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

Zebiri, I.; Anak, B.; Djebli, Y.; Boufas, S.; Bencharif, L.

doi:10.1107/S1600536809031092

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 9| September 2009| Pages m1063-m1064

doi:10.1107/S1600536809031092

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

Ikram Zebiri,^a Berkahoum Anak,^a Yacine Djebli,^a Sihem Boufas ^a,^b ^* and Leïla Bencharif ^a

^aLaboratoire de Chimie des Matériaux, Faculté des Sciences, Université Mentouri, 25000 Constantine, Algeria, and ^bUniversité 20 Aout 1955, Skikda, Algeria
^*Correspondence e-mail: boufas_sihem@yahoo.fr

(Received 30 July 2009; accepted 5 August 2009; online 12 August 2009)

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

Experimental

Crystal data

(C₆H₄S₄)₈[Mo₆O₁₉]₂·C₂H₃N
M_r = 3434.99
Monoclinic, P 2₁ /m
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 ) 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[F² > 2σ(F²)] = 0.036
wR(F²) = 0.073
S = 1
11170 reflections
629 parameters
H-atom parameters constrained
Δρ_max = 0.88 e Å⁻³
Δρ_min = −0.70 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C5—H5⋯O11ⁱ	0.93	2.28	3.192 (6)	167
C7—H7⋯O19ⁱⁱ	0.93	2.47	3.251 (7)	141
C7—H7⋯O19ⁱⁱⁱ	0.93	2.47	3.251 (7)	141
C9—H9⋯O12	0.93	2.54	3.388 (5)	151
C13—H13⋯O17^iv	0.93	2.41	3.239 (6)	149
C14—H14⋯O19^v	0.93	2.59	3.175 (5)	121
C18—H18⋯O18^vi	0.93	2.41	3.145 (5)	136
C19—H19⋯O10^vii	0.93	2.41	3.298 (5)	160
C20—H20⋯O12	0.93	2.54	3.437 (5)	162
C24—H24⋯O8^viii	0.93	2.25	3.075 (6)	148
C28—H28⋯O4^viii	0.93	2.53	3.384 (6)	152
C29—H29⋯O5^viii	0.93	2.52	3.256 (6)	137
C29—H29⋯O6^viii	0.93	2.55	3.284 (6)	136
Symmetry codes: (i) $[x+1, -y+{\script{1\over 2}}, z]$ ; (ii) $[-x, y+{\script{1\over 2}}, -z+1]$ ; (iii) -x, -y+1, -z+1; (iv) $[x, -y+{\script{1\over 2}}, z-1]$ ; (v) x+1, y, z-1; (vi) x, y, z-1; (vii) $[x+1, -y+{\script{1\over 2}}, z-1]$ ; (viii) $[-x+1, y+{\script{1\over 2}}, -z+1]$ .

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

Supporting information

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

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

checkCIF report

Comment top

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.

Related literature top

For the chemical and physical properties of polyoxomolybdates, see: Shi et al. (2006); Wang et al. (2004); Hagrman et al. (1999). For the structure of ammonium tris(tetraethylammonium) hexacosaoxidooctamolybdate, see: Zebiri et al. (2008). The title compound is isostructural to (TTF)₄W₆O₁₉.0.5CH₃CN, see: Triki et al. (1993). The structure of the anions is the same as that in bis[2-(pyrimidin-2-ylamino)pyrimidinium] hexamolybdate, see: Yeh et al. (2008);. For Mo—O distances, see: Boyle et al. (1998); Deng et al. (2006); Maeda et al. (2006).

Experimental top

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.

Computing details top

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

Figures top

	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.

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

Crystal data top

(C₆H₄S₄)₈[Mo₆O₁₉]₂·C₂H₃N	F(000) = 3324
M_r = 3434.99	D_x = 2.396 Mg m⁻³
Monoclinic, P2₁/m	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yb	Cell parameters from 2190 reflections
a = 14.3179 (8) Å	θ = 2.8–27.3°
b = 20.2299 (10) Å	µ = 2.31 mm⁻¹
c = 16.7625 (10) Å	T = 100 K
β = 101.266 (3)°	Plates, colourless
V = 4761.7 (5) Å³	0.25 × 0.15 × 0.1 mm
Z = 2

Data collection top

Nonius KappaCCD diffractometer	11170 independent reflections
Radiation source: fine-focus sealed X-ray tube	8144 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.072
ϕ scans, and ω scans with κ offsets	θ_max = 27.5°, θ_min = 1.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −18→18
T_min = 0.597, T_max = 0.802	k = −26→26
45527 measured reflections	l = −21→21

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.036	H-atom parameters constrained
wR(F²) = 0.073	w = 1/[σ²(F_o²) + (0.021P)²] where P = (F_o² + 2F_c²)/3
S = 1	(Δ/σ)_max = 0.003
11170 reflections	Δρ_max = 0.88 e Å⁻³
629 parameters	Δρ_min = −0.70 e Å⁻³
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.08 (2)

Crystal data top

(C₆H₄S₄)₈[Mo₆O₁₉]₂·C₂H₃N	V = 4761.7 (5) Å³
M_r = 3434.99	Z = 2
Monoclinic, P2₁/m	Mo Kα radiation
a = 14.3179 (8) Å	µ = 2.31 mm⁻¹
b = 20.2299 (10) Å	T = 100 K
c = 16.7625 (10) Å	0.25 × 0.15 × 0.1 mm
β = 101.266 (3)°

Data collection top

Nonius KappaCCD diffractometer	11170 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	8144 reflections with I > 2σ(I)
T_min = 0.597, T_max = 0.802	R_int = 0.072
45527 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.036	0 restraints
wR(F²) = 0.073	H-atom parameters constrained
S = 1	Δρ_max = 0.88 e Å⁻³
11170 reflections	Δρ_min = −0.70 e Å⁻³
629 parameters

