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Acta Cryst. (2009). E65, m1545    [ doi:10.1107/S1600536809046327 ]

Tetracarbonylbis([eta]5-cyclopentadienyl)bis[(dec-9-en-1-yl)diphenylphosphine]dimolybdenum(0)(Mo-Mo) tetrahydrofuran disolvate

G. Shultz, L. N. Zakharov and D. R. Tyler

Abstract top

The asymmetric unit of the title compound, [Mo2([eta]5-C5H5)2(C22H29P)2(CO)4]·2C4H8O, contains two half-molecules of the organometallic species and two solvent molecules. Both organometallic molecules are completed by crystallographic inversion symmetry, yielding dimeric units with Mo-Mo single-bond lengths of 3.2703 (6) and 3.2548 (6) Å. Each Mo atom is also coordinated by an [eta]5-cyclopentdienyl ligand, two carbonyl ligands, and a (dec-9-en-1-yl)diphenylphosphine ligand.

Comment top

In an on-going mechanistic study in our lab we have examined the effects of external parameters, such as mechanical stress (Chen et al., 2004) and temperature (Daglen et al., 2007), on the rate and onset of polymer degradation using polymers with metal-metal bonds in the main chain. Such polymers are synthesized from functionalized dimeric metal carbonyl complexes. Recently, we examined ADMET, Acyclic Diene Metathesis Polymerization, as a method for preparing polymers with metal-metal bonds, using phosphine-substituted dimeric molybdenum complexes as precursors (Shultz et al., 2008). Specifically the title complex was synthesized for polymerization by ADMET and purification of this complex yielded single crystals.

The structure of complex 1 reported here consists of two centrosymmetrical units [(η5-C5H5)Mo(CO)2(Ph2P(CH2)8CH=CH2)]2 (where Cp is cyclopentadienyl) and two solvent (C4H8O) molecules. In each unit the Mo atom is coordinated by a Cp moiety, two carbonyl groups and a Ph2P(CH2)8CH=CH2 ligand in a piano-stool fashion and bonded by a Mo—Mo bond as well (Fig. 1). The Mo—Mo bond lengths in 1, 3.2703 (6) and 3.2548 (6) Å, are within the range of single Mo—Mo bond lengths observed in other relevant dimeric molybdenum complexes such as [(η5-C5H5)Mo(CO)2]2 (Wilson & Shoemaker, 1957) and [MoCp(CO)2(Ph2P(CH2)6CH=CH2)]2 (Shultz et al., 2008).

Related literature top

For related literature from our group in this area, see: Chen et al. (2004); Daglen et al. (2007); For other compounds containing Mo—Mo single bonds, see: Wilson & Shoemaker (1957); Shultz et al. (2008).

Experimental top

The synthesis of the title compound was carried out under rigorous light and air free conditions. A solution of Cp2Mo2(CO)4 (408.15 mg, 0.94 mmol) in CH2Cl2 (10 ml) was treated with a solution of Ph2P(CH2)8CH=CH2 (481.84 mg, 1.88 mmol) in CH2Cl2 (10 ml) by adding dropwise while stirring. Red plates of (I) were obtained by cooling a solution of the complex in THF/CH2Cl2/hexanes.

Refinement top

The H atoms were positioned geometrically and refined with riding or rigid group models: C—H = 1.00 (Cp-ring), 0.95 (Ph-rings) and 0.99 (CH2 groups) Å; Uiso(H) = 1.2Ueq(C).

