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Acta Crystallogr Sect E Struct Rep Online. 2008 November 1; 64(Pt 11): m1370–m1371.
Published online 2008 October 9. doi:  10.1107/S1600536808031668
PMCID: PMC2959595

Di-μ3-oxido-di-μ2-oxido-tetra­oxido­bis­(1,1,2,2-tetra­methyl­ethylenedicyclo­penta­dien­yl)­dimolyb­denum(IV)­dimolybdenum(VI) hexa­hydrate

Abstract

The title compound, [Mo4(C16H20)2O8]·6H2O, is a centrosymmetric ansa-molybdocene complex in which two dinuclear [C2Me45-C5H4)2]Mo(μ2-O)2MoO2 units dimerize by forming two μ3-O bridges between three Mo atoms. The ansa-molybdocene [C2Me45-C5H4)2]Mo unit has a typical bent-sandwich metallocene structure with an inter-ring angle of 127.98 (8)°. The Mo atom in the bridging (μ2-O)(μ3-O)2MoO2 group has a distorted trigonal–bipyramidal coordination. The Mo—(μ3-O) and Mo—(μ2-O) bond distances inside the units [2.0869 (14) and 2.1014 (15) Å, respectively] are slightly longer than the Mo(−x + 1, −y + 1, −z)—(μ3-O) bond distance between the units [1.9986 (14) Å]. The solvent water mol­ecules together with complex O atoms form a network of O—H(...)O hydrogen bonds.

Related literature

For related structures, see: Prout & Daran (1978 [triangle]); Adam & Green (1981 [triangle]); Daran & Prout (1977 [triangle]); Prout et al. (1974 [triangle]). For general synthesis and reactivity information on related tetramethylethylene-bridged ansa-molybdocene complexes, see: Ahmed et al. (2007 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-64-m1370-scheme1.jpg

Experimental

Crystal data

  • [Mo4(C16H20)2O8]·6H2O
  • M r = 1044.50
  • Triclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-m1370-efi1.jpg
  • a = 7.4106 (7) Å
  • b = 9.3518 (8) Å
  • c = 13.5735 (12) Å
  • α = 93.365 (1)°
  • β = 98.604 (1)°
  • γ = 103.175 (1)°
  • V = 901.39 (14) Å3
  • Z = 1
  • Mo Kα radiation
  • μ = 1.43 mm−1
  • T = 173 (2) K
  • 0.30 × 0.09 × 0.07 mm

Data collection

  • Bruker APEX CCD diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 2000 [triangle]) T min = 0.673, T max = 0.907
  • 10175 measured reflections
  • 3916 independent reflections
  • 3621 reflections with I > 2σ(I)
  • R int = 0.014

Refinement

  • R[F 2 > 2σ(F 2)] = 0.021
  • wR(F 2) = 0.054
  • S = 1.09
  • 3916 reflections
  • 250 parameters
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 0.46 e Å−3
  • Δρmin = −0.41 e Å−3

Data collection: SMART (Bruker, 2000 [triangle]); cell refinement: SAINT (Bruker, 2000 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Table 1
Selected bond lengths (Å)
Table 2
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808031668/hb2806sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808031668/hb2806Isup2.hkl

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

Acknowledgments

We thank the NSF for funding.

supplementary crystallographic information

Comment

We previously reported the synthesis and characterization of ansa-molybdocenes bridged by tetramethylethylene linkages (Ahmed et al., 2007). Of those species, the monomeric [{C2Me45-C5H4)2}Mo(OH)(OH2)][C7H7SO3] was exploited for catalytic hydration and hydrolysis reactions in aqueous solution.

The title complex, (I), was obtained as large needles from the slow oxidation of the [{C2Me45-C5H4)2}Mo(OH)(OH2)][C7H7SO3] catalyst in the presence of 0.50 ml ethyl acetate in water at approximately pH 4. It is uncertain whether the title compound exists in equilibrium with the catalytic complex in water under anaerobic conditions. The compound is a centrosymmetric ansa-molybdocene complex in which two {C2Me45-C5H4)2}Mo(µ2-O)2MoO2 units are connected by two µ3-O bridges between three Mo atoms (Fig. 1). The ansa-molybdocene {C2Me45-C5H4)2}Mo2 has a typical bent-sandwich structure with an angle of 127.98 (8)° between the average planes of the C5-rings. The Mo atom in the bridging (µ2-0)(µ3-O)2MoO2 group has a distorted trigonal bipyramidal coordination. The Mo(1)-(µ3-O) and Mo(1)-(µ2-O) bond distances, 2.0869 (14) and 2.1014 (15) Å, respectively, are slightly longer than the O(1)-Mo(2)(1-x, 1-y,-z) bond distance, 1.9986 (14) Å (Table 1). Solvent water molecules together with O atoms of the (µ2-0)(µ3-O)2MoO2 groups form a network of H-bonds (Table 2, Fig. 2).

Analogous non-ansa oxides, [(η5-C5H4R)2Mo2O4]2 (where R = H or Me), were reported in previous literature (Prout et al., 1974, Prout & Daran, 1978, Adam & Green, 1981). In those cases, the tetranuclear molybdenum dimers were prepared by reaction of the respective molybdocene dichloride, (η5-C5H4R)2MoCl2, and sodium molybdate. The structure of the [(η5-C5H4Me)2Mo2O4]2 was determined by single crystal diffraction methods (Prout & Daran, 1978). The central framework in this compound is similar to that found in the title compound.

