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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

(μ-4-Methyl­benzene­thiol­ato-κ2 S:S)bis­[carbon­yl(η5-cyclo­penta­dien­yl)molybdenum(II)]

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]).

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Object name is e-64-0m695-scheme1.jpg

Experimental

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
Selected bond lengths (Å)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808010751/ci2579sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808010751/ci2579Isup2.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.
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 ...

Crystal data

[Mo2(C5H5)2(C7H7S)2(CO)2]F000 = 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 = 2.3–24.8º
b = 10.135 (1) ŵ = 1.27 mm1
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 Å3
291 parametersΔρmin = −1.77 e Å3
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.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: CI2579).

References

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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.
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