Computing details top

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

Figures top
[Figure 1] Fig. 1. The structure of the Mo1 molecule of (I) with 50% probability displacement ellipsoids Symmetry code (i): -x,-y,-z].
Tetracarbonylbis(η5-cyclopentadienyl)bis[(dec-9-en-1- yl)diphenylphosphine]dimolybdenum(0)(Mo—Mo) tetrahydrofuran disolvate top
Crystal data top
[Mo2(C5H5)2(C22H29P)2(CO)4]·2C4H8OZ = 2
Mr = 1227.16F(000) = 1284
Triclinic, P1Dx = 1.363 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 11.2755 (4) ÅCell parameters from 6981 reflections
b = 15.5660 (5) Åθ = 2.3–24.5°
c = 18.8566 (6) ŵ = 0.52 mm−1
α = 109.166 (1)°T = 173 K
β = 98.008 (1)°Plate, red
γ = 101.323 (1)°0.21 × 0.12 × 0.02 mm
V = 2990.20 (17) Å3
Data collection top
Bruker APEX CCD area-detector
diffractometer		12955 independent reflections
Radiation source: fine-focus sealed tube10237 reflections with I > 2σ(I)
graphiteRint = 0.036
φ and ω scansθmax = 27.0°, θmin = 1.2°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)		h = −14→14
Tmin = 0.898, Tmax = 0.990k = −19→19
33790 measured reflectionsl = −24→24
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.047Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.121H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0507P)2 + 2.7213P]
where P = (Fo2 + 2Fc2)/3
12955 reflections(Δ/σ)max = 0.001
686 parametersΔρmax = 0.73 e Å−3
0 restraintsΔρmin = −0.68 e Å−3
Crystal data top
[Mo2(C5H5)2(C22H29P)2(CO)4]·2C4H8Oγ = 101.323 (1)°
Mr = 1227.16V = 2990.20 (17) Å3
Triclinic, P1Z = 2
a = 11.2755 (4) ÅMo Kα radiation
b = 15.5660 (5) ŵ = 0.52 mm−1
c = 18.8566 (6) ÅT = 173 K
α = 109.166 (1)°0.21 × 0.12 × 0.02 mm
β = 98.008 (1)°
Data collection top
Bruker APEX CCD area-detector
diffractometer		12955 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2000)		10237 reflections with I > 2σ(I)
Tmin = 0.898, Tmax = 0.990Rint = 0.036
33790 measured reflectionsθmax = 27.0°
Refinement top
R[F2 > 2σ(F2)] = 0.047H-atom parameters constrained
wR(F2) = 0.121Δρmax = 0.73 e Å−3
S = 1.05Δρmin = −0.68 e Å−3
12955 reflectionsAbsolute structure: ?
686 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
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.