Experimental

Ethyl acetate (7 ml) was added to an NMR tube containing [{C2Me455-C5H4)2}Mo(OH)(OH2)][C7H7SO3] (0.0023 mg, 0.0026 mmol) in 0.50 ml D2O. The mixture was allowed to react over two months at 323 K during which time the ethyl acetate was converted to ethanol and acetic acid. As the reaction proceeded, the mixture turned dark in color and crystalline needles of (I) suitable for X-ray analysis appeared on the NMR tube walls.

Refinement

The positions of the H atoms in solvent water molecules were found from the residual density and their positions were freely refined with isotropic thermal parameters. Other H atoms were positioned geometrically and refined in a rigid group model, C—H = 0.98 Å (C5-rings) and 0.96 Å (Me-groups); Uiso(H) = 1.2 and 1.5 Ueq(C), respectively.

Figures

Fig. 1.
The structure of the [{C2Me4(η5-C5H4)2}Mo2O4]2 unit in (I) with 50% probability displacement ellipsoids [Symmetry code (i): 1-x,1-y,-z]. The H atoms were omitted for clarity.
Fig. 2.
The network of H-bonds (dashed lines) in the structure of (I).

Crystal data

[Mo4(C16H20)2O8]·6H2OZ = 1
Mr = 1044.50F(000) = 524
Triclinic, P1Dx = 1.924 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.4106 (7) ÅCell parameters from 6153 reflections
b = 9.3518 (8) Åθ = 2.6–28.2°
c = 13.5735 (12) ŵ = 1.43 mm1
α = 93.365 (1)°T = 173 K
β = 98.604 (1)°Cut block, orange
γ = 103.175 (1)°0.30 × 0.09 × 0.07 mm
V = 901.39 (14) Å3

Data collection

Bruker APEX CCD diffractometer3916 independent reflections
Radiation source: fine-focus sealed tube3621 reflections with I > 2σ(I)
graphiteRint = 0.014
ω scansθmax = 27.0°, θmin = 1.5°
Absorption correction: multi-scan (SADABS; Bruker, 2000)h = −9→9
Tmin = 0.673, Tmax = 0.907k = −11→11
10175 measured reflectionsl = −17→17

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.021Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.054H atoms treated by a mixture of independent and constrained refinement
S = 1.09w = 1/[σ2(Fo2) + (0.0277P)2 + 0.6752P] where P = (Fo2 + 2Fc2)/3
3916 reflections(Δ/σ)max = 0.001
250 parametersΔρmax = 0.46 e Å3
0 restraintsΔρmin = −0.41 e Å3

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2sigma(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