Special details top

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) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Mo1	0.56723 (3)	0.411518 (19)	0.58067 (2)	0.01535 (9)
Mo2	0.37343 (3)	0.500847 (18)	0.56738 (2)	0.01262 (8)
Mo5	0.41862 (3)	0.425991 (19)	0.40423 (2)	0.01562 (9)
Mo3	0.09471 (3)	0.007942 (18)	0.90255 (2)	0.01440 (9)
Mo4	0.12057 (3)	0.050345 (18)	1.09450 (2)	0.01550 (9)
Mo6	−0.06607 (3)	0.102673 (18)	0.96110 (2)	0.01461 (9)
S4	0.69926 (8)	0.32365 (5)	0.32774 (7)	0.0171 (2)
S1	0.83864 (9)	0.32314 (6)	0.19478 (7)	0.0194 (3)
S2	0.31973 (9)	0.32349 (5)	0.68472 (7)	0.0193 (3)
S3	1.13888 (8)	0.41650 (5)	0.47871 (7)	0.0141 (2)
S5	0.85700 (8)	0.41673 (5)	0.53863 (7)	0.0134 (2)
S6	0.94719 (8)	0.41562 (5)	0.37833 (7)	0.0148 (2)
S7	1.04691 (8)	0.41757 (5)	0.64209 (7)	0.0158 (2)
S8	0.19893 (11)	0.75	0.39380 (10)	0.0162 (3)
S9	0.38303 (8)	0.16665 (6)	0.03769 (7)	0.0186 (3)
S10	−0.09582 (11)	0.75	0.43604 (10)	0.0167 (3)
S11	0.01173 (12)	0.75	0.27956 (10)	0.0187 (4)
S12	0.09410 (11)	0.75	0.54638 (9)	0.0157 (3)
S13	0.57537 (8)	0.16549 (5)	0.13620 (7)	0.0169 (2)
S14	0.47171 (8)	0.16799 (6)	−0.12637 (7)	0.0174 (2)
S15	0.66417 (8)	0.16465 (6)	−0.02771 (7)	0.0204 (3)
S18	0.21028 (8)	0.32348 (5)	0.83822 (7)	0.0177 (2)
O1	0	0	1	0.0106 (9)
O2	0.5	0.5	0.5	0.0119 (9)
O5	0.4513 (2)	0.43340 (14)	0.62260 (17)	0.0153 (7)
O4	0.2801 (2)	0.50318 (14)	0.61450 (18)	0.0159 (7)
O3	0.6587 (2)	0.43007 (14)	0.51664 (18)	0.0169 (7)
O6	0.4587 (2)	0.56620 (14)	0.62598 (17)	0.0150 (7)
O12	0.4888 (2)	0.36829 (14)	0.49387 (18)	0.0161 (7)
O7	0.6179 (2)	0.49293 (14)	0.64424 (17)	0.0166 (7)
O8	−0.0228 (2)	−0.03840 (14)	0.84668 (18)	0.0195 (7)
O9	0.3326 (2)	0.44003 (14)	0.47865 (18)	0.0159 (7)
O10	0.0391 (2)	0.12578 (13)	1.03983 (18)	0.0166 (7)
O11	0.0124 (2)	0.08657 (13)	0.88356 (18)	0.0178 (7)
O13	0.1560 (2)	−0.03770 (14)	1.10491 (19)	0.0204 (7)
O14	0.1549 (2)	0.01313 (14)	0.82549 (19)	0.0215 (7)
O15	0.1685 (2)	0.05279 (13)	0.99087 (18)	0.0158 (7)
O16	0.3610 (2)	0.36980 (15)	0.33835 (19)	0.0234 (8)
O19	−0.1227 (2)	0.17476 (14)	0.93106 (19)	0.0221 (7)
O18	0.2048 (2)	0.09129 (14)	1.1612 (2)	0.0245 (8)
O17	0.6166 (2)	0.35055 (15)	0.64365 (19)	0.0245 (8)
O20	0.1308 (2)	−0.07465 (14)	0.95163 (19)	0.0200 (7)
C1	0.7991 (4)	0.25	0.2352 (4)	0.0127 (13)
C4	0.9789 (3)	0.4167 (2)	0.5449 (3)	0.0145 (9)
C3	0.1983 (5)	0.75	0.2897 (4)	0.0204 (15)
H3	0.2548	0.75	0.2703	0.025*
C2	0.7423 (4)	0.25	0.2902 (4)	0.0143 (13)
C7	0.1143 (5)	0.75	0.2388 (4)	0.0224 (15)
H7	0.1107	0.75	0.1828	0.027*
C8	0.0738 (5)	0.75	0.3820 (4)	0.0170 (14)
C6	0.8635 (3)	0.4170 (2)	0.6423 (3)	0.0166 (10)
H6	0.8088	0.4169	0.6643	0.02*
C5	0.9505 (3)	0.4174 (2)	0.6901 (3)	0.0178 (10)
H5	0.9585	0.4176	0.7465	0.021*
C11	0.2420 (4)	0.25	0.7930 (4)	0.0149 (13)
C10	0.2854 (4)	0.25	0.7292 (4)	0.0160 (14)
C15	0.5424 (3)	0.1666 (2)	−0.0301 (3)	0.0174 (10)
C16	0.5044 (3)	0.1662 (2)	0.0406 (3)	0.0172 (10)
C13	0.5655 (3)	0.1660 (2)	−0.1775 (3)	0.0216 (11)
H13	0.5553	0.166	−0.234	0.026*
C12	0.1572 (3)	0.2831 (2)	0.9098 (3)	0.0223 (11)
H12	0.1297	0.3068	0.9468	0.027*
C14	0.6539 (3)	0.1643 (2)	−0.1321 (3)	0.0210 (11)
H14	0.7074	0.163	−0.1559	0.025*
C9	0.3514 (3)	0.2832 (2)	0.6016 (3)	0.0231 (11)
H9	0.3676	0.307	0.5588	0.028*
C22	1.0177 (3)	0.41639 (19)	0.4749 (3)	0.0132 (9)
C17	0.4818 (3)	0.1637 (2)	0.1873 (3)	0.0180 (10)
H17	0.4923	0.1623	0.2438	0.022*
C18	0.3931 (3)	0.1643 (2)	0.1421 (3)	0.0185 (10)
H18	0.3396	0.1635	0.1659	0.022*
C21	0.0295 (4)	0.75	0.4457 (4)	0.0165 (14)
C20	0.6422 (3)	0.2833 (2)	0.3968 (3)	0.0211 (11)
H20	0.6127	0.307	0.4325	0.025*
C19	0.9255 (3)	0.2830 (2)	0.1533 (3)	0.0235 (11)
H19	0.9704	0.3067	0.1319	0.028*
C24	1.0417 (3)	0.4110 (2)	0.3287 (3)	0.0197 (10)
H24	1.0322	0.4084	0.2723	0.024*
C23	1.1297 (3)	0.4114 (2)	0.3748 (3)	0.0174 (10)
H23	1.1836	0.4089	0.3516	0.021*
C26	−0.0077 (4)	0.75	0.5908 (4)	0.0184 (14)
H26	−0.0027	0.75	0.6469	0.022*
C25	−0.0915 (5)	0.75	0.5408 (4)	0.0186 (14)
H25	−0.1474	0.75	0.5613	0.022*
S16	0.43075 (9)	0.99818 (6)	0.10594 (7)	0.0200 (3)
S27	0.63331 (9)	0.99422 (6)	0.09037 (7)	0.0203 (3)
C27	0.5135 (3)	0.9988 (2)	0.0403 (3)	0.0166 (10)
C29	0.5178 (4)	0.9954 (2)	0.1949 (3)	0.0245 (11)
H29	0.5008	0.9954	0.2457	0.029*
C28	0.6083 (4)	0.9931 (2)	0.1884 (3)	0.0247 (11)
H28	0.6568	0.991	0.2342	0.03*
N1	0.1799 (6)	0.25	0.1110 (5)	0.061 (2)
C30	0.1822 (6)	0.25	0.1791 (7)	0.049 (3)
C31	0.1876 (6)	0.25	0.2689 (6)	0.050 (2)
H31A	0.1353	0.2749	0.2815	0.076*	0.5
H31B	0.2466	0.2697	0.2953	0.076*	0.5
H31C	0.1845	0.2054	0.2876	0.076*	0.5