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 > σ(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) top
xyzUiso*/Ueq
Mo10.04404 (3)0.54395 (2)0.093859 (16)0.02578 (8)
P10.09180 (8)0.70546 (6)0.18453 (5)0.0290 (2)
O1−0.1968 (2)0.60007 (19)0.04523 (15)0.0399 (6)
O20.2526 (2)0.64265 (19)0.03326 (16)0.0458 (7)
C10.0195 (4)0.3859 (3)0.0856 (2)0.0397 (9)
H1A−0.01250.32880.03730.048*
C2−0.0525 (4)0.4267 (3)0.1359 (3)0.0484 (11)
H2A−0.14370.40310.13030.058*
C30.0289 (4)0.5008 (3)0.1992 (2)0.0469 (11)
H3A0.00560.53800.24700.056*
C40.1508 (4)0.5050 (3)0.1885 (2)0.0414 (9)
H4A0.22840.54570.22720.050*
C50.1446 (4)0.4336 (3)0.1179 (2)0.0387 (9)
H5A0.21690.41600.09720.046*
C6−0.1050 (3)0.5791 (2)0.05908 (19)0.0310 (8)
C70.1711 (3)0.6050 (2)0.0525 (2)0.0342 (8)
C80.2490 (3)0.7483 (3)0.2454 (2)0.0358 (8)
C90.3483 (4)0.7917 (3)0.2219 (3)0.0482 (10)
H9A0.33380.80520.17640.058*
C100.4679 (4)0.8150 (4)0.2647 (3)0.0682 (15)
H10A0.53510.84560.24900.082*
C110.4899 (5)0.7941 (4)0.3301 (3)0.0768 (18)
H11A0.57250.80850.35840.092*
C120.3935 (5)0.7526 (4)0.3544 (3)0.0648 (14)
H12A0.40920.73940.40000.078*
C130.2728 (4)0.7296 (3)0.3127 (2)0.0468 (10)
H13A0.20610.70100.33010.056*
C14−0.0038 (3)0.7368 (3)0.2558 (2)0.0321 (8)
C15−0.1242 (3)0.6820 (3)0.2424 (2)0.0370 (8)
H15A−0.15570.62780.19660.044*
C16−0.1987 (4)0.7050 (3)0.2947 (2)0.0465 (10)
H16A−0.28060.66690.28470.056*
C17−0.1528 (4)0.7838 (3)0.3612 (2)0.0512 (11)
H17A−0.20320.79950.39750.061*
C18−0.0355 (4)0.8395 (3)0.3754 (2)0.0484 (10)
H18A−0.00530.89410.42110.058*
C190.0400 (4)0.8165 (3)0.3232 (2)0.0402 (9)
H19A0.12160.85520.33360.048*
C200.0808 (4)0.7893 (3)0.1360 (2)0.0384 (9)
H20A0.14100.78400.10220.046*
H20B−0.00280.76740.10180.046*
C210.1017 (4)0.8945 (3)0.1826 (2)0.0427 (9)
H21A0.04580.90280.21900.051*
H21B0.18830.92120.21270.051*
C220.0760 (4)0.9465 (3)0.1282 (3)0.0480 (10)
H22A0.13810.94290.09570.058*
H22B−0.00670.91350.09360.058*
C230.0792 (4)1.0484 (3)0.1679 (3)0.0509 (11)
H23A0.16381.08350.19890.061*
H23B0.02141.05330.20320.061*
C240.0424 (5)1.0919 (3)0.1088 (3)0.0571 (12)
H24A0.09901.08390.07280.069*
H24B−0.04231.05600.07850.069*
C250.0446 (5)1.1941 (3)0.1412 (3)0.0684 (14)
H25A0.02251.21470.09790.082*
H25B0.13041.23050.16890.082*
C26−0.0423 (6)1.2185 (4)0.1961 (4)0.0849 (18)
H26A−0.01511.20390.24200.102*
H26B−0.03431.28720.21340.102*
C27−0.1782 (7)1.1669 (4)0.1614 (4)0.093 (2)
H27A−0.18691.09860.14810.111*
H27B−0.22641.18680.20120.111*
C28−0.2335 (6)1.1819 (5)0.0925 (5)0.098 (2)
H28A−0.23491.24490.09930.117*
C29−0.2788 (7)1.1222 (6)0.0261 (5)0.123 (3)