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

xyzUiso*/Ueq
Mo10.29716 (2)0.241010 (19)0.116363 (13)0.01106 (6)
Mo20.40229 (2)0.365828 (19)−0.091484 (13)0.01260 (6)
O10.4426 (2)0.42724 (16)0.05904 (11)0.0143 (3)
O20.2879 (2)0.19918 (16)−0.03835 (11)0.0177 (3)
O30.2214 (2)0.40535 (18)−0.17230 (13)0.0252 (4)
O40.5547 (3)0.30518 (18)−0.15855 (14)0.0267 (4)
C10.3632 (3)0.0962 (2)0.23884 (16)0.0145 (4)
C20.3911 (3)0.0317 (2)0.14559 (16)0.0164 (4)
H2A0.3272−0.06960.11320.020*
C30.5455 (3)0.1302 (3)0.11548 (17)0.0184 (5)
H3B0.60360.11130.05560.022*
C40.6129 (3)0.2517 (3)0.18767 (17)0.0181 (5)
H4B0.72340.33560.18620.022*
C50.5003 (3)0.2357 (2)0.26298 (17)0.0171 (4)
H5A0.52050.30320.32560.021*
C60.0704 (3)0.2045 (2)0.21417 (16)0.0149 (4)
C7−0.0141 (3)0.1375 (2)0.11433 (16)0.0156 (4)
H7A−0.07990.03150.09510.019*
C8−0.0106 (3)0.2551 (3)0.05167 (17)0.0180 (5)
H8A−0.06620.2437−0.02100.022*
C90.0778 (3)0.3893 (3)0.10838 (18)0.0196 (5)
H9A0.09530.48890.08290.024*
C100.1328 (3)0.3613 (2)0.20837 (17)0.0172 (4)
H10A0.18810.43760.26630.021*
C110.2217 (3)0.0245 (2)0.30248 (16)0.0162 (4)
C120.0833 (3)0.1277 (2)0.31082 (16)0.0171 (4)
C130.3320 (4)0.0042 (3)0.40383 (18)0.0244 (5)
H13A0.4152−0.06100.39330.037*
H13B0.2439−0.03970.44710.037*
H13C0.40730.10030.43570.037*
C140.1182 (3)−0.1308 (2)0.25306 (18)0.0208 (5)
H14A0.2091−0.19160.24930.031*
H14B0.0551−0.12340.18540.031*
H14C0.0248−0.17630.29300.031*
C15−0.1156 (3)0.0416 (3)0.3224 (2)0.0258 (5)
H15A−0.19630.11060.32720.039*
H15B−0.1079−0.00980.38310.039*
H15C−0.1688−0.03060.26400.039*
C160.1514 (4)0.2459 (3)0.40115 (18)0.0265 (5)
H16A0.06050.30700.40290.040*
H16B0.27410.30810.39480.040*
H16C0.16300.19750.46310.040*
O1S0.8478 (3)0.5646 (2)0.37887 (16)0.0327 (4)
O2S0.4926 (4)0.6405 (3)0.36850 (19)0.0472 (6)
O3S0.2122 (3)0.6526 (2)0.48301 (17)0.0336 (4)
H1S0.843 (4)0.569 (3)0.319 (3)0.032 (9)*
H2S0.951 (6)0.596 (4)0.402 (3)0.051 (12)*
H3S0.592 (6)0.631 (5)0.380 (3)0.063 (14)*
H4S0.483 (5)0.668 (4)0.317 (3)0.047 (11)*
H5S0.219 (5)0.596 (4)0.526 (3)0.038 (9)*
H6S0.296 (5)0.646 (4)0.453 (3)0.041 (10)*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Mo10.00936 (9)0.01184 (10)0.01173 (10)0.00140 (7)0.00206 (7)0.00287 (7)
Mo20.01369 (10)0.01183 (10)0.01116 (10)0.00041 (7)0.00266 (7)0.00113 (7)
O10.0162 (8)0.0134 (7)0.0109 (7)−0.0019 (6)0.0029 (6)0.0023 (6)
O20.0212 (8)0.0147 (8)0.0137 (7)−0.0026 (6)0.0032 (6)0.0012 (6)
O30.0246 (9)0.0191 (8)0.0254 (9)−0.0005 (7)−0.0079 (7)0.0040 (7)
O40.0319 (10)0.0184 (8)0.0336 (10)0.0051 (7)0.0195 (8)0.0007 (7)
C10.0126 (10)0.0155 (10)0.0162 (10)0.0058 (8)0.0002 (8)0.0048 (8)
C20.0162 (11)0.0137 (10)0.0205 (11)0.0055 (8)0.0033 (9)0.0030 (8)
C30.0128 (10)0.0220 (11)0.0229 (12)0.0073 (9)0.0048 (9)0.0055 (9)
C40.0097 (10)0.0200 (11)0.0251 (12)0.0050 (8)0.0002 (8)0.0067 (9)
C50.0135 (10)0.0182 (11)0.0186 (11)0.0044 (8)−0.0023 (8)0.0032 (8)
C60.0113 (10)0.0169 (11)0.0185 (11)0.0049 (8)0.0058 (8)0.0037 (8)
C70.0090 (10)0.0208 (11)0.0176 (11)0.0030 (8)0.0034 (8)0.0052 (9)
C80.0098 (10)0.0252 (12)0.0201 (11)0.0053 (9)0.0013 (8)0.0084 (9)
C90.0144 (11)0.0204 (11)0.0286 (13)0.0089 (9)0.0071 (9)0.0111 (9)
C100.0139 (10)0.0160 (11)0.0231 (12)0.0051 (8)0.0055 (9)0.0022 (9)
C110.0165 (10)0.0175 (11)0.0150 (10)0.0039 (8)0.0031 (8)0.0058 (8)
C120.0200 (11)0.0195 (11)0.0141 (10)0.0060 (9)0.0062 (8)0.0055 (8)
C130.0262 (13)0.0291 (13)0.0189 (12)0.0083 (10)0.0011 (10)0.0098 (10)
C140.0210 (12)0.0158 (11)0.0251 (12)0.0010 (9)0.0063 (9)0.0052 (9)
C150.0217 (12)0.0334 (14)0.0283 (13)0.0103 (10)0.0125 (10)0.0153 (11)
C160.0353 (14)0.0311 (14)0.0162 (11)0.0124 (11)0.0072 (10)0.0015 (10)
O1S0.0298 (12)0.0441 (12)0.0231 (11)0.0051 (9)0.0032 (9)0.0115 (9)
O2S0.0370 (14)0.0829 (19)0.0293 (12)0.0235 (13)0.0123 (10)0.0135 (12)
O3S0.0328 (11)0.0361 (11)0.0341 (11)0.0074 (9)0.0109 (9)0.0124 (9)

Geometric parameters (Å, °)

