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Acta Crystallogr Sect E Struct Rep Online. 2009 September 1; 65(Pt 9): m1063–m1064.
Published online 2009 August 12. doi:  10.1107/S1600536809031092
PMCID: PMC2970104

Octa­kis[2,2′,5,5′-tetra­thia­fulvalenium(0.5+)] bis­[hexa­molybdate(2−)] acetonitrile solvate

Abstract

The asymmetric unit of the title compound, (C6H4S4)8[Mo6O19]2·CH3CN, contains two halves of two centrosymmetric [Mo6O19]2− hexa­molybdate anions, which are each built up from six distorted MoO6 octa­hedra sharing common edges and one common vertex at the central O atom, six tetra­thia­fulvalene cations (three of which are located on mirror planes) to balance the charge and a half of an acetonitrile solvent mol­ecule, likewise located on a mirror plane. The two central hexa­molybdate O atoms occupy special positions 2a and 2d, respectively. The cations and anions are inter­linked through C—H(...)O contacts.

Related literature

For the chemical and physical properties of polyoxo­molybdates, see: Shi et al. (2006 [triangle]); Wang et al. (2004 [triangle]); Hagrman et al. (1999 [triangle]). For the structure of ammonium tris­(tetra­ethyl­ammonium) hexa­cosa­oxidoocta­molybdate, see: Zebiri et al. (2008 [triangle]). The title compound is isostructural with its tungsten analogue, see: Triki et al. (1993 [triangle]). The structure of the anions is the same as that in bis­[2-(pyrimidin-2-yl­amino)pyrimidinium] hexa­molybdate, see: Yeh et al. (2008 [triangle]). For Mo—O distances, see: Boyle et al. (1998 [triangle]); Deng et al. (2006 [triangle]); Maeda et al. (2006 [triangle]).

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Object name is e-65-m1063-scheme1.jpg

Experimental

Crystal data

  • (C6H4S4)8[Mo6O19]2·C2H3N
  • M r = 3434.99
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-65-m1063-efi1.jpg
  • a = 14.3179 (8) Å
  • b = 20.2299 (10) Å
  • c = 16.7625 (10) Å
  • β = 101.266 (3)°
  • V = 4761.7 (5) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 2.31 mm−1
  • T = 100 K
  • 0.25 × 0.15 × 0.10 mm

Data collection

  • Nonius KappaCCD diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996 [triangle]) T min = 0.597, T max = 0.802
  • 45527 measured reflections
  • 11170 independent reflections
  • 8144 reflections with I > 2σ(I)
  • R int = 0.072

Refinement

  • R[F 2 > 2σ(F 2)] = 0.036
  • wR(F 2) = 0.073
  • S = 1
  • 11170 reflections
  • 629 parameters
  • H-atom parameters constrained
  • Δρmax = 0.88 e Å−3
  • Δρmin = −0.70 e Å−3

Data collection: COLLECT (Nonius, 2002 [triangle]); cell refinement: DENZO and SCALEPACK (Otwinowski & Minor, 1997 [triangle]); data reduction: DENZO and SCALEPACK; program(s) used to solve structure: SIR92 (Altomare et al., 1993 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: ORTEP-3 (Farrugia, 1997 [triangle]) and Mercury (Macrae et al., 2006 [triangle]); software used to prepare material for publication: WinGX (Farrugia, 1999 [triangle]) and PARST (Nardelli, 1995 [triangle]).

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809031092/hg2545sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809031092/hg2545Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

This work was supported by Laboratoire de Chimie des Matériaux Faculté des Sciences, Université Mentouri. We would like to thank J.-Y. Saillard and Thierry Roisnel from Rennes 1 University for providing diffraction facilities.

supplementary crystallographic information

Comment

As part of an ongoing study of materials containing polyoxomolybdates, we have just recently determined the structure of ammonium tris(tetraethylammonium) hexacosaoxidooctamolybdate (Zebiri et al., 2008). These materials show interesting chemical and physical properties (Shi et al., 2006; Wang, et al., 2004; Hagrman, et al., 1999).

The asymmetric unit of the title compound consists of a half neutral acetonitrile; two hexamolybdate anions and six tetrathiafulvalene in witch two ones are (+1) charged and the rest ones with +0.5 charge (Fig. 1). The title compound is isostructural to (TTF)4W6O19.0.5(CH3CN) reported by Triki et al. (1993). The structure of the anions, as reported recently in Bis[2-(pyrimidin-2-ylamino)pyrimidinium] hexamolybdate (Yeh et al., 2008), is constructed from an array of six edge-shared MoO6 octahedra with six O(t), ten O(µ2) and one O(µ6) atoms.