H29A−0.28021.05800.01560.147*
H29B−0.31191.1411−0.01380.147*
Mo20.45151 (3)0.43825 (2)0.408367 (16)0.02669 (9)
P20.56343 (9)0.39119 (7)0.30767 (5)0.0320 (2)
O30.6040 (3)0.63647 (19)0.42382 (15)0.0410 (6)
O40.6224 (3)0.33879 (19)0.48002 (15)0.0445 (7)
C300.2469 (3)0.4366 (3)0.4266 (2)0.0375 (9)
H30A0.22490.47540.47430.045*
C310.2578 (3)0.4615 (3)0.3621 (2)0.0359 (8)
H31A0.24380.52020.35550.043*
C320.2811 (3)0.3847 (3)0.3056 (2)0.0345 (8)
H32A0.28410.37900.25160.041*
C330.2825 (3)0.3122 (3)0.3353 (2)0.0369 (8)
H33A0.28620.24680.30580.044*
C340.2619 (3)0.3446 (3)0.4103 (2)0.0380 (9)
H34A0.25010.30660.44360.046*
C350.5534 (3)0.5630 (3)0.42241 (19)0.0321 (8)
C360.5626 (3)0.3807 (3)0.4562 (2)0.0338 (8)
C370.5122 (4)0.2638 (3)0.2506 (2)0.0400 (9)
C380.5452 (4)0.2006 (3)0.2828 (3)0.0498 (10)
H38A0.59830.22420.33260.060*
C390.5025 (5)0.1046 (3)0.2441 (3)0.0601 (12)
H39A0.52580.06270.26710.072*
C400.4258 (5)0.0696 (3)0.1717 (3)0.0648 (14)
H40A0.39770.00350.14450.078*
C410.3899 (5)0.1303 (4)0.1389 (3)0.0648 (13)
H41A0.33600.10600.08940.078*
C420.4330 (4)0.2275 (3)0.1786 (2)0.0506 (11)
H42A0.40770.26910.15600.061*
C430.5537 (3)0.4431 (3)0.2330 (2)0.0339 (8)
C440.4886 (3)0.5112 (3)0.2358 (2)0.0376 (9)
H44A0.44810.53110.27700.045*
C450.4819 (4)0.5503 (3)0.1794 (2)0.0433 (9)
H45A0.43640.59600.18180.052*
C460.5419 (4)0.5224 (3)0.1198 (2)0.0500 (11)
H46A0.53770.54900.08110.060*
C470.6075 (4)0.4562 (3)0.1167 (2)0.0507 (11)
H47A0.64890.43740.07590.061*
C480.6136 (4)0.4167 (3)0.1725 (2)0.0438 (10)
H48A0.65940.37090.16950.053*
C490.7325 (3)0.4054 (3)0.3349 (2)0.0412 (9)
H49A0.74810.37800.37470.049*
H49B0.75970.36870.28920.049*
C500.8117 (3)0.5060 (3)0.3651 (2)0.0393 (9)
H50A0.78350.54410.40970.047*
H50B0.80100.53300.32460.047*
C510.9497 (4)0.5115 (3)0.3899 (2)0.0470 (10)
H51A0.95960.48550.43110.056*
H51B0.97610.47130.34550.056*
C521.0339 (4)0.6096 (3)0.4185 (2)0.0510 (11)
H52A1.01870.63710.37870.061*
H52B1.12080.60500.42440.061*
C531.0201 (5)0.6769 (3)0.4941 (2)0.0567 (12)
H53A1.02200.64570.53210.068*
H53B0.93810.69040.48620.068*
C541.1215 (4)0.7710 (4)0.5275 (3)0.0605 (12)
H54A1.20360.75700.53190.073*
H54B1.11600.80380.49070.073*
C551.1147 (6)0.8347 (4)0.6027 (3)0.0864 (18)
H55A1.12500.80300.64000.104*
H55B1.03060.84520.59890.104*
C561.2094 (5)0.9304 (4)0.6348 (3)0.0793 (16)
H56A1.29190.92070.62790.095*
H56B1.18720.96840.60460.095*
C571.2186 (7)0.9840 (5)0.7170 (5)0.114 (2)
H57A1.24610.95480.75090.137*
C581.1963 (6)1.0619 (5)0.7500 (5)0.103 (2)
H58A1.16841.09600.72040.124*
H58B1.20741.08650.80440.124*
O1S1.2824 (4)1.1169 (3)0.9547 (3)0.1031 (15)