Mo1—O12.0869 (14)C7—C81.428 (3)
Mo1—O22.1014 (15)C7—H7A1.0000
Mo1—C22.259 (2)C8—C91.399 (3)
Mo1—C62.272 (2)C8—H8A1.0000
Mo1—C12.272 (2)C9—C101.415 (3)
Mo1—C72.284 (2)C9—H9A1.0000
Mo1—C102.286 (2)C10—H10A1.0000
Mo1—C32.310 (2)C11—C131.537 (3)
Mo1—C52.319 (2)C11—C141.540 (3)
Mo1—C82.354 (2)C11—C121.572 (3)
Mo1—C92.360 (2)C12—C161.543 (3)
Mo1—C42.372 (2)C12—C151.545 (3)
Mo2—O41.7217 (16)C13—H13A0.9800
Mo2—O31.7237 (16)C13—H13B0.9800
Mo2—O21.8385 (15)C13—H13C0.9800
Mo2—O1i1.9986 (14)C14—H14A0.9800
Mo2—O12.0481 (15)C14—H14B0.9800
O1—Mo2i1.9985 (14)C14—H14C0.9800
C1—C21.433 (3)C15—H15A0.9800
C1—C51.445 (3)C15—H15B0.9800
C1—C111.521 (3)C15—H15C0.9800
C2—C31.424 (3)C16—H16A0.9800
C2—H2A1.0000C16—H16B0.9800
C3—C41.402 (3)C16—H16C0.9800
C3—H3B1.0000O1S—H1S0.82 (3)
C4—C51.407 (3)O1S—H2S0.76 (4)
C4—H4B1.0000O2S—H3S0.76 (4)
C5—H5A1.0000O2S—H4S0.76 (4)
C6—C101.444 (3)O3S—H5S0.81 (4)
C6—C71.445 (3)O3S—H6S0.80 (4)
C6—C121.533 (3)
O1—Mo1—O269.58 (6)C1—C2—H2A126.2
O1—Mo1—C2127.58 (7)Mo1—C2—H2A126.2
O2—Mo1—C291.12 (7)C4—C3—C2109.1 (2)
O1—Mo1—C6133.26 (7)C4—C3—Mo175.01 (13)
O2—Mo1—C6132.42 (7)C2—C3—Mo169.91 (12)
C2—Mo1—C696.13 (8)C4—C3—H3B125.3
O1—Mo1—C1136.34 (7)C2—C3—H3B125.3
O2—Mo1—C1127.87 (7)Mo1—C3—H3B125.3
C2—Mo1—C136.88 (8)C3—C4—C5108.7 (2)
C6—Mo1—C169.27 (8)C3—C4—Mo170.18 (12)
O1—Mo1—C7133.87 (7)C5—C4—Mo170.51 (12)
O2—Mo1—C795.63 (7)C3—C4—H4B125.6
C2—Mo1—C794.87 (8)C5—C4—H4B125.6
C6—Mo1—C736.99 (8)Mo1—C4—H4B125.6
C1—Mo1—C787.77 (8)C4—C5—C1107.6 (2)
O1—Mo1—C1096.48 (7)C4—C5—Mo174.60 (13)
O2—Mo1—C10132.96 (7)C1—C5—Mo169.88 (12)
C2—Mo1—C10128.54 (8)C4—C5—H5A126.0
C6—Mo1—C1036.95 (8)C1—C5—H5A126.0
C1—Mo1—C1093.79 (8)Mo1—C5—H5A126.0
C7—Mo1—C1061.30 (8)C10—C6—C7107.47 (19)
O1—Mo1—C391.40 (7)C10—C6—C12125.1 (2)
O2—Mo1—C379.28 (7)C7—C6—C12127.30 (19)
C2—Mo1—C336.30 (8)C10—C6—Mo172.04 (12)
C6—Mo1—C3128.90 (8)C7—C6—Mo171.97 (12)
C1—Mo1—C360.16 (8)C12—C6—Mo1124.10 (14)
C7—Mo1—C3129.81 (8)C8—C7—C6106.60 (19)
C10—Mo1—C3147.47 (8)C8—C7—Mo174.77 (12)
O1—Mo1—C5101.32 (7)C6—C7—Mo171.04 (12)
O2—Mo1—C5137.56 (7)C8—C7—H7A126.4
C2—Mo1—C560.90 (8)C6—C7—H7A126.4
C6—Mo1—C584.85 (8)Mo1—C7—H7A126.4
C1—Mo1—C536.67 (8)C9—C8—C7109.4 (2)
C7—Mo1—C5116.53 (8)C9—C8—Mo172.97 (12)
C10—Mo1—C588.38 (8)C7—C8—Mo169.42 (12)
C3—Mo1—C559.11 (8)C9—C8—H8A125.3
O1—Mo1—C898.21 (7)C7—C8—H8A125.3
O2—Mo1—C878.13 (7)Mo1—C8—H8A125.3
C2—Mo1—C8125.79 (8)C8—C9—C10108.8 (2)
C6—Mo1—C859.69 (8)C8—C9—Mo172.50 (13)
C1—Mo1—C8123.14 (8)C10—C9—Mo169.41 (12)
C7—Mo1—C835.81 (7)C8—C9—H9A125.6
C10—Mo1—C859.07 (8)C10—C9—H9A125.6
C3—Mo1—C8150.51 (8)Mo1—C9—H9A125.6
C5—Mo1—C8143.69 (8)C9—C10—C6107.6 (2)
O1—Mo1—C978.84 (7)C9—C10—Mo175.18 (13)
O2—Mo1—C997.77 (7)C6—C10—Mo171.01 (12)
C2—Mo1—C9153.50 (8)C9—C10—H10A125.9
C6—Mo1—C959.71 (8)C6—C10—H10A125.9
C1—Mo1—C9127.20 (8)Mo1—C10—H10A125.9
C7—Mo1—C959.55 (8)C1—C11—C13107.72 (18)
C10—Mo1—C935.41 (8)C1—C11—C14109.32 (18)
C3—Mo1—C9170.20 (8)C13—C11—C14106.88 (19)
C5—Mo1—C9121.75 (8)C1—C11—C12107.16 (17)
C8—Mo1—C934.53 (8)C13—C11—C12113.68 (19)