The Mo—O distances, ranging from 1.681 (3) to 2.3363 (4) Å, agree with those reported for other [Mo6O19]2- anions in the literature (Deng et al., 2006; Maeda et al., 2006; Boyle et al., 1998) and can be grouped into three sets bridging groups [Mo—O(terminal) 1.681 (3) -1.696 (3) Å, Mo—O(µ2): 1.850 (3) -2.027 (3) (1) Å and Mo—O(µ6): 2.3151 (4) (1)- 2.3363 (4) (1) Å.

Hexamolybdate anions spread along the b axis (Fig. 2) between which organic moieties intercalate. The cations and anions are interlinked through C—H···O contacts.

Experimental

Single crystals of the title compound were prepared from a mixture of (NH4)6Mo7O24. 1.5 H2O (137 mg, 1 mmol), C6S4H4 (TTF) (612 mg, 3 mmol) and 3 ml H2O, heated in a Teflon-lined steel autoclave inside a programmable electric furnace at 160 ° C for 3 days. After cooling the autoclave to room temperature for 72 h, colorless crystals were obtained, filtered, washed with H2O, EtOH, Et2O and dried in air.

Refinement

H atoms were positioned geometrically and treated as riding, with C—H = 0.93 Å with Uiso(H) = 1.2Ueq(C). The methyl H atoms were constrained to an ideal geometry (C—H = 0.96 Å) with Uiso(H) = 1.2Ueq(C), but were allowed to rotate freely about the C—C bonds.

Figures

Fig. 1.
The independent components of (I), showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 50% probability level.
Fig. 2.
hexamolybdate anions positions on the unit cell.

Crystal data

(C6H4S4)8[Mo6O19]2·C2H3NF(000) = 3324
Mr = 3434.99Dx = 2.396 Mg m3
Monoclinic, P21/mMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybCell parameters from 2190 reflections
a = 14.3179 (8) Åθ = 2.8–27.3°
b = 20.2299 (10) ŵ = 2.31 mm1
c = 16.7625 (10) ÅT = 100 K
β = 101.266 (3)°Plates, colourless
V = 4761.7 (5) Å30.25 × 0.15 × 0.1 mm
Z = 2

Data collection

Nonius KappaCCD diffractometer11170 independent reflections
Radiation source: fine-focus sealed X-ray tube8144 reflections with I > 2σ(I)
graphiteRint = 0.072
[var phi] scans, and ω scans with κ offsetsθmax = 27.5°, θmin = 1.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −18→18
Tmin = 0.597, Tmax = 0.802k = −26→26
45527 measured reflectionsl = −21→21

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.036H-atom parameters constrained
wR(F2) = 0.073w = 1/[σ2(Fo2) + (0.021P)2] where P = (Fo2 + 2Fc2)/3
S = 1(Δ/σ)max = 0.003
11170 reflectionsΔρmax = 0.88 e Å3
629 parametersΔρmin = −0.70 e Å3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.08 (2)