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mo1	0.0150 (2)	0.0195 (2)	0.0125 (2)	0.00474 (16)	0.00522 (16)	0.00528 (16)
Mo2	0.01036 (18)	0.0189 (2)	0.00921 (18)	0.00057 (16)	0.00335 (15)	0.00047 (15)
Mo5	0.0138 (2)	0.0217 (2)	0.01209 (19)	−0.00355 (16)	0.00420 (16)	−0.00492 (16)
Mo3	0.0168 (2)	0.0162 (2)	0.01122 (19)	−0.00087 (16)	0.00517 (16)	0.00087 (15)
Mo4	0.0164 (2)	0.0170 (2)	0.01202 (19)	−0.00345 (16)	0.00029 (16)	−0.00233 (15)
Mo6	0.0185 (2)	0.0131 (2)	0.01240 (19)	0.00125 (16)	0.00348 (16)	0.00127 (15)
S4	0.0199 (6)	0.0162 (6)	0.0154 (6)	0.0025 (5)	0.0038 (5)	−0.0010 (5)
S1	0.0213 (6)	0.0191 (6)	0.0189 (6)	−0.0011 (5)	0.0062 (5)	0.0029 (5)
S2	0.0241 (7)	0.0177 (6)	0.0166 (6)	−0.0050 (5)	0.0055 (5)	0.0010 (5)
S3	0.0110 (5)	0.0164 (6)	0.0148 (6)	−0.0019 (4)	0.0023 (5)	−0.0003 (4)
S5	0.0114 (5)	0.0163 (6)	0.0122 (5)	0.0001 (4)	0.0018 (4)	0.0009 (4)
S6	0.0148 (6)	0.0171 (6)	0.0117 (5)	−0.0021 (4)	0.0006 (5)	0.0014 (4)
S7	0.0152 (6)	0.0186 (6)	0.0121 (5)	−0.0005 (5)	−0.0008 (5)	0.0000 (4)
S8	0.0155 (8)	0.0175 (8)	0.0151 (8)	0	0.0017 (7)	0
S9	0.0149 (6)	0.0223 (6)	0.0184 (6)	−0.0005 (5)	0.0028 (5)	−0.0022 (5)
S10	0.0151 (8)	0.0176 (8)	0.0161 (8)	0	−0.0006 (7)	0
S11	0.0227 (9)	0.0184 (8)	0.0124 (8)	0	−0.0027 (7)	0
S12	0.0155 (8)	0.0173 (8)	0.0126 (8)	0	−0.0016 (7)	0
S13	0.0163 (6)	0.0215 (6)	0.0127 (6)	0.0001 (5)	0.0021 (5)	−0.0004 (5)
S14	0.0188 (6)	0.0213 (6)	0.0118 (6)	0.0011 (5)	0.0019 (5)	−0.0001 (5)
S15	0.0158 (6)	0.0278 (7)	0.0182 (6)	0.0030 (5)	0.0046 (5)	0.0017 (5)
S18	0.0210 (6)	0.0147 (6)	0.0177 (6)	−0.0002 (5)	0.0046 (5)	−0.0021 (5)
O1	0.013 (2)	0.012 (2)	0.007 (2)	−0.0012 (17)	0.0024 (17)	−0.0010 (16)
O2	0.010 (2)	0.016 (2)	0.011 (2)	0.0002 (17)	0.0043 (18)	0.0001 (17)
O5	0.0175 (17)	0.0193 (16)	0.0103 (15)	0.0010 (13)	0.0054 (13)	0.0021 (12)
O4	0.0135 (16)	0.0218 (17)	0.0133 (16)	−0.0001 (13)	0.0047 (13)	−0.0004 (13)
O3	0.0134 (16)	0.0221 (16)	0.0164 (17)	0.0041 (13)	0.0052 (14)	0.0028 (13)
O6	0.0153 (16)	0.0199 (16)	0.0109 (15)	−0.0017 (13)	0.0053 (13)	−0.0024 (13)
O12	0.0207 (17)	0.0149 (16)	0.0149 (16)	−0.0004 (13)	0.0091 (14)	−0.0004 (12)
O7	0.0131 (16)	0.0259 (17)	0.0102 (16)	0.0016 (13)	0.0012 (13)	0.0014 (13)
O8	0.0240 (18)	0.0230 (17)	0.0114 (16)	−0.0007 (14)	0.0032 (14)	−0.0036 (13)
O9	0.0137 (16)	0.0207 (17)	0.0149 (16)	−0.0036 (13)	0.0068 (13)	−0.0031 (13)
O10	0.0193 (17)	0.0122 (15)	0.0188 (17)	−0.0036 (13)	0.0049 (14)	−0.0019 (13)
O11	0.0200 (17)	0.0164 (16)	0.0168 (17)	−0.0021 (13)	0.0026 (14)	0.0020 (13)
O13	0.0192 (17)	0.0219 (17)	0.0173 (17)	−0.0010 (14)	−0.0034 (14)	0.0015 (14)