O1—Mo1—C478.20 (7)C14—C11—C12111.97 (18)
O2—Mo1—C4104.43 (7)C6—C12—C16109.04 (19)
C2—Mo1—C459.57 (8)C6—C12—C15109.10 (18)
C6—Mo1—C4119.70 (8)C16—C12—C15106.4 (2)
C1—Mo1—C459.39 (8)C6—C12—C11106.92 (17)
C7—Mo1—C4147.17 (8)C16—C12—C11112.75 (19)
C10—Mo1—C4116.66 (8)C15—C12—C11112.60 (19)
C3—Mo1—C434.82 (8)C11—C13—H13A109.5
C5—Mo1—C434.89 (8)C11—C13—H13B109.5
C8—Mo1—C4174.32 (8)H13A—C13—H13B109.5
C9—Mo1—C4139.82 (8)C11—C13—H13C109.5
O4—Mo2—O3109.85 (9)H13A—C13—H13C109.5
O4—Mo2—O2103.42 (8)H13B—C13—H13C109.5
O3—Mo2—O2103.62 (8)C11—C14—H14A109.5
O4—Mo2—O1i95.84 (7)C11—C14—H14B109.5
O3—Mo2—O1i97.04 (7)H14A—C14—H14B109.5
O2—Mo2—O1i144.73 (6)C11—C14—H14C109.5
O4—Mo2—O1127.83 (8)H14A—C14—H14C109.5
O3—Mo2—O1121.19 (8)H14B—C14—H14C109.5
O2—Mo2—O175.67 (6)C12—C15—H15A109.5
O1i—Mo2—O169.18 (7)C12—C15—H15B109.5
Mo2i—O1—Mo2110.82 (7)H15A—C15—H15B109.5
Mo2i—O1—Mo1145.59 (8)C12—C15—H15C109.5
Mo2—O1—Mo1103.59 (6)H15A—C15—H15C109.5
Mo2—O2—Mo1110.95 (7)H15B—C15—H15C109.5
C2—C1—C5107.47 (19)C12—C16—H16A109.5
C2—C1—C11125.40 (19)C12—C16—H16B109.5
C5—C1—C11127.0 (2)H16A—C16—H16B109.5
C2—C1—Mo171.08 (12)C12—C16—H16C109.5
C5—C1—Mo173.45 (12)H16A—C16—H16C109.5
C11—C1—Mo1123.64 (14)H16B—C16—H16C109.5
C3—C2—C1106.98 (19)H1S—O1S—H2S105 (3)
C3—C2—Mo173.79 (13)H3S—O2S—H4S106 (4)
C1—C2—Mo172.03 (12)H5S—O3S—H6S105 (3)
C3—C2—H2A126.2
O4—Mo2—O1—Mo2i80.94 (10)O2—Mo1—C5—C1−93.12 (14)
O3—Mo2—O1—Mo2i−85.59 (9)C2—Mo1—C5—C1−38.26 (12)
O2—Mo2—O1—Mo2i176.97 (9)C6—Mo1—C5—C161.70 (13)
O1i—Mo2—O1—Mo2i0.0C7—Mo1—C5—C141.99 (15)
O4—Mo2—O1—Mo1−99.53 (9)C10—Mo1—C5—C198.55 (13)
O3—Mo2—O1—Mo193.93 (9)C3—Mo1—C5—C1−80.37 (14)
O2—Mo2—O1—Mo1−3.51 (6)C8—Mo1—C5—C173.63 (18)
O1i—Mo2—O1—Mo1179.52 (12)C9—Mo1—C5—C1111.06 (13)
O2—Mo1—O1—Mo2i−177.62 (16)C4—Mo1—C5—C1−115.83 (19)
C2—Mo1—O1—Mo2i−102.69 (15)O1—Mo1—C6—C10−6.53 (17)
C6—Mo1—O1—Mo2i52.73 (18)O2—Mo1—C6—C10−108.72 (13)
C1—Mo1—O1—Mo2i−53.65 (19)C2—Mo1—C6—C10154.11 (13)
C7—Mo1—O1—Mo2i104.65 (15)C1—Mo1—C6—C10128.38 (14)
C10—Mo1—O1—Mo2i48.79 (15)C7—Mo1—C6—C10−115.94 (18)
C3—Mo1—O1—Mo2i−99.60 (15)C3—Mo1—C6—C10136.84 (13)
C5—Mo1—O1—Mo2i−40.86 (16)C5—Mo1—C6—C1094.17 (13)
C8—Mo1—O1—Mo2i108.37 (15)C8—Mo1—C6—C10−77.68 (14)
C9—Mo1—O1—Mo2i79.64 (15)C9—Mo1—C6—C10−37.48 (13)
C4—Mo1—O1—Mo2i−67.17 (15)C4—Mo1—C6—C1095.80 (14)
O2—Mo1—O1—Mo23.17 (6)O1—Mo1—C6—C7109.41 (13)
C2—Mo1—O1—Mo278.09 (10)O2—Mo1—C6—C77.22 (16)
C6—Mo1—O1—Mo2−126.48 (9)C2—Mo1—C6—C7−89.95 (13)
C1—Mo1—O1—Mo2127.14 (9)C1—Mo1—C6—C7−115.69 (14)
C7—Mo1—O1—Mo2−74.56 (11)C10—Mo1—C6—C7115.94 (18)
C10—Mo1—O1—Mo2−130.42 (8)C3—Mo1—C6—C7−107.22 (14)
C3—Mo1—O1—Mo281.19 (8)C5—Mo1—C6—C7−149.89 (13)
C5—Mo1—O1—Mo2139.93 (8)C8—Mo1—C6—C738.25 (12)
C8—Mo1—O1—Mo2−70.84 (8)C9—Mo1—C6—C778.46 (13)
C9—Mo1—O1—Mo2−99.57 (8)C4—Mo1—C6—C7−148.27 (12)
C4—Mo1—O1—Mo2113.62 (8)O1—Mo1—C6—C12−127.28 (16)
O4—Mo2—O2—Mo1129.77 (9)O2—Mo1—C6—C12130.54 (16)
O3—Mo2—O2—Mo1−115.59 (9)C2—Mo1—C6—C1233.37 (18)
O1i—Mo2—O2—Mo18.53 (16)C1—Mo1—C6—C127.63 (17)
O1—Mo2—O2—Mo13.62 (7)C7—Mo1—C6—C12123.3 (2)
O1—Mo1—O2—Mo2−3.68 (7)C10—Mo1—C6—C12−120.7 (2)