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/UeqOcc. (<1)
Mo10.56723 (3)0.411518 (19)0.58067 (2)0.01535 (9)
Mo20.37343 (3)0.500847 (18)0.56738 (2)0.01262 (8)
Mo50.41862 (3)0.425991 (19)0.40423 (2)0.01562 (9)
Mo30.09471 (3)0.007942 (18)0.90255 (2)0.01440 (9)
Mo40.12057 (3)0.050345 (18)1.09450 (2)0.01550 (9)
Mo6−0.06607 (3)0.102673 (18)0.96110 (2)0.01461 (9)
S40.69926 (8)0.32365 (5)0.32774 (7)0.0171 (2)
S10.83864 (9)0.32314 (6)0.19478 (7)0.0194 (3)
S20.31973 (9)0.32349 (5)0.68472 (7)0.0193 (3)
S31.13888 (8)0.41650 (5)0.47871 (7)0.0141 (2)
S50.85700 (8)0.41673 (5)0.53863 (7)0.0134 (2)
S60.94719 (8)0.41562 (5)0.37833 (7)0.0148 (2)
S71.04691 (8)0.41757 (5)0.64209 (7)0.0158 (2)
S80.19893 (11)0.750.39380 (10)0.0162 (3)
S90.38303 (8)0.16665 (6)0.03769 (7)0.0186 (3)
S10−0.09582 (11)0.750.43604 (10)0.0167 (3)
S110.01173 (12)0.750.27956 (10)0.0187 (4)
S120.09410 (11)0.750.54638 (9)0.0157 (3)
S130.57537 (8)0.16549 (5)0.13620 (7)0.0169 (2)
S140.47171 (8)0.16799 (6)−0.12637 (7)0.0174 (2)
S150.66417 (8)0.16465 (6)−0.02771 (7)0.0204 (3)
S180.21028 (8)0.32348 (5)0.83822 (7)0.0177 (2)
O10010.0106 (9)
O20.50.50.50.0119 (9)
O50.4513 (2)0.43340 (14)0.62260 (17)0.0153 (7)
O40.2801 (2)0.50318 (14)0.61450 (18)0.0159 (7)
O30.6587 (2)0.43007 (14)0.51664 (18)0.0169 (7)
O60.4587 (2)0.56620 (14)0.62598 (17)0.0150 (7)
O120.4888 (2)0.36829 (14)0.49387 (18)0.0161 (7)
O70.6179 (2)0.49293 (14)0.64424 (17)0.0166 (7)
O8−0.0228 (2)−0.03840 (14)0.84668 (18)0.0195 (7)
O90.3326 (2)0.44003 (14)0.47865 (18)0.0159 (7)
O100.0391 (2)0.12578 (13)1.03983 (18)0.0166 (7)
O110.0124 (2)0.08657 (13)0.88356 (18)0.0178 (7)
O130.1560 (2)−0.03770 (14)1.10491 (19)0.0204 (7)
O140.1549 (2)0.01313 (14)0.82549 (19)0.0215 (7)
O150.1685 (2)0.05279 (13)0.99087 (18)0.0158 (7)
O160.3610 (2)0.36980 (15)0.33835 (19)0.0234 (8)
O19−0.1227 (2)0.17476 (14)0.93106 (19)0.0221 (7)
O180.2048 (2)0.09129 (14)1.1612 (2)0.0245 (8)
O170.6166 (2)0.35055 (15)0.64365 (19)0.0245 (8)
O200.1308 (2)−0.07465 (14)0.95163 (19)0.0200 (7)
C10.7991 (4)0.250.2352 (4)0.0127 (13)
C40.9789 (3)0.4167 (2)0.5449 (3)0.0145 (9)
C30.1983 (5)0.750.2897 (4)0.0204 (15)
H30.25480.750.27030.025*
C20.7423 (4)0.250.2902 (4)0.0143 (13)
C70.1143 (5)0.750.2388 (4)0.0224 (15)
H70.11070.750.18280.027*
C80.0738 (5)0.750.3820 (4)0.0170 (14)
C60.8635 (3)0.4170 (2)0.6423 (3)0.0166 (10)
H60.80880.41690.66430.02*
C50.9505 (3)0.4174 (2)0.6901 (3)0.0178 (10)
H50.95850.41760.74650.021*
C110.2420 (4)0.250.7930 (4)0.0149 (13)
C100.2854 (4)0.250.7292 (4)0.0160 (14)
C150.5424 (3)0.1666 (2)−0.0301 (3)0.0174 (10)
C160.5044 (3)0.1662 (2)0.0406 (3)0.0172 (10)
C130.5655 (3)0.1660 (2)−0.1775 (3)0.0216 (11)
H130.55530.166−0.2340.026*
C120.1572 (3)0.2831 (2)0.9098 (3)0.0223 (11)
H120.12970.30680.94680.027*
C140.6539 (3)0.1643 (2)−0.1321 (3)0.0210 (11)
H140.70740.163−0.15590.025*
C90.3514 (3)0.2832 (2)0.6016 (3)0.0231 (11)
H90.36760.3070.55880.028*
C221.0177 (3)0.41639 (19)0.4749 (3)0.0132 (9)
C170.4818 (3)0.1637 (2)0.1873 (3)0.0180 (10)
H170.49230.16230.24380.022*
C180.3931 (3)0.1643 (2)0.1421 (3)0.0185 (10)
H180.33960.16350.16590.022*
C210.0295 (4)0.750.4457 (4)0.0165 (14)
C200.6422 (3)0.2833 (2)0.3968 (3)0.0211 (11)
H200.61270.3070.43250.025*
C190.9255 (3)0.2830 (2)0.1533 (3)0.0235 (11)
H190.97040.30670.13190.028*
C241.0417 (3)0.4110 (2)0.3287 (3)0.0197 (10)
H241.03220.40840.27230.024*
C231.1297 (3)0.4114 (2)0.3748 (3)0.0174 (10)
H231.18360.40890.35160.021*
C26−0.0077 (4)0.750.5908 (4)0.0184 (14)
H26−0.00270.750.64690.022*
C25−0.0915 (5)0.750.5408 (4)0.0186 (14)
H25−0.14740.750.56130.022*
S160.43075 (9)0.99818 (6)0.10594 (7)0.0200 (3)
S270.63331 (9)0.99422 (6)0.09037 (7)0.0203 (3)
C270.5135 (3)0.9988 (2)0.0403 (3)0.0166 (10)
C290.5178 (4)0.9954 (2)0.1949 (3)0.0245 (11)
H290.50080.99540.24570.029*
C280.6083 (4)0.9931 (2)0.1884 (3)0.0247 (11)
H280.65680.9910.23420.03*
N10.1799 (6)0.250.1110 (5)0.061 (2)
C300.1822 (6)0.250.1791 (7)0.049 (3)
C310.1876 (6)0.250.2689 (6)0.050 (2)
H31A0.13530.27490.28150.076*0.5
H31B0.24660.26970.29530.076*0.5
H31C0.18450.20540.28760.076*0.5