O2S0.2211 (5)0.0400 (4)0.4745 (3)0.1144 (16)
C1S1.4026 (6)1.1116 (5)0.9393 (5)0.108 (2)
H1SA1.39571.07210.88490.130*
H1SB1.44611.08510.97300.130*
C2S1.4673 (8)1.2091 (6)0.9558 (7)0.166 (4)
H2SA1.52251.23621.00770.199*
H2SB1.51841.21240.91770.199*
C3S1.3780 (7)1.2588 (5)0.9520 (6)0.141 (4)
H3SA1.35551.25970.89960.170*
H3SB1.40891.32450.98920.170*
C4S1.2724 (7)1.2088 (5)0.9713 (5)0.112 (3)
H4SA1.27311.23871.02650.135*
H4SB1.19411.20930.94050.135*
C5S0.3311 (7)0.0087 (5)0.4703 (4)0.094 (2)
H5SA0.3108−0.06080.45240.112*
H5SB0.38780.03490.52170.112*
C6S0.3910 (8)0.0415 (6)0.4155 (5)0.134 (3)
H6SA0.48170.06670.43560.160*
H6SB0.3748−0.01020.36490.160*
C7S0.3325 (8)0.1159 (6)0.4095 (6)0.134 (3)
H7SA0.38400.17840.44550.161*
H7SB0.32150.11590.35650.161*
C8S0.2144 (8)0.0944 (5)0.4292 (5)0.112 (2)
H8SA0.19380.15330.45780.134*
H8SB0.14870.05940.38180.134*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.02704 (16)0.02878 (16)0.02517 (16)0.00944 (12)0.00681 (12)0.01285 (12)
P10.0259 (5)0.0319 (5)0.0303 (5)0.0083 (4)0.0075 (4)0.0119 (4)
O10.0352 (15)0.0501 (16)0.0402 (15)0.0230 (13)0.0103 (12)0.0164 (13)
O20.0375 (16)0.0449 (16)0.0477 (17)−0.0013 (12)0.0208 (13)0.0097 (13)
C10.052 (2)0.032 (2)0.041 (2)0.0110 (17)0.0059 (19)0.0223 (17)
C20.051 (3)0.051 (3)0.063 (3)0.016 (2)0.024 (2)0.042 (2)
C30.075 (3)0.054 (3)0.033 (2)0.032 (2)0.024 (2)0.029 (2)
C40.054 (3)0.045 (2)0.031 (2)0.0215 (19)0.0014 (18)0.0179 (18)
C50.049 (2)0.041 (2)0.035 (2)0.0221 (18)0.0083 (18)0.0190 (17)
C60.036 (2)0.0311 (18)0.0272 (18)0.0095 (15)0.0096 (15)0.0110 (15)
C70.036 (2)0.0320 (19)0.0325 (19)0.0120 (16)0.0086 (16)0.0073 (16)
C80.0289 (19)0.0342 (19)0.036 (2)0.0102 (15)0.0033 (16)0.0023 (16)
C90.031 (2)0.045 (2)0.056 (3)0.0042 (18)0.0104 (19)0.006 (2)
C100.027 (2)0.063 (3)0.084 (4)0.001 (2)0.010 (2)−0.006 (3)
C110.036 (3)0.078 (4)0.078 (4)0.022 (3)−0.016 (3)−0.014 (3)
C120.058 (3)0.070 (3)0.050 (3)0.033 (3)−0.011 (2)0.001 (2)
C130.042 (2)0.048 (2)0.042 (2)0.0159 (19)−0.0003 (19)0.0067 (19)
C140.0303 (19)0.038 (2)0.0318 (19)0.0126 (15)0.0102 (15)0.0134 (16)
C150.034 (2)0.042 (2)0.033 (2)0.0099 (17)0.0072 (16)0.0115 (17)
C160.034 (2)0.060 (3)0.048 (2)0.0125 (19)0.0172 (19)0.021 (2)
C170.047 (3)0.072 (3)0.043 (2)0.028 (2)0.022 (2)0.021 (2)
C180.053 (3)0.053 (3)0.036 (2)0.021 (2)0.011 (2)0.0071 (19)
C190.039 (2)0.044 (2)0.035 (2)0.0117 (18)0.0091 (17)0.0103 (18)
C200.043 (2)0.037 (2)0.039 (2)0.0092 (17)0.0126 (18)0.0180 (17)
C210.050 (2)0.037 (2)0.045 (2)0.0163 (18)0.0132 (19)0.0157 (18)
C220.055 (3)0.039 (2)0.054 (3)0.0134 (19)0.012 (2)0.020 (2)