C2—Mo1—O2—Mo2−133.74 (9)C3—Mo1—C6—C1216.1 (2)
C6—Mo1—O2—Mo2126.90 (9)C5—Mo1—C6—C12−26.57 (18)
C1—Mo1—O2—Mo2−137.18 (9)C8—Mo1—C6—C12161.6 (2)
C7—Mo1—O2—Mo2131.26 (9)C9—Mo1—C6—C12−158.2 (2)
C10—Mo1—O2—Mo275.83 (12)C4—Mo1—C6—C12−24.9 (2)
C3—Mo1—O2—Mo2−99.24 (9)C10—C6—C7—C8−3.2 (2)
C5—Mo1—O2—Mo2−88.12 (12)C12—C6—C7—C8173.5 (2)
C8—Mo1—O2—Mo299.85 (9)Mo1—C6—C7—C8−66.90 (14)
C9—Mo1—O2—Mo271.29 (9)C10—C6—C7—Mo163.74 (14)
C4—Mo1—O2—Mo2−74.94 (9)C12—C6—C7—Mo1−119.5 (2)
O1—Mo1—C1—C2−94.33 (14)O1—Mo1—C7—C86.30 (17)
O2—Mo1—C1—C25.73 (16)O2—Mo1—C7—C8−60.66 (13)
C6—Mo1—C1—C2134.00 (14)C2—Mo1—C7—C8−152.27 (14)
C7—Mo1—C1—C2101.14 (13)C6—Mo1—C7—C8113.99 (19)
C10—Mo1—C1—C2162.19 (13)C1—Mo1—C7—C8171.50 (14)
C3—Mo1—C1—C2−38.41 (12)C10—Mo1—C7—C875.95 (14)
C5—Mo1—C1—C2−115.66 (18)C3—Mo1—C7—C8−141.40 (14)
C8—Mo1—C1—C2107.07 (14)C5—Mo1—C7—C8147.93 (13)
C9—Mo1—C1—C2149.37 (13)C9—Mo1—C7—C835.06 (13)
C4—Mo1—C1—C2−78.92 (13)C4—Mo1—C7—C8171.41 (14)
O1—Mo1—C1—C521.33 (17)O1—Mo1—C7—C6−107.69 (13)
O2—Mo1—C1—C5121.39 (13)O2—Mo1—C7—C6−174.65 (12)
C2—Mo1—C1—C5115.66 (18)C2—Mo1—C7—C693.74 (13)
C6—Mo1—C1—C5−110.34 (14)C1—Mo1—C7—C657.51 (13)
C7—Mo1—C1—C5−143.20 (13)C10—Mo1—C7—C6−38.04 (12)
C10—Mo1—C1—C5−82.16 (13)C3—Mo1—C7—C6104.61 (14)
C3—Mo1—C1—C577.25 (14)C5—Mo1—C7—C633.94 (15)
C8—Mo1—C1—C5−137.27 (13)C8—Mo1—C7—C6−113.99 (19)
C9—Mo1—C1—C5−94.98 (14)C9—Mo1—C7—C6−78.93 (13)
C4—Mo1—C1—C536.74 (12)C4—Mo1—C7—C657.4 (2)
O1—Mo1—C1—C11145.17 (15)C6—C7—C8—C92.0 (2)
O2—Mo1—C1—C11−114.77 (17)Mo1—C7—C8—C9−62.35 (16)
C2—Mo1—C1—C11−120.5 (2)C6—C7—C8—Mo164.37 (14)
C6—Mo1—C1—C1113.50 (16)O1—Mo1—C8—C9−56.30 (14)
C7—Mo1—C1—C11−19.36 (18)O2—Mo1—C8—C9−123.32 (14)
C10—Mo1—C1—C1141.68 (18)C2—Mo1—C8—C9153.97 (13)
C3—Mo1—C1—C11−158.9 (2)C6—Mo1—C8—C979.57 (14)
C5—Mo1—C1—C11123.8 (2)C1—Mo1—C8—C9108.95 (14)
C8—Mo1—C1—C11−13.4 (2)C7—Mo1—C8—C9119.12 (19)
C9—Mo1—C1—C1128.9 (2)C10—Mo1—C8—C936.36 (13)
C4—Mo1—C1—C11160.6 (2)C3—Mo1—C8—C9−164.06 (15)
C5—C1—C2—C31.1 (2)C5—Mo1—C8—C965.78 (19)
C11—C1—C2—C3−175.59 (19)O1—Mo1—C8—C7−175.42 (13)
Mo1—C1—C2—C366.06 (15)O2—Mo1—C8—C7117.57 (13)
C5—C1—C2—Mo1−64.94 (14)C2—Mo1—C8—C734.86 (17)
C11—C1—C2—Mo1118.4 (2)C6—Mo1—C8—C7−39.55 (13)
O1—Mo1—C2—C35.24 (16)C1—Mo1—C8—C7−10.16 (17)
O2—Mo1—C2—C370.07 (13)C10—Mo1—C8—C7−82.75 (14)
C6—Mo1—C2—C3−157.03 (13)C3—Mo1—C8—C776.8 (2)
C1—Mo1—C2—C3−114.45 (19)C5—Mo1—C8—C7−53.3 (2)
C7—Mo1—C2—C3165.83 (14)C9—Mo1—C8—C7−119.12 (19)
C10—Mo1—C2—C3−137.42 (13)C7—C8—C9—C10−0.1 (3)
C5—Mo1—C2—C3−76.42 (14)Mo1—C8—C9—C10−60.21 (15)
C8—Mo1—C2—C3146.22 (13)C7—C8—C9—Mo160.14 (15)
C9—Mo1—C2—C3−179.91 (17)O1—Mo1—C9—C8122.93 (14)
C4—Mo1—C2—C3−36.04 (13)O2—Mo1—C9—C855.62 (13)
O1—Mo1—C2—C1119.69 (12)C2—Mo1—C9—C8−52.9 (2)
O2—Mo1—C2—C1−175.47 (12)C6—Mo1—C9—C8−79.51 (14)
C6—Mo1—C2—C1−42.58 (13)C1—Mo1—C9—C8−96.18 (15)
C7—Mo1—C2—C1−79.72 (13)C7—Mo1—C9—C8−36.36 (13)
C10—Mo1—C2—C1−22.97 (16)C10—Mo1—C9—C8−118.64 (19)
C3—Mo1—C2—C1114.45 (19)C5—Mo1—C9—C8−140.58 (13)
C5—Mo1—C2—C138.03 (12)C4—Mo1—C9—C8179.09 (13)