O14	0.0254 (19)	0.0192 (17)	0.0229 (19)	−0.0013 (14)	0.0120 (16)	0.0011 (14)
O15	0.0126 (16)	0.0171 (16)	0.0183 (17)	−0.0035 (13)	0.0040 (13)	−0.0032 (13)
O16	0.0220 (18)	0.0321 (19)	0.0167 (18)	−0.0051 (15)	0.0054 (15)	−0.0125 (14)
O19	0.0264 (19)	0.0181 (17)	0.0227 (18)	0.0025 (14)	0.0066 (16)	0.0043 (14)
O18	0.0244 (18)	0.0251 (18)	0.0215 (18)	−0.0084 (14)	−0.0017 (15)	−0.0043 (14)
O17	0.028 (2)	0.0275 (18)	0.0197 (19)	0.0115 (15)	0.0097 (16)	0.0075 (14)
O20	0.0219 (18)	0.0160 (16)	0.0245 (19)	−0.0015 (13)	0.0102 (15)	−0.0005 (14)
C1	0.015 (3)	0.013 (3)	0.011 (3)	0	0.006 (3)	0
C4	0.011 (2)	0.012 (2)	0.019 (2)	0.0005 (17)	−0.0005 (19)	0.0019 (18)
C3	0.022 (4)	0.028 (4)	0.012 (3)	0	0.006 (3)	0
C2	0.018 (3)	0.014 (3)	0.009 (3)	0	−0.002 (3)	0
C7	0.036 (4)	0.021 (4)	0.012 (3)	0	0.010 (3)	0
C8	0.026 (4)	0.019 (3)	0.005 (3)	0	−0.001 (3)	0
C6	0.016 (2)	0.017 (2)	0.018 (2)	0.0003 (18)	0.006 (2)	0.0009 (19)
C5	0.026 (3)	0.017 (2)	0.011 (2)	−0.002 (2)	0.005 (2)	−0.0006 (18)
C11	0.014 (3)	0.015 (3)	0.014 (3)	0	−0.003 (3)	0
C10	0.016 (3)	0.015 (3)	0.015 (3)	0	0.000 (3)	0
C15	0.016 (2)	0.021 (2)	0.014 (2)	0.0026 (19)	0.001 (2)	−0.0020 (19)
C16	0.019 (2)	0.018 (2)	0.015 (2)	−0.0004 (19)	0.004 (2)	−0.0005 (19)
C13	0.032 (3)	0.021 (3)	0.014 (2)	0.005 (2)	0.010 (2)	0.0023 (19)
C12	0.019 (3)	0.028 (3)	0.021 (3)	0.005 (2)	0.009 (2)	−0.001 (2)
C14	0.020 (3)	0.028 (3)	0.017 (3)	0.006 (2)	0.010 (2)	0.001 (2)
C9	0.024 (3)	0.031 (3)	0.016 (3)	−0.003 (2)	0.008 (2)	0.002 (2)
C22	0.014 (2)	0.007 (2)	0.016 (2)	−0.0029 (17)	−0.0017 (19)	−0.0001 (17)
C17	0.023 (3)	0.019 (2)	0.013 (2)	0.001 (2)	0.007 (2)	−0.0021 (19)
C18	0.021 (3)	0.016 (2)	0.022 (3)	−0.0033 (19)	0.011 (2)	−0.0040 (19)
C21	0.014 (3)	0.018 (3)	0.013 (3)	0	−0.006 (3)	0
C20	0.024 (3)	0.030 (3)	0.010 (2)	0.006 (2)	0.007 (2)	−0.0007 (19)
C19	0.023 (3)	0.034 (3)	0.017 (3)	−0.003 (2)	0.011 (2)	0.001 (2)
C24	0.025 (3)	0.022 (3)	0.011 (2)	−0.005 (2)	0.002 (2)	0.0009 (19)
C23	0.021 (2)	0.020 (2)	0.012 (2)	−0.0021 (19)	0.005 (2)	0.0018 (18)
C26	0.021 (4)	0.015 (3)	0.020 (4)	0	0.005 (3)	0
C25	0.027 (4)	0.013 (3)	0.017 (3)	0	0.006 (3)	0
S16	0.0263 (7)	0.0219 (6)	0.0124 (6)	0.0039 (5)	0.0053 (5)	−0.0005 (5)
S27	0.0219 (6)	0.0245 (6)	0.0127 (6)	0.0035 (5)	−0.0012 (5)	−0.0004 (5)
C27	0.021 (2)	0.015 (2)	0.013 (2)	0.0028 (19)	0.003 (2)	−0.0002 (18)
C29	0.039 (3)	0.022 (3)	0.010 (2)	0.002 (2)	−0.001 (2)	−0.0004 (19)
C28	0.035 (3)	0.022 (3)	0.012 (2)	0.005 (2)	−0.007 (2)	−0.0015 (19)
N1	0.071 (6)	0.060 (5)	0.050 (5)	0	0.002 (5)	0
C30	0.038 (5)	0.026 (5)	0.084 (8)	0	0.014 (6)	0
C31	0.051 (6)	0.033 (5)	0.071 (7)	0	0.021 (5)	0