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Mo10.0150 (2)0.0195 (2)0.0125 (2)0.00474 (16)0.00522 (16)0.00528 (16)
Mo20.01036 (18)0.0189 (2)0.00921 (18)0.00057 (16)0.00335 (15)0.00047 (15)
Mo50.0138 (2)0.0217 (2)0.01209 (19)−0.00355 (16)0.00420 (16)−0.00492 (16)
Mo30.0168 (2)0.0162 (2)0.01122 (19)−0.00087 (16)0.00517 (16)0.00087 (15)
Mo40.0164 (2)0.0170 (2)0.01202 (19)−0.00345 (16)0.00029 (16)−0.00233 (15)
Mo60.0185 (2)0.0131 (2)0.01240 (19)0.00125 (16)0.00348 (16)0.00127 (15)
S40.0199 (6)0.0162 (6)0.0154 (6)0.0025 (5)0.0038 (5)−0.0010 (5)
S10.0213 (6)0.0191 (6)0.0189 (6)−0.0011 (5)0.0062 (5)0.0029 (5)
S20.0241 (7)0.0177 (6)0.0166 (6)−0.0050 (5)0.0055 (5)0.0010 (5)
S30.0110 (5)0.0164 (6)0.0148 (6)−0.0019 (4)0.0023 (5)−0.0003 (4)
S50.0114 (5)0.0163 (6)0.0122 (5)0.0001 (4)0.0018 (4)0.0009 (4)
S60.0148 (6)0.0171 (6)0.0117 (5)−0.0021 (4)0.0006 (5)0.0014 (4)
S70.0152 (6)0.0186 (6)0.0121 (5)−0.0005 (5)−0.0008 (5)0.0000 (4)
S80.0155 (8)0.0175 (8)0.0151 (8)00.0017 (7)0
S90.0149 (6)0.0223 (6)0.0184 (6)−0.0005 (5)0.0028 (5)−0.0022 (5)
S100.0151 (8)0.0176 (8)0.0161 (8)0−0.0006 (7)0
S110.0227 (9)0.0184 (8)0.0124 (8)0−0.0027 (7)0
S120.0155 (8)0.0173 (8)0.0126 (8)0−0.0016 (7)0
S130.0163 (6)0.0215 (6)0.0127 (6)0.0001 (5)0.0021 (5)−0.0004 (5)
S140.0188 (6)0.0213 (6)0.0118 (6)0.0011 (5)0.0019 (5)−0.0001 (5)
S150.0158 (6)0.0278 (7)0.0182 (6)0.0030 (5)0.0046 (5)0.0017 (5)
S180.0210 (6)0.0147 (6)0.0177 (6)−0.0002 (5)0.0046 (5)−0.0021 (5)
O10.013 (2)0.012 (2)0.007 (2)−0.0012 (17)0.0024 (17)−0.0010 (16)
O20.010 (2)0.016 (2)0.011 (2)0.0002 (17)0.0043 (18)0.0001 (17)
O50.0175 (17)0.0193 (16)0.0103 (15)0.0010 (13)0.0054 (13)0.0021 (12)
O40.0135 (16)0.0218 (17)0.0133 (16)−0.0001 (13)0.0047 (13)−0.0004 (13)
O30.0134 (16)0.0221 (16)0.0164 (17)0.0041 (13)0.0052 (14)0.0028 (13)
O60.0153 (16)0.0199 (16)0.0109 (15)−0.0017 (13)0.0053 (13)−0.0024 (13)
O120.0207 (17)0.0149 (16)0.0149 (16)−0.0004 (13)0.0091 (14)−0.0004 (12)
O70.0131 (16)0.0259 (17)0.0102 (16)0.0016 (13)0.0012 (13)0.0014 (13)
O80.0240 (18)0.0230 (17)0.0114 (16)−0.0007 (14)0.0032 (14)−0.0036 (13)
O90.0137 (16)0.0207 (17)0.0149 (16)−0.0036 (13)0.0068 (13)−0.0031 (13)
O100.0193 (17)0.0122 (15)0.0188 (17)−0.0036 (13)0.0049 (14)−0.0019 (13)
O110.0200 (17)0.0164 (16)0.0168 (17)−0.0021 (13)0.0026 (14)0.0020 (13)
O130.0192 (17)0.0219 (17)0.0173 (17)−0.0010 (14)−0.0034 (14)0.0015 (14)