C230.058 (3)0.044 (2)0.053 (3)0.016 (2)0.012 (2)0.019 (2)
C240.069 (3)0.051 (3)0.062 (3)0.021 (2)0.018 (2)0.030 (2)
C250.081 (4)0.042 (3)0.076 (4)0.011 (2)0.003 (3)0.021 (3)
C260.124 (6)0.059 (3)0.082 (4)0.042 (4)0.032 (4)0.025 (3)
C270.110 (6)0.073 (4)0.114 (5)0.036 (4)0.059 (5)0.038 (4)
C280.073 (4)0.058 (4)0.153 (7)0.017 (3)0.017 (5)0.030 (4)
C290.101 (6)0.087 (5)0.145 (8)0.002 (4)0.008 (5)0.019 (5)
Mo20.02711 (16)0.03345 (17)0.02372 (16)0.01178 (13)0.01064 (12)0.01154 (13)
P20.0309 (5)0.0419 (5)0.0283 (5)0.0147 (4)0.0135 (4)0.0134 (4)
O30.0474 (16)0.0424 (16)0.0367 (15)0.0090 (13)0.0122 (12)0.0193 (13)
O40.0522 (17)0.0517 (17)0.0413 (16)0.0313 (14)0.0126 (13)0.0207 (13)
C300.0276 (19)0.052 (2)0.033 (2)0.0126 (17)0.0131 (16)0.0122 (18)
C310.0265 (18)0.046 (2)0.038 (2)0.0133 (16)0.0075 (16)0.0163 (17)
C320.0277 (18)0.046 (2)0.0279 (18)0.0082 (16)0.0044 (15)0.0122 (16)
C330.032 (2)0.038 (2)0.035 (2)0.0054 (16)0.0081 (16)0.0088 (17)
C340.0289 (19)0.049 (2)0.038 (2)0.0052 (17)0.0108 (16)0.0203 (18)
C350.035 (2)0.043 (2)0.0249 (18)0.0181 (17)0.0115 (15)0.0145 (16)
C360.037 (2)0.037 (2)0.0283 (18)0.0103 (16)0.0130 (16)0.0104 (16)
C370.039 (2)0.043 (2)0.042 (2)0.0165 (18)0.0207 (18)0.0120 (18)
C380.055 (3)0.046 (2)0.053 (3)0.022 (2)0.017 (2)0.016 (2)
C390.062 (3)0.049 (3)0.070 (3)0.021 (2)0.019 (3)0.018 (2)
C400.064 (3)0.045 (3)0.078 (4)0.015 (2)0.023 (3)0.010 (3)
C410.065 (3)0.061 (3)0.054 (3)0.009 (3)0.012 (2)0.007 (2)
C420.053 (3)0.050 (3)0.044 (2)0.013 (2)0.012 (2)0.011 (2)
C430.0316 (19)0.045 (2)0.0259 (18)0.0083 (16)0.0109 (15)0.0133 (16)
C440.037 (2)0.047 (2)0.0292 (19)0.0091 (17)0.0119 (16)0.0142 (17)
C450.043 (2)0.049 (2)0.039 (2)0.0077 (19)0.0082 (18)0.0195 (19)
C460.056 (3)0.061 (3)0.034 (2)0.004 (2)0.011 (2)0.024 (2)
C470.054 (3)0.064 (3)0.036 (2)0.010 (2)0.025 (2)0.017 (2)
C480.045 (2)0.053 (2)0.037 (2)0.0144 (19)0.0208 (19)0.0156 (19)
C490.037 (2)0.059 (3)0.038 (2)0.0244 (19)0.0189 (18)0.0216 (19)
C500.036 (2)0.055 (2)0.036 (2)0.0182 (18)0.0130 (17)0.0222 (19)
C510.043 (2)0.063 (3)0.043 (2)0.023 (2)0.0136 (19)0.022 (2)
C520.038 (2)0.069 (3)0.047 (3)0.019 (2)0.014 (2)0.018 (2)
C530.067 (3)0.066 (3)0.043 (3)0.020 (3)0.015 (2)0.025 (2)
C540.053 (3)0.074 (3)0.050 (3)0.020 (3)0.005 (2)0.018 (2)
C550.093 (5)0.071 (4)0.082 (4)0.012 (3)0.030 (4)0.012 (3)
C560.077 (4)0.084 (4)0.061 (3)0.007 (3)0.008 (3)0.016 (3)
C570.110 (6)0.087 (5)0.134 (7)0.017 (5)0.042 (5)0.026 (5)
C580.090 (5)0.094 (5)0.117 (6)0.027 (4)0.014 (4)0.030 (5)
O1S0.073 (3)0.095 (3)0.155 (4)0.027 (2)0.030 (3)0.057 (3)
O2S0.117 (4)0.119 (4)0.142 (4)0.047 (3)0.050 (3)0.073 (4)