C8—Mo1—C2—C1−99.33 (14)O1—Mo1—C9—C10−118.43 (13)
C9—Mo1—C2—C1−65.5 (2)O2—Mo1—C9—C10174.27 (13)
C4—Mo1—C2—C178.41 (13)C2—Mo1—C9—C1065.7 (2)
C1—C2—C3—C40.4 (2)C6—Mo1—C9—C1039.13 (13)
Mo1—C2—C3—C465.27 (16)C1—Mo1—C9—C1022.46 (17)
C1—C2—C3—Mo1−64.87 (14)C7—Mo1—C9—C1082.28 (14)
O1—Mo1—C3—C466.83 (13)C5—Mo1—C9—C10−21.94 (16)
O2—Mo1—C3—C4135.74 (14)C8—Mo1—C9—C10118.64 (19)
C2—Mo1—C3—C4−117.32 (19)C4—Mo1—C9—C10−62.27 (18)
C6—Mo1—C3—C4−87.41 (15)C8—C9—C10—C6−1.9 (2)
C1—Mo1—C3—C4−78.28 (14)Mo1—C9—C10—C6−64.08 (14)
C7—Mo1—C3—C4−135.84 (13)C8—C9—C10—Mo162.15 (16)
C10—Mo1—C3—C4−37.5 (2)C7—C6—C10—C93.2 (2)
C5—Mo1—C3—C4−35.54 (13)C12—C6—C10—C9−173.64 (19)
C8—Mo1—C3—C4176.29 (14)Mo1—C6—C10—C966.86 (15)
O1—Mo1—C3—C2−175.85 (13)C7—C6—C10—Mo1−63.70 (14)
O2—Mo1—C3—C2−106.93 (13)C12—C6—C10—Mo1119.5 (2)
C6—Mo1—C3—C229.91 (17)O1—Mo1—C10—C960.26 (13)
C1—Mo1—C3—C239.04 (13)O2—Mo1—C10—C9−7.77 (17)
C7—Mo1—C3—C2−18.52 (17)C2—Mo1—C10—C9−148.67 (13)
C10—Mo1—C3—C279.78 (19)C6—Mo1—C10—C9−114.96 (19)
C5—Mo1—C3—C281.79 (14)C1—Mo1—C10—C9−162.24 (13)
C8—Mo1—C3—C2−66.4 (2)C7—Mo1—C10—C9−76.87 (14)
C4—Mo1—C3—C2117.32 (19)C3—Mo1—C10—C9163.19 (15)
C2—C3—C4—C5−1.8 (3)C5—Mo1—C10—C9161.47 (14)
Mo1—C3—C4—C560.21 (15)C8—Mo1—C10—C9−35.44 (13)
C2—C3—C4—Mo1−62.02 (15)C4—Mo1—C10—C9140.28 (13)
O1—Mo1—C4—C3−110.13 (14)O1—Mo1—C10—C6175.22 (12)
O2—Mo1—C4—C3−45.07 (14)O2—Mo1—C10—C6107.18 (13)
C2—Mo1—C4—C337.59 (13)C2—Mo1—C10—C6−33.71 (16)
C6—Mo1—C4—C3116.49 (14)C1—Mo1—C10—C6−47.29 (13)
C1—Mo1—C4—C380.68 (14)C7—Mo1—C10—C638.08 (12)
C7—Mo1—C4—C380.78 (19)C3—Mo1—C10—C6−81.86 (19)
C10—Mo1—C4—C3158.49 (13)C5—Mo1—C10—C6−83.57 (13)
C5—Mo1—C4—C3119.3 (2)C8—Mo1—C10—C679.51 (14)
C9—Mo1—C4—C3−166.48 (13)C9—Mo1—C10—C6114.96 (19)
O1—Mo1—C4—C5130.55 (14)C4—Mo1—C10—C6−104.76 (13)
O2—Mo1—C4—C5−164.39 (12)C2—C1—C11—C13117.9 (2)
C2—Mo1—C4—C5−81.73 (14)C5—C1—C11—C13−58.1 (3)
C6—Mo1—C4—C5−2.83 (16)Mo1—C1—C11—C13−152.36 (16)
C1—Mo1—C4—C5−38.64 (13)C2—C1—C11—C142.1 (3)
C7—Mo1—C4—C5−38.5 (2)C5—C1—C11—C14−173.9 (2)
C10—Mo1—C4—C539.17 (15)Mo1—C1—C11—C1491.9 (2)
C3—Mo1—C4—C5−119.3 (2)C2—C1—C11—C12−119.4 (2)
C9—Mo1—C4—C574.20 (17)C5—C1—C11—C1264.5 (3)
C3—C4—C5—C12.5 (2)Mo1—C1—C11—C12−29.7 (2)
Mo1—C4—C5—C162.48 (14)C10—C6—C12—C166.5 (3)
C3—C4—C5—Mo1−60.01 (15)C7—C6—C12—C16−169.6 (2)
C2—C1—C5—C4−2.2 (2)Mo1—C6—C12—C1697.7 (2)
C11—C1—C5—C4174.4 (2)C10—C6—C12—C15122.3 (2)
Mo1—C1—C5—C4−65.59 (15)C7—C6—C12—C15−53.8 (3)
C2—C1—C5—Mo163.38 (14)Mo1—C6—C12—C15−146.47 (17)
C11—C1—C5—Mo1−120.0 (2)C10—C6—C12—C11−115.6 (2)
O1—Mo1—C5—C4−49.33 (14)C7—C6—C12—C1168.2 (3)
O2—Mo1—C5—C422.71 (18)Mo1—C6—C12—C11−24.4 (2)
C2—Mo1—C5—C477.57 (14)C1—C11—C12—C630.3 (2)
C6—Mo1—C5—C4177.53 (14)C13—C11—C12—C6149.24 (19)
C1—Mo1—C5—C4115.83 (19)C14—C11—C12—C6−89.5 (2)
C7—Mo1—C5—C4157.82 (13)C1—C11—C12—C16−89.5 (2)
C10—Mo1—C5—C4−145.62 (14)C13—C11—C12—C1629.4 (3)
C3—Mo1—C5—C435.46 (13)C14—C11—C12—C16150.66 (19)
C8—Mo1—C5—C4−170.54 (13)C1—C11—C12—C15150.16 (19)
C9—Mo1—C5—C4−133.11 (13)C13—C11—C12—C15−91.0 (2)
O1—Mo1—C5—C1−165.16 (12)C14—C11—C12—C1530.3 (3)