O140.0254 (19)0.0192 (17)0.0229 (19)−0.0013 (14)0.0120 (16)0.0011 (14)
O150.0126 (16)0.0171 (16)0.0183 (17)−0.0035 (13)0.0040 (13)−0.0032 (13)
O160.0220 (18)0.0321 (19)0.0167 (18)−0.0051 (15)0.0054 (15)−0.0125 (14)
O190.0264 (19)0.0181 (17)0.0227 (18)0.0025 (14)0.0066 (16)0.0043 (14)
O180.0244 (18)0.0251 (18)0.0215 (18)−0.0084 (14)−0.0017 (15)−0.0043 (14)
O170.028 (2)0.0275 (18)0.0197 (19)0.0115 (15)0.0097 (16)0.0075 (14)
O200.0219 (18)0.0160 (16)0.0245 (19)−0.0015 (13)0.0102 (15)−0.0005 (14)
C10.015 (3)0.013 (3)0.011 (3)00.006 (3)0
C40.011 (2)0.012 (2)0.019 (2)0.0005 (17)−0.0005 (19)0.0019 (18)
C30.022 (4)0.028 (4)0.012 (3)00.006 (3)0
C20.018 (3)0.014 (3)0.009 (3)0−0.002 (3)0
C70.036 (4)0.021 (4)0.012 (3)00.010 (3)0
C80.026 (4)0.019 (3)0.005 (3)0−0.001 (3)0
C60.016 (2)0.017 (2)0.018 (2)0.0003 (18)0.006 (2)0.0009 (19)
C50.026 (3)0.017 (2)0.011 (2)−0.002 (2)0.005 (2)−0.0006 (18)
C110.014 (3)0.015 (3)0.014 (3)0−0.003 (3)0
C100.016 (3)0.015 (3)0.015 (3)00.000 (3)0
C150.016 (2)0.021 (2)0.014 (2)0.0026 (19)0.001 (2)−0.0020 (19)
C160.019 (2)0.018 (2)0.015 (2)−0.0004 (19)0.004 (2)−0.0005 (19)
C130.032 (3)0.021 (3)0.014 (2)0.005 (2)0.010 (2)0.0023 (19)
C120.019 (3)0.028 (3)0.021 (3)0.005 (2)0.009 (2)−0.001 (2)
C140.020 (3)0.028 (3)0.017 (3)0.006 (2)0.010 (2)0.001 (2)
C90.024 (3)0.031 (3)0.016 (3)−0.003 (2)0.008 (2)0.002 (2)
C220.014 (2)0.007 (2)0.016 (2)−0.0029 (17)−0.0017 (19)−0.0001 (17)
C170.023 (3)0.019 (2)0.013 (2)0.001 (2)0.007 (2)−0.0021 (19)
C180.021 (3)0.016 (2)0.022 (3)−0.0033 (19)0.011 (2)−0.0040 (19)
C210.014 (3)0.018 (3)0.013 (3)0−0.006 (3)0
C200.024 (3)0.030 (3)0.010 (2)0.006 (2)0.007 (2)−0.0007 (19)
C190.023 (3)0.034 (3)0.017 (3)−0.003 (2)0.011 (2)0.001 (2)
C240.025 (3)0.022 (3)0.011 (2)−0.005 (2)0.002 (2)0.0009 (19)
C230.021 (2)0.020 (2)0.012 (2)−0.0021 (19)0.005 (2)0.0018 (18)
C260.021 (4)0.015 (3)0.020 (4)00.005 (3)0
C250.027 (4)0.013 (3)0.017 (3)00.006 (3)0
S160.0263 (7)0.0219 (6)0.0124 (6)0.0039 (5)0.0053 (5)−0.0005 (5)
S270.0219 (6)0.0245 (6)0.0127 (6)0.0035 (5)−0.0012 (5)−0.0004 (5)
C270.021 (2)0.015 (2)0.013 (2)0.0028 (19)0.003 (2)−0.0002 (18)
C290.039 (3)0.022 (3)0.010 (2)0.002 (2)−0.001 (2)−0.0004 (19)
C280.035 (3)0.022 (3)0.012 (2)0.005 (2)−0.007 (2)−0.0015 (19)
N10.071 (6)0.060 (5)0.050 (5)00.002 (5)0
C300.038 (5)0.026 (5)0.084 (8)00.014 (6)0
C310.051 (6)0.033 (5)0.071 (7)00.021 (5)0

