−111.1 (4)C14—Mo2—C18—C17116.9 (4)
C6—Mo1—C4—C395.8 (3)C15—Mo2—C18—C1778.3 (3)
C2—Mo1—C4—C3−38.1 (3)C16—Mo2—C18—C1736.9 (3)
C5—Mo1—C4—C3−115.6 (4)S2ii—Mo2—C18—C17150.1 (2)
C1—Mo1—C4—C3−79.3 (3)S2—Mo2—C18—C17−76.4 (3)
S1—Mo1—C4—C313.8 (3)Mo2ii—Mo2—C18—C17−129.3 (3)
S1i—Mo1—C4—C3174.4 (2)C19—Mo2—C18—C14−92.5 (4)
Mo1i—Mo1—C4—C3133.3 (3)C15—Mo2—C18—C14−38.6 (3)
C2—C1—C5—C40.1 (5)C16—Mo2—C18—C14−80.0 (3)
Mo1—C1—C5—C462.2 (3)C17—Mo2—C18—C14−116.9 (4)
C2—C1—C5—Mo1−62.1 (3)S2ii—Mo2—C18—C1433.2 (3)
C3—C4—C5—C10.2 (5)S2—Mo2—C18—C14166.7 (3)
Mo1—C4—C5—C1−63.9 (3)Mo2ii—Mo2—C18—C14113.8 (3)
C3—C4—C5—Mo164.0 (3)Mo2ii—S2—C20—C21−104.6 (4)
C6—Mo1—C5—C1152.3 (3)Mo2—S2—C20—C21−33.7 (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—C22−2.0 (7)
S1—Mo1—C5—C124.3 (4)S2—C20—C21—C22−176.6 (3)
S1i—Mo1—C5—C1−126.1 (3)C20—C21—C22—C230.3 (7)
Mo1i—Mo1—C5—C1−98.2 (3)C21—C22—C23—C240.9 (7)
C6—Mo1—C5—C435.0 (3)C21—C22—C23—C26−178.2 (4)
C3—Mo1—C5—C4−38.2 (3)C22—C23—C24—C25−0.5 (6)
C2—Mo1—C5—C4−80.5 (3)C26—C23—C24—C25178.6 (4)
C1—Mo1—C5—C4−117.3 (4)C23—C24—C25—C20−1.1 (7)
S1—Mo1—C5—C4−93.0 (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.
 
Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: CI2579).
References
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  • Benson, I. B., Killops, S. D., Know, S. A. R. & Welch, A. J. (1980). J. Chem. Soc. Chem. Commun. pp. 1137–1139.
  • Bruker (2007). APEX2 and SAINT Bruker AXS Inc., Madison, Wisconsin, USA.
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  • Song, L.-C., Wang, J.-Q., Hu, Q.-M., Wang, R.-J. & Mak, T. C. W. (1997). Inorg. Chim. Acta, 256, 129–135.
  • Westrip, S. P. (2008). publCIF In preparation.
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