Symmetry codes: (i) −x+1, −y+1, −z.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O1S—H2S···O3Sii0.76 (4)2.02 (4)2.771 (3)169 (4)
O3S—H6S···O2S0.80 (4)1.99 (4)2.792 (3)175 (3)
O2S—H4S···O4i0.76 (4)2.16 (4)2.908 (3)167 (4)
O3S—H5S···O1Siii0.81 (4)2.06 (4)2.850 (3)163 (3)
O2S—H3S···O1S0.76 (4)2.12 (4)2.865 (3)165 (4)
O1S—H1S···O3i0.82 (3)2.01 (3)2.816 (3)167 (3)

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

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HB2806).

References

  • Adam, G. J. S. & Green, M. L. H. (1981). J. Organomet. Chem.208, 299–308.
  • Ahmed, T. J., Zakharov, L. N. & Tyler, D. R. (2007). Organometallics, 26, 5179–5187.
  • Bruker (2000). SMART, SAINT and SADABS Bruker AXS Inc., Madison, Wisconsin, USA.
  • Daran, J. C., Prout, K., Adam, G. J. S., Green, M. L. H. & Sala-Pala, J. (1977). J. Organomet. Chem.131, C40–C42.
  • Prout, K., Cameron, T. S., Forder, R. A., Critchley, S. R., Denton, B. & Rees, G. V. (1974). Acta Cryst. B30, 2290–2304.
  • Prout, K. & Daran, J.-C. (1978). Acta Cryst. B34, 3586–3591.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]

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