Geometric parameters (Å, °)

Mo1—O171.686 (3)S15—C141.727 (5)
Mo1—O121.872 (3)S15—C151.736 (5)
Mo1—O31.886 (3)S18—C121.743 (5)
Mo1—O51.974 (3)S18—C111.768 (4)
Mo1—O72.018 (3)O1—Mo6ii2.3222 (4)
Mo1—O22.3345 (4)O1—Mo3ii2.3234 (4)
Mo2—O41.680 (3)O1—Mo4ii2.3363 (4)
Mo2—O51.887 (3)O2—Mo2i2.3151 (4)
Mo2—O91.931 (3)O2—Mo5i2.3335 (4)
Mo2—O61.932 (3)O2—Mo1i2.3345 (4)
Mo2—O3i1.974 (3)O3—Mo2i1.974 (3)
Mo2—O22.3151 (4)O6—Mo5i1.928 (3)
Mo5—O161.684 (3)O7—Mo5i1.860 (3)
Mo5—O7i1.860 (3)O8—Mo4ii1.879 (3)
Mo5—O6i1.928 (3)O13—Mo6ii2.013 (3)
Mo5—O91.937 (3)O20—Mo6ii1.962 (3)
Mo5—O122.010 (3)C1—C21.343 (8)
Mo5—O22.3335 (4)C1—S1iii1.766 (3)
Mo3—O141.690 (3)C4—C221.393 (6)
Mo3—O151.876 (3)C3—C71.331 (9)
Mo3—O201.889 (3)C3—H30.93
Mo3—O111.968 (3)C2—S4iii1.774 (4)
Mo3—O81.993 (3)C7—H70.93
Mo3—O12.3234 (4)C8—C211.345 (9)
Mo4—O181.692 (3)C6—C51.343 (6)
Mo4—O131.851 (3)C6—H60.93
Mo4—O8ii1.879 (3)C5—H50.93
Mo4—O151.989 (3)C11—C101.339 (9)
Mo4—O102.028 (3)C11—S18iii1.768 (4)
Mo4—O12.3363 (4)C10—S2iii1.774 (4)
Mo6—O191.696 (3)C15—C161.398 (6)
Mo6—O101.858 (3)C13—C141.343 (6)
Mo6—O111.905 (3)C13—H130.93
Mo6—O20ii1.962 (3)C12—C12iii1.340 (9)
Mo6—O13ii2.013 (3)C12—H120.93
Mo6—O12.3222 (4)C14—H140.93
S4—C201.746 (5)C9—C9iii1.343 (9)
S4—C21.774 (4)C9—H90.93
S1—C191.739 (5)C17—C181.347 (6)
S1—C11.766 (3)C17—H170.93
S2—C91.749 (5)C18—H180.93
S2—C101.774 (4)C20—C20iii1.347 (9)
S3—C231.723 (4)C20—H200.93
S3—C221.724 (4)C19—C19iii1.335 (9)
S5—C61.721 (5)C19—H190.93
S5—C41.727 (4)C24—C231.344 (6)
S6—C241.724 (5)C24—H240.93
S6—C221.732 (4)C23—H230.93
S7—C41.728 (4)C26—C251.323 (9)
S7—C51.728 (5)C26—H260.93
S8—C31.743 (6)C25—H250.93
S8—C81.764 (7)S16—C291.748 (5)
S9—C181.728 (5)S16—C271.767 (5)
S9—C161.728 (5)S27—C281.749 (5)
S10—C251.746 (6)S27—C271.759 (5)
S10—C211.769 (6)C27—C27iv1.330 (8)
S11—C71.737 (7)C29—C281.322 (7)
S11—C81.772 (6)C29—H290.93
S12—C211.759 (6)C28—H280.93
S12—C261.761 (7)N1—C301.136 (12)
S13—C161.722 (5)C30—C311.492 (13)
S13—C171.725 (5)C31—H31A0.96
S14—C151.729 (4)C31—H31B0.96
S14—C131.729 (5)C31—H31C0.96
O17—Mo1—O12105.04 (14)Mo2—O2—Mo5i89.589 (13)
O17—Mo1—O3104.43 (14)Mo2i—O2—Mo5i90.411 (14)
O12—Mo1—O391.61 (13)Mo2—O2—Mo590.411 (14)
O17—Mo1—O5102.70 (14)Mo2i—O2—Mo589.589 (13)
O12—Mo1—O587.90 (12)Mo5i—O2—Mo5180.000 (15)
O3—Mo1—O5152.02 (12)Mo2—O2—Mo189.800 (13)
O17—Mo1—O7101.69 (14)Mo2i—O2—Mo190.200 (13)
O12—Mo1—O7152.99 (12)Mo5i—O2—Mo189.969 (14)
O3—Mo1—O785.42 (12)Mo5—O2—Mo190.031 (14)
O5—Mo1—O782.51 (12)Mo2—O2—Mo1i90.200 (13)
O17—Mo1—O2176.68 (11)Mo2i—O2—Mo1i89.800 (13)
O12—Mo1—O277.94 (9)Mo5i—O2—Mo1i90.031 (14)
O3—Mo1—O276.77 (9)Mo5—O2—Mo1i89.969 (14)
O5—Mo1—O275.78 (8)Mo1—O2—Mo1i180