C1S0.083 (5)0.091 (5)0.164 (7)0.035 (4)0.044 (5)0.050 (5)
C2S0.100 (6)0.112 (7)0.315 (14)0.019 (5)0.089 (8)0.106 (8)
C3S0.072 (5)0.074 (5)0.270 (12)0.011 (4)−0.010 (6)0.076 (6)
C4S0.103 (6)0.083 (5)0.161 (7)0.045 (4)0.014 (5)0.050 (5)
C5S0.104 (5)0.074 (4)0.085 (5)0.023 (4)−0.008 (4)0.020 (4)
C6S0.160 (8)0.172 (8)0.161 (8)0.113 (7)0.099 (7)0.112 (7)
C7S0.168 (8)0.134 (7)0.182 (9)0.082 (6)0.095 (7)0.113 (7)
C8S0.141 (7)0.107 (6)0.127 (6)0.071 (5)0.049 (5)0.064 (5)
Geometric parameters (Å, °) top
Mo1—C71.956 (4)C30—C311.406 (5)
Mo1—C61.961 (4)C30—C341.413 (5)
Mo1—C32.313 (4)C30—H30A1.0000
Mo1—C42.323 (3)C31—C321.414 (5)
Mo1—C22.356 (4)C31—H31A1.0000
Mo1—C52.360 (4)C32—C331.416 (5)
Mo1—C12.371 (4)C32—H32A1.0000
Mo1—P12.4337 (10)C33—C341.405 (5)
P1—C81.835 (4)C33—H33A1.0000
P1—C201.838 (4)C34—H34A1.0000
P1—C141.840 (4)C37—C421.385 (6)
O1—C61.165 (4)C37—C381.397 (6)
O2—C71.158 (4)C38—C391.379 (6)
C1—C51.401 (5)C38—H38A0.9500
C1—C21.409 (6)C39—C401.380 (7)
C1—H1A1.0000C39—H39A0.9500
C2—C31.404 (6)C40—C411.380 (7)
C2—H2A1.0000C40—H40A0.9500
C3—C41.409 (6)C41—C421.397 (6)
C3—H3A1.0000C41—H41A0.9500
C4—C51.408 (5)C42—H42A0.9500
C4—H4A1.0000C43—C481.395 (5)
C5—H5A1.0000C43—C441.394 (5)
C8—C91.393 (5)C44—C451.388 (5)
C8—C131.396 (5)C44—H44A0.9500
C9—C101.384 (6)C45—C461.385 (6)
C9—H9A0.9500C45—H45A0.9500
C10—C111.377 (8)C46—C471.372 (6)
C10—H10A0.9500C46—H46A0.9500
C11—C121.366 (8)C47—C481.382 (6)
C11—H11A0.9500C47—H47A0.9500
C12—C131.387 (6)C48—H48A0.9500
C12—H12A0.9500C49—C501.516 (6)
C13—H13A0.9500C49—H49A0.9900
C14—C151.394 (5)C49—H49B0.9900
C14—C191.395 (5)C50—C511.537 (5)
C15—C161.387 (5)C50—H50A0.9900
C15—H15A0.9500C50—H50B0.9900
C16—C171.381 (6)C51—C521.507 (6)
C16—H16A0.9500C51—H51A0.9900
C17—C181.369 (6)C51—H51B0.9900
C17—H17A0.9500C52—C531.515 (6)
C18—C191.394 (5)C52—H52A0.9900
C18—H18A0.9500C52—H52B0.9900
C19—H19A0.9500C53—C541.544 (7)
C20—C211.534 (5)C53—H53A0.9900
C20—H20A0.9900C53—H53B0.9900
C20—H20B0.9900C54—C551.462 (7)
C21—C221.531 (5)C54—H54A0.9900
C21—H21A0.9900C54—H54B0.9900
C21—H21B0.9900C55—C561.526 (8)
C22—C231.506 (6)C55—H55A0.9900
C22—H22A0.9900C55—H55B0.9900
C22—H22B0.9900C56—C571.477 (9)
C23—C241.532 (6)C56—H56A0.9900
C23—H23A0.9900C56—H56B0.9900
C23—H23B0.9900C57—C581.259 (9)
C24—C251.499 (6)C57—H57A0.9500
C24—H24A0.9900C58—H58A0.9500
C24—H24B0.9900C58—H58B0.9500
C25—C261.532 (8)O1S—C4S1.391 (7)
C25—H25A0.9900O1S—C1S1.437 (7)
C25—H25B0.9900O2S—C8S1.392 (7)
C26—C271.521 (9)O2S—C5S1.422 (7)
C26—H26A0.9900C1S—C2S1.457 (9)
C26—H26B0.9900C1S—H1SA0.9900
C27—C281.471 (9)C1S—H1SB0.9900