Geometric parameters (Å, º) top

Mo1—O17	1.686 (3)	S15—C14	1.727 (5)
Mo1—O12	1.872 (3)	S15—C15	1.736 (5)
Mo1—O3	1.886 (3)	S18—C12	1.743 (5)
Mo1—O5	1.974 (3)	S18—C11	1.768 (4)
Mo1—O7	2.018 (3)	O1—Mo6ⁱⁱ	2.3222 (4)
Mo1—O2	2.3345 (4)	O1—Mo3ⁱⁱ	2.3234 (4)
Mo2—O4	1.680 (3)	O1—Mo4ⁱⁱ	2.3363 (4)
Mo2—O5	1.887 (3)	O2—Mo2ⁱ	2.3151 (4)
Mo2—O9	1.931 (3)	O2—Mo5ⁱ	2.3335 (4)
Mo2—O6	1.932 (3)	O2—Mo1ⁱ	2.3345 (4)
Mo2—O3ⁱ	1.974 (3)	O3—Mo2ⁱ	1.974 (3)
Mo2—O2	2.3151 (4)	O6—Mo5ⁱ	1.928 (3)
Mo5—O16	1.684 (3)	O7—Mo5ⁱ	1.860 (3)
Mo5—O7ⁱ	1.860 (3)	O8—Mo4ⁱⁱ	1.879 (3)
Mo5—O6ⁱ	1.928 (3)	O13—Mo6ⁱⁱ	2.013 (3)
Mo5—O9	1.937 (3)	O20—Mo6ⁱⁱ	1.962 (3)
Mo5—O12	2.010 (3)	C1—C2	1.343 (8)
Mo5—O2	2.3335 (4)	C1—S1ⁱⁱⁱ	1.766 (3)
Mo3—O14	1.690 (3)	C4—C22	1.393 (6)
Mo3—O15	1.876 (3)	C3—C7	1.331 (9)
Mo3—O20	1.889 (3)	C3—H3	0.93
Mo3—O11	1.968 (3)	C2—S4ⁱⁱⁱ	1.774 (4)
Mo3—O8	1.993 (3)	C7—H7	0.93
Mo3—O1	2.3234 (4)	C8—C21	1.345 (9)
Mo4—O18	1.692 (3)	C6—C5	1.343 (6)
Mo4—O13	1.851 (3)	C6—H6	0.93
Mo4—O8ⁱⁱ	1.879 (3)	C5—H5	0.93
Mo4—O15	1.989 (3)	C11—C10	1.339 (9)
Mo4—O10	2.028 (3)	C11—S18ⁱⁱⁱ	1.768 (4)
Mo4—O1	2.3363 (4)	C10—S2ⁱⁱⁱ	1.774 (4)
Mo6—O19	1.696 (3)	C15—C16	1.398 (6)
Mo6—O10	1.858 (3)	C13—C14	1.343 (6)
Mo6—O11	1.905 (3)	C13—H13	0.93
Mo6—O20ⁱⁱ	1.962 (3)	C12—C12ⁱⁱⁱ	1.340 (9)
Mo6—O13ⁱⁱ	2.013 (3)	C12—H12	0.93
Mo6—O1	2.3222 (4)	C14—H14	0.93
S4—C20	1.746 (5)	C9—C9ⁱⁱⁱ	1.343 (9)
S4—C2	1.774 (4)	C9—H9	0.93
S1—C19	1.739 (5)	C17—C18	1.347 (6)
S1—C1	1.766 (3)	C17—H17	0.93
S2—C9	1.749 (5)	C18—H18	0.93
S2—C10	1.774 (4)	C20—C20ⁱⁱⁱ	1.347 (9)
S3—C23	1.723 (4)	C20—H20	0.93
S3—C22	1.724 (4)	C19—C19ⁱⁱⁱ	1.335 (9)
S5—C6	1.721 (5)	C19—H19	0.93
S5—C4	1.727 (4)	C24—C23	1.344 (6)
S6—C24	1.724 (5)	C24—H24	0.93
S6—C22	1.732 (4)	C23—H23	0.93
S7—C4	1.728 (4)	C26—C25	1.323 (9)
S7—C5	1.728 (5)	C26—H26	0.93
S8—C3	1.743 (6)	C25—H25	0.93
S8—C8	1.764 (7)	S16—C29	1.748 (5)
S9—C18	1.728 (5)	S16—C27	1.767 (5)
S9—C16	1.728 (5)	S27—C28	1.749 (5)
S10—C25	1.746 (6)	S27—C27	1.759 (5)
S10—C21	1.769 (6)	C27—C27^iv	1.330 (8)
S11—C7	1.737 (7)	C29—C28	1.322 (7)
S11—C8	1.772 (6)	C29—H29	0.93
S12—C21	1.759 (6)	C28—H28	0.93
S12—C26	1.761 (7)	N1—C30	1.136 (12)
S13—C16	1.722 (5)	C30—C31	1.492 (13)
S13—C17	1.725 (5)	C31—H31A	0.96
S14—C15	1.729 (4)	C31—H31B	0.96
S14—C13	1.729 (5)	C31—H31C	0.96