O7—Mo1—O275.24 (8)Mo2—O5—Mo1116.42 (14)
O4—Mo2—O5103.76 (13)Mo1—O3—Mo2i117.16 (14)
O4—Mo2—O9103.37 (13)Mo5i—O6—Mo2116.11 (14)
O5—Mo2—O988.74 (12)Mo1—O12—Mo5116.50 (14)
O4—Mo2—O6102.89 (13)Mo5i—O7—Mo1116.59 (14)
O5—Mo2—O689.50 (12)Mo4ii—O8—Mo3117.46 (15)
O9—Mo2—O6153.33 (12)Mo2—O9—Mo5117.05 (14)
O4—Mo2—O3i102.71 (13)Mo6—O10—Mo4116.53 (14)
O5—Mo2—O3i153.52 (12)Mo6—O11—Mo3116.24 (15)
O9—Mo2—O3i84.73 (12)Mo4—O13—Mo6ii116.26 (15)
O6—Mo2—O3i85.07 (12)Mo3—O15—Mo4116.10 (14)
O4—Mo2—O2178.36 (10)Mo3—O20—Mo6ii116.81 (15)
O5—Mo2—O277.87 (9)C2—C1—S1123.08 (17)
O9—Mo2—O276.54 (9)C2—C1—S1iii123.08 (17)
O6—Mo2—O277.07 (9)S1—C1—S1iii113.8 (3)
O3i—Mo2—O275.66 (8)C22—C4—S5120.9 (3)
O16—Mo5—O7i104.41 (14)C22—C4—S7123.4 (3)
O16—Mo5—O6i103.77 (14)S5—C4—S7115.7 (3)
O7i—Mo5—O6i90.34 (12)C7—C3—S8118.0 (5)
O16—Mo5—O9103.27 (14)C7—C3—H3121
O7i—Mo5—O989.55 (12)S8—C3—H3121
O6i—Mo5—O9152.09 (12)C1—C2—S4iii122.83 (18)
O16—Mo5—O12101.98 (14)C1—C2—S4122.83 (18)
O7i—Mo5—O12153.60 (12)S4iii—C2—S4114.3 (4)
O6i—Mo5—O1284.01 (12)C3—C7—S11118.3 (5)
O9—Mo5—O1283.78 (12)C3—C7—H7120.8
O16—Mo5—O2177.36 (11)S11—C7—H7120.8
O7i—Mo5—O278.16 (9)C21—C8—S8122.5 (5)
O6i—Mo5—O276.70 (8)C21—C8—S11123.0 (5)
O9—Mo5—O275.98 (8)S8—C8—S11114.5 (4)
O12—Mo5—O275.45 (8)C5—C6—S5117.6 (4)
O14—Mo3—O15106.28 (14)C5—C6—H6121.2
O14—Mo3—O20104.51 (14)S5—C6—H6121.2
O15—Mo3—O2091.14 (13)C6—C5—S7117.0 (4)
O14—Mo3—O11101.82 (14)C6—C5—H5121.5
O15—Mo3—O1187.94 (12)S7—C5—H5121.5
O20—Mo3—O11152.81 (13)C10—C11—S18iii122.77 (18)
O14—Mo3—O8100.35 (14)C10—C11—S18122.77 (18)
O15—Mo3—O8153.12 (13)S18iii—C11—S18114.5 (4)
O20—Mo3—O885.58 (13)C11—C10—S2123.05 (18)
O11—Mo3—O883.12 (12)C11—C10—S2iii123.05 (18)
O14—Mo3—O1175.05 (11)S2—C10—S2iii113.8 (4)
O15—Mo3—O178.15 (9)C16—C15—S14122.5 (3)
O20—Mo3—O177.32 (9)C16—C15—S15122.4 (3)
O11—Mo3—O175.90 (9)S14—C15—S15115.1 (3)
O8—Mo3—O175.10 (9)C15—C16—S13122.1 (4)
O18—Mo4—O13105.18 (14)C15—C16—S9122.2 (4)
O18—Mo4—O8ii102.97 (15)S13—C16—S9115.7 (3)
O13—Mo4—O8ii92.59 (13)C14—C13—S14117.2 (4)
O18—Mo4—O15103.98 (14)C14—C13—H13121.4
O13—Mo4—O1588.36 (13)S14—C13—H13121.4
O8ii—Mo4—O15151.77 (12)C12iii—C12—S18117.92 (15)
O18—Mo4—O10101.72 (13)C12iii—C12—H12121
O13—Mo4—O10152.84 (12)S18—C12—H12121
O8ii—Mo4—O1084.97 (12)C13—C14—S15117.2 (4)
O15—Mo4—O1081.52 (12)C13—C14—H14121.4
O18—Mo4—O1176.53 (11)S15—C14—H14121.4
O13—Mo4—O178.29 (9)C9iii—C9—S2117.77 (15)
O8ii—Mo4—O176.83 (9)C9iii—C9—H9121.1
O15—Mo4—O175.75 (8)S2—C9—H9121.1
O10—Mo4—O174.81 (8)C4—C22—S3122.2 (3)
O19—Mo6—O10105.57 (14)C4—C22—S6122.1 (3)
O19—Mo6—O11104.81 (14)S3—C22—S6115.7 (3)
O10—Mo6—O1191.35 (13)C18—C17—S13117.3 (4)
O19—Mo6—O20ii101.65 (14)C18—C17—H17121.3