O17—Mo1—O12	105.04 (14)	Mo2—O2—Mo5ⁱ	89.589 (13)
O17—Mo1—O3	104.43 (14)	Mo2ⁱ—O2—Mo5ⁱ	90.411 (14)
O12—Mo1—O3	91.61 (13)	Mo2—O2—Mo5	90.411 (14)
O17—Mo1—O5	102.70 (14)	Mo2ⁱ—O2—Mo5	89.589 (13)
O12—Mo1—O5	87.90 (12)	Mo5ⁱ—O2—Mo5	180.000 (15)
O3—Mo1—O5	152.02 (12)	Mo2—O2—Mo1	89.800 (13)
O17—Mo1—O7	101.69 (14)	Mo2ⁱ—O2—Mo1	90.200 (13)
O12—Mo1—O7	152.99 (12)	Mo5ⁱ—O2—Mo1	89.969 (14)
O3—Mo1—O7	85.42 (12)	Mo5—O2—Mo1	90.031 (14)
O5—Mo1—O7	82.51 (12)	Mo2—O2—Mo1ⁱ	90.200 (13)
O17—Mo1—O2	176.68 (11)	Mo2ⁱ—O2—Mo1ⁱ	89.800 (13)
O12—Mo1—O2	77.94 (9)	Mo5ⁱ—O2—Mo1ⁱ	90.031 (14)
O3—Mo1—O2	76.77 (9)	Mo5—O2—Mo1ⁱ	89.969 (14)
O5—Mo1—O2	75.78 (8)	Mo1—O2—Mo1ⁱ	180
O7—Mo1—O2	75.24 (8)	Mo2—O5—Mo1	116.42 (14)
O4—Mo2—O5	103.76 (13)	Mo1—O3—Mo2ⁱ	117.16 (14)
O4—Mo2—O9	103.37 (13)	Mo5ⁱ—O6—Mo2	116.11 (14)
O5—Mo2—O9	88.74 (12)	Mo1—O12—Mo5	116.50 (14)
O4—Mo2—O6	102.89 (13)	Mo5ⁱ—O7—Mo1	116.59 (14)
O5—Mo2—O6	89.50 (12)	Mo4ⁱⁱ—O8—Mo3	117.46 (15)
O9—Mo2—O6	153.33 (12)	Mo2—O9—Mo5	117.05 (14)
O4—Mo2—O3ⁱ	102.71 (13)	Mo6—O10—Mo4	116.53 (14)
O5—Mo2—O3ⁱ	153.52 (12)	Mo6—O11—Mo3	116.24 (15)
O9—Mo2—O3ⁱ	84.73 (12)	Mo4—O13—Mo6ⁱⁱ	116.26 (15)
O6—Mo2—O3ⁱ	85.07 (12)	Mo3—O15—Mo4	116.10 (14)
O4—Mo2—O2	178.36 (10)	Mo3—O20—Mo6ⁱⁱ	116.81 (15)
O5—Mo2—O2	77.87 (9)	C2—C1—S1	123.08 (17)
O9—Mo2—O2	76.54 (9)	C2—C1—S1ⁱⁱⁱ	123.08 (17)
O6—Mo2—O2	77.07 (9)	S1—C1—S1ⁱⁱⁱ	113.8 (3)
O3ⁱ—Mo2—O2	75.66 (8)	C22—C4—S5	120.9 (3)
O16—Mo5—O7ⁱ	104.41 (14)	C22—C4—S7	123.4 (3)
O16—Mo5—O6ⁱ	103.77 (14)	S5—C4—S7	115.7 (3)
O7ⁱ—Mo5—O6ⁱ	90.34 (12)	C7—C3—S8	118.0 (5)
O16—Mo5—O9	103.27 (14)	C7—C3—H3	121
O7ⁱ—Mo5—O9	89.55 (12)	S8—C3—H3	121
O6ⁱ—Mo5—O9	152.09 (12)	C1—C2—S4ⁱⁱⁱ	122.83 (18)
O16—Mo5—O12	101.98 (14)	C1—C2—S4	122.83 (18)
O7ⁱ—Mo5—O12	153.60 (12)	S4ⁱⁱⁱ—C2—S4	114.3 (4)
O6ⁱ—Mo5—O12	84.01 (12)	C3—C7—S11	118.3 (5)
O9—Mo5—O12	83.78 (12)	C3—C7—H7	120.8
O16—Mo5—O2	177.36 (11)	S11—C7—H7	120.8
O7ⁱ—Mo5—O2	78.16 (9)	C21—C8—S8	122.5 (5)
O6ⁱ—Mo5—O2	76.70 (8)	C21—C8—S11	123.0 (5)
O9—Mo5—O2	75.98 (8)	S8—C8—S11	114.5 (4)
O12—Mo5—O2	75.45 (8)	C5—C6—S5	117.6 (4)
O14—Mo3—O15	106.28 (14)	C5—C6—H6	121.2
O14—Mo3—O20	104.51 (14)	S5—C6—H6	121.2
O15—Mo3—O20	91.14 (13)	C6—C5—S7	117.0 (4)
O14—Mo3—O11	101.82 (14)	C6—C5—H5	121.5
O15—Mo3—O11	87.94 (12)	S7—C5—H5	121.5
O20—Mo3—O11	152.81 (13)	C10—C11—S18ⁱⁱⁱ	122.77 (18)
O14—Mo3—O8	100.35 (14)	C10—C11—S18	122.77 (18)
O15—Mo3—O8	153.12 (13)	S18ⁱⁱⁱ—C11—S18	114.5 (4)
O20—Mo3—O8	85.58 (13)	C11—C10—S2	123.05 (18)
O11—Mo3—O8	83.12 (12)	C11—C10—S2ⁱⁱⁱ	123.05 (18)
O14—Mo3—O1	175.05 (11)	S2—C10—S2ⁱⁱⁱ	113.8 (4)
O15—Mo3—O1	78.15 (9)	C16—C15—S14	122.5 (3)
O20—Mo3—O1	77.32 (9)	C16—C15—S15	122.4 (3)
O11—Mo3—O1	75.90 (9)	S14—C15—S15	115.1 (3)
O8—Mo3—O1	75.10 (9)	C15—C16—S13	122.1 (4)
O18—Mo4—O13	105.18 (14)	C15—C16—S9	122.2 (4)
O18—Mo4—O8ⁱⁱ	102.97 (15)	S13—C16—S9	115.7 (3)
O13—Mo4—O8ⁱⁱ	92.59 (13)	C14—C13—S14	117.2 (4)
O18—Mo4—O15	103.98 (14)	C14—C13—H13	121.4
O13—Mo4—O15	88.36 (13)	S14—C13—H13	121.4
O8ⁱⁱ—Mo4—O15	151.77 (12)	C12ⁱⁱⁱ—C12—S18	117.92 (15)
O18—Mo4—O10	101.72 (13)	C12ⁱⁱⁱ—C12—H12	121
O13—Mo4—O10	152.84 (12)	S18—C12—H12	121
O8ⁱⁱ—Mo4—O10	84.97 (12)	C13—C14—S15	117.2 (4)
O15—Mo4—O10	81.52 (12)	C13—C14—H14	121.4
O18—Mo4—O1	176.53 (11)	S15—C14—H14	121.4
O13—Mo4—O1	78.29 (9)	C9ⁱⁱⁱ—C9—S2	117.77 (15)
O8ⁱⁱ—Mo4—O1	76.83 (9)	C9ⁱⁱⁱ—C9—H9	121.1
O15—Mo4—O1	75.75 (8)	S2—C9—H9	121.1
O10—Mo4—O1	74.81 (8)	C4—C22—S3	122.2 (3)
O19—Mo6—O10	105.57 (14)	C4—C22—S6	122.1 (3)
O19—Mo6—O11	104.81 (14)	S3—C22—S6	115.7 (3)
O10—Mo6—O11	91.35 (13)	C18—C17—S13	117.3 (4)
O19—Mo6—O20ⁱⁱ	101.65 (14)	C18—C17—H17	121.3
O10—Mo6—O20ⁱⁱ	88.78 (13)	S13—C17—H17	121.3
O11—Mo6—O20ⁱⁱ	152.48 (12)	C17—C18—S9	117.0 (4)
O19—Mo6—O13ⁱⁱ	100.43 (14)	C17—C18—H18	121.5
O10—Mo6—O13ⁱⁱ	153.81 (12)	S9—C18—H18	121.5
O11—Mo6—O13ⁱⁱ	84.97 (13)	C8—C21—S12	121.4 (5)
O20ⁱⁱ—Mo6—O13ⁱⁱ	82.91 (13)	C8—C21—S10	123.7 (5)
O19—Mo6—O1	175.58 (11)	S12—C21—S10	115.0 (4)
O10—Mo6—O1	78.25 (9)	C20ⁱⁱⁱ—C20—S4	117.88 (15)
O11—Mo6—O1	77.08 (8)	C20ⁱⁱⁱ—C20—H20	121.1
O20ⁱⁱ—Mo6—O1	76.01 (9)	S4—C20—H20	121.1
O13ⁱⁱ—Mo6—O1	75.65 (8)	C19ⁱⁱⁱ—C19—S1	117.84 (15)
C20—S4—C2	94.7 (2)	C19ⁱⁱⁱ—C19—H19	121.1
C19—S1—C1	94.0 (2)	S1—C19—H19	121.1
C9—S2—C10	94.6 (2)	C23—C24—S6	117.3 (4)
C23—S3—C22	94.9 (2)	C23—C24—H24	121.4
C6—S5—C4	94.8 (2)	S6—C24—H24	121.4
C24—S6—C22	94.7 (2)	C24—C23—S3	117.4 (4)
C4—S7—C5	94.9 (2)	C24—C23—H23	121.3
C3—S8—C8	94.6 (3)	S3—C23—H23	121.3
C18—S9—C16	95.0 (2)	C25—C26—S12	117.1 (5)
C25—S10—C21	94.1 (3)	C25—C26—H26	121.4
C7—S11—C8	94.5 (3)	S12—C26—H26	121.4
C21—S12—C26	94.7 (3)	C26—C25—S10	119.1 (5)
C16—S13—C17	95.0 (2)	C26—C25—H25	120.4
C15—S14—C13	95.3 (2)	S10—C25—H25	120.4
C14—S15—C15	95.2 (2)	C29—S16—C27	94.5 (2)
C12—S18—C11	94.8 (2)	C28—S27—C27	95.1 (2)
Mo6—O1—Mo6ⁱⁱ	180.000 (19)	C27^iv—C27—S27	123.3 (5)
Mo6—O1—Mo3ⁱⁱ	89.861 (13)	C27^iv—C27—S16	122.4 (5)
Mo6ⁱⁱ—O1—Mo3ⁱⁱ	90.139 (13)	S27—C27—S16	114.3 (2)
Mo6—O1—Mo3	90.139 (13)	C28—C29—S16	118.5 (4)
Mo6ⁱⁱ—O1—Mo3	89.861 (13)	C28—C29—H29	120.8
Mo3ⁱⁱ—O1—Mo3	180.0000 (10)	S16—C29—H29	120.8
Mo6—O1—Mo4	90.402 (14)	C29—C28—S27	117.5 (4)
Mo6ⁱⁱ—O1—Mo4	89.598 (13)	C29—C28—H28	121.3
Mo3ⁱⁱ—O1—Mo4	90.504 (14)	S27—C28—H28	121.3
Mo3—O1—Mo4	89.496 (14)	N1—C30—C31	178.7 (11)
Mo6—O1—Mo4ⁱⁱ	89.598 (13)	C30—C31—H31A	109.5
Mo6ⁱⁱ—O1—Mo4ⁱⁱ	90.402 (14)	C30—C31—H31B	109.5
Mo3ⁱⁱ—O1—Mo4ⁱⁱ	89.496 (14)	H31A—C31—H31B	109.5
Mo3—O1—Mo4ⁱⁱ	90.504 (14)	C30—C31—H31C	109.5
Mo4—O1—Mo4ⁱⁱ	180.0000 (10)	H31A—C31—H31C	109.5
Mo2—O2—Mo2ⁱ	180	H31B—C31—H31C	109.5