O10—Mo6—O20ii88.78 (13)S13—C17—H17121.3
O11—Mo6—O20ii152.48 (12)C17—C18—S9117.0 (4)
O19—Mo6—O13ii100.43 (14)C17—C18—H18121.5
O10—Mo6—O13ii153.81 (12)S9—C18—H18121.5
O11—Mo6—O13ii84.97 (13)C8—C21—S12121.4 (5)
O20ii—Mo6—O13ii82.91 (13)C8—C21—S10123.7 (5)
O19—Mo6—O1175.58 (11)S12—C21—S10115.0 (4)
O10—Mo6—O178.25 (9)C20iii—C20—S4117.88 (15)
O11—Mo6—O177.08 (8)C20iii—C20—H20121.1
O20ii—Mo6—O176.01 (9)S4—C20—H20121.1
O13ii—Mo6—O175.65 (8)C19iii—C19—S1117.84 (15)
C20—S4—C294.7 (2)C19iii—C19—H19121.1
C19—S1—C194.0 (2)S1—C19—H19121.1
C9—S2—C1094.6 (2)C23—C24—S6117.3 (4)
C23—S3—C2294.9 (2)C23—C24—H24121.4
C6—S5—C494.8 (2)S6—C24—H24121.4
C24—S6—C2294.7 (2)C24—C23—S3117.4 (4)
C4—S7—C594.9 (2)C24—C23—H23121.3
C3—S8—C894.6 (3)S3—C23—H23121.3
C18—S9—C1695.0 (2)C25—C26—S12117.1 (5)
C25—S10—C2194.1 (3)C25—C26—H26121.4
C7—S11—C894.5 (3)S12—C26—H26121.4
C21—S12—C2694.7 (3)C26—C25—S10119.1 (5)
C16—S13—C1795.0 (2)C26—C25—H25120.4
C15—S14—C1395.3 (2)S10—C25—H25120.4
C14—S15—C1595.2 (2)C29—S16—C2794.5 (2)
C12—S18—C1194.8 (2)C28—S27—C2795.1 (2)
Mo6—O1—Mo6ii180.000 (19)C27iv—C27—S27123.3 (5)
Mo6—O1—Mo3ii89.861 (13)C27iv—C27—S16122.4 (5)
Mo6ii—O1—Mo3ii90.139 (13)S27—C27—S16114.3 (2)
Mo6—O1—Mo390.139 (13)C28—C29—S16118.5 (4)
Mo6ii—O1—Mo389.861 (13)C28—C29—H29120.8
Mo3ii—O1—Mo3180.0000 (10)S16—C29—H29120.8
Mo6—O1—Mo490.402 (14)C29—C28—S27117.5 (4)
Mo6ii—O1—Mo489.598 (13)C29—C28—H28121.3
Mo3ii—O1—Mo490.504 (14)S27—C28—H28121.3
Mo3—O1—Mo489.496 (14)N1—C30—C31178.7 (11)
Mo6—O1—Mo4ii89.598 (13)C30—C31—H31A109.5
Mo6ii—O1—Mo4ii90.402 (14)C30—C31—H31B109.5
Mo3ii—O1—Mo4ii89.496 (14)H31A—C31—H31B109.5
Mo3—O1—Mo4ii90.504 (14)C30—C31—H31C109.5
Mo4—O1—Mo4ii180.0000 (10)H31A—C31—H31C109.5
Mo2—O2—Mo2i180H31B—C31—H31C109.5

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x, −y, −z+2; (iii) x, −y+1/2, z; (iv) −x+1, −y+2, −z.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
C5—H5···O11v0.932.283.192 (6)167
C7—H7···O19vi0.932.473.251 (7)141
C7—H7···O19vii0.932.473.251 (7)141
C9—H9···O120.932.543.388 (5)151
C13—H13···O17viii0.932.413.239 (6)149
C14—H14···O19ix0.932.593.175 (5)121
C18—H18···O18x0.932.413.145 (5)136
C19—H19···O10xi0.932.413.298 (5)160
C20—H20···O120.932.543.437 (5)162
C24—H24···O8xii0.932.253.075 (6)148
C28—H28···O4xii0.932.533.384 (6)152
C29—H29···O5xii0.932.523.256 (6)137
C29—H29···O6xii0.932.553.284 (6)136

Symmetry codes: (v) x+1, −y+1/2, z; (vi) −x, y+1/2, −z+1; (vii) −x, −y+1, −z+1; (viii) x, −y+1/2, z−1; (ix) x+1, y, z−1; (x) x, y, z−1; (xi) x+1, −y+1/2, z−1; (xii) −x+1, y+1/2, −z+1.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HG2545).

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