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, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C5—H5···O11^v	0.93	2.28	3.192 (6)	167
C7—H7···O19^vi	0.93	2.47	3.251 (7)	141
C7—H7···O19^vii	0.93	2.47	3.251 (7)	141
C9—H9···O12	0.93	2.54	3.388 (5)	151
C13—H13···O17^viii	0.93	2.41	3.239 (6)	149
C14—H14···O19^ix	0.93	2.59	3.175 (5)	121
C18—H18···O18^x	0.93	2.41	3.145 (5)	136
C19—H19···O10^xi	0.93	2.41	3.298 (5)	160
C20—H20···O12	0.93	2.54	3.437 (5)	162
C24—H24···O8^xii	0.93	2.25	3.075 (6)	148
C28—H28···O4^xii	0.93	2.53	3.384 (6)	152
C29—H29···O5^xii	0.93	2.52	3.256 (6)	137
C29—H29···O6^xii	0.93	2.55	3.284 (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.

Experimental details

Crystal data
Chemical formula	(C₆H₄S₄)₈[Mo₆O₁₉]₂·C₂H₃N
M_r	3434.99
Crystal system, space group	Monoclinic, P2₁/m
Temperature (K)	100
a, b, c (Å)	14.3179 (8), 20.2299 (10), 16.7625 (10)
β (°)	101.266 (3)
V (Å³)	4761.7 (5)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	2.31
Crystal size (mm)	0.25 × 0.15 × 0.1

Data collection
Diffractometer	Nonius KappaCCD diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.597, 0.802
No. of measured, independent and observed [I > 2σ(I)] reflections	45527, 11170, 8144
R_int	0.072
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.036, 0.073, 1
No. of reflections	11170
No. of parameters	629
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.88, −0.70

Computer programs: COLLECT (Nonius, 2002), DENZO and SCALEPACK (Otwinowski & Minor, 1997), SIR92 (Altomare et al., 1993), SHELXL97 (Sheldrick, 2008), ORTEP-3 (Farrugia, 1997) and Mercury (Macrae et al., 2006), WinGX (Farrugia, 1999) and PARST (Nardelli, 1995).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C5—H5···O11ⁱ	0.9300	2.2800	3.192 (6)	167.00
C7—H7···O19ⁱⁱ	0.9300	2.4700	3.251 (7)	141.00
C7—H7···O19ⁱⁱⁱ	0.9300	2.4700	3.251 (7)	141.00
C9—H9···O12	0.9300	2.5400	3.388 (5)	151.00
C13—H13···O17^iv	0.9300	2.4100	3.239 (6)	149.00
C14—H14···O19^v	0.9300	2.5900	3.175 (5)	121.00
C18—H18···O18^vi	0.9300	2.4100	3.145 (5)	136.00
C19—H19···O10^vii	0.9300	2.4100	3.298 (5)	160.00
C20—H20···O12	0.9300	2.5400	3.437 (5)	162.00
C24—H24···O8^viii	0.9300	2.2500	3.075 (6)	148.00
C28—H28···O4^viii	0.9300	2.5300	3.384 (6)	152.00
C29—H29···O5^viii	0.9300	2.5200	3.256 (6)	137.00
C29—H29···O6^viii	0.9300	2.5500	3.284 (6)	136.00

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

Acknowledgements

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.

References

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Volume 65| Part 9| September 2009| Pages m1063-m1064

doi:10.1107/S1600536809031092

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

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