C27—H27A0.9900C2S—C3S1.394 (10)
C27—H27B0.9900C2S—H2SA0.9900
C28—C291.250 (9)C2S—H2SB0.9900
C28—H28A0.9500C3S—C4S1.449 (10)
C29—H29A0.9500C3S—H3SA0.9900
C29—H29B0.9500C3S—H3SB0.9900
Mo2—C361.960 (4)C4S—H4SA0.9900
Mo2—C351.965 (4)C4S—H4SB0.9900
Mo2—C332.325 (4)C5S—C6S1.480 (9)
Mo2—C322.327 (3)C5S—H5SA0.9900
Mo2—C342.351 (4)C5S—H5SB0.9900
Mo2—C302.375 (3)C6S—C7S1.467 (9)
Mo2—C312.378 (3)C6S—H6SA0.9900
Mo2—P22.4191 (9)C6S—H6SB0.9900
P2—C431.839 (4)C7S—C8S1.438 (10)
P2—C371.844 (4)C7S—H7SA0.9900
P2—C491.853 (4)C7S—H7SB0.9900
O3—C351.164 (4)C8S—H8SA0.9900
O4—C361.168 (4)C8S—H8SB0.9900
C7—Mo1—C6103.92 (14)C34—Mo2—P2123.22 (10)
C7—Mo1—C3139.05 (16)C30—Mo2—P2141.12 (9)
C6—Mo1—C3111.19 (15)C31—Mo2—P2112.24 (9)
C7—Mo1—C4105.76 (15)C43—P2—C37102.50 (17)
C6—Mo1—C4146.03 (14)C43—P2—C49101.89 (17)
C3—Mo1—C435.38 (14)C37—P2—C4999.87 (18)
C7—Mo1—C2155.25 (15)C43—P2—Mo2118.30 (12)
C6—Mo1—C297.77 (15)C37—P2—Mo2112.64 (12)
C3—Mo1—C234.98 (15)C49—P2—Mo2118.88 (13)
C4—Mo1—C258.31 (15)C31—C30—C34108.8 (3)
C7—Mo1—C597.95 (14)C31—C30—Mo272.9 (2)
C6—Mo1—C5151.64 (15)C34—C30—Mo271.7 (2)
C3—Mo1—C558.30 (14)C31—C30—H30A125.5
C4—Mo1—C534.99 (13)C34—C30—H30A125.5
C2—Mo1—C557.84 (14)Mo2—C30—H30A125.5
C7—Mo1—C1121.87 (14)C30—C31—C32107.3 (3)
C6—Mo1—C1117.22 (14)C30—C31—Mo272.7 (2)
C3—Mo1—C157.91 (14)C32—C31—Mo270.6 (2)
C4—Mo1—C157.82 (14)C30—C31—H31A126.2
C2—Mo1—C134.67 (14)C32—C31—H31A126.2
C5—Mo1—C134.44 (13)Mo2—C31—H31A126.2
C7—Mo1—P179.76 (10)C31—C32—C33108.3 (3)
C6—Mo1—P180.28 (10)C31—C32—Mo274.5 (2)
C3—Mo1—P185.92 (11)C33—C32—Mo272.2 (2)
C4—Mo1—P189.06 (10)C31—C32—H32A125.6
C2—Mo1—P1116.03 (12)C33—C32—H32A125.6
C5—Mo1—P1121.76 (10)Mo2—C32—H32A125.6
C1—Mo1—P1143.12 (10)C34—C33—C32107.9 (3)
C8—P1—C20105.18 (18)C34—C33—Mo273.5 (2)
C8—P1—C14102.12 (17)C32—C33—Mo272.4 (2)
C20—P1—C14102.22 (17)C34—C33—H33A125.8
C8—P1—Mo1114.01 (12)C32—C33—H33A125.8
C20—P1—Mo1112.27 (13)Mo2—C33—H33A125.8
C14—P1—Mo1119.39 (12)C33—C34—C30107.7 (3)
C5—C1—C2108.6 (4)C33—C34—Mo271.5 (2)
C5—C1—Mo172.4 (2)C30—C34—Mo273.5 (2)
C2—C1—Mo172.1 (2)C33—C34—H34A125.9
C5—C1—H1A125.6C30—C34—H34A125.9
C2—C1—H1A125.6Mo2—C34—H34A125.9
Mo1—C1—H1A125.6O3—C35—Mo2172.3 (3)
C3—C2—C1107.5 (4)O4—C36—Mo2174.0 (3)
C3—C2—Mo170.8 (2)C42—C37—C38118.2 (4)
C1—C2—Mo173.2 (2)C42—C37—P2122.1 (3)
C3—C2—H2A126.1C38—C37—P2119.5 (3)
C1—C2—H2A126.1C39—C38—C37121.4 (4)
Mo1—C2—H2A126.1C39—C38—H38A119.3
C2—C3—C4108.3 (4)C37—C38—H38A119.3
C2—C3—Mo174.2 (2)C38—C39—C40119.7 (5)
C4—C3—Mo172.7 (2)C38—C39—H39A120.2
C2—C3—H3A125.6C40—C39—H39A120.2
C4—C3—H3A125.6C39—C40—C41120.2 (5)
Mo1—C3—H3A125.6C39—C40—H40A119.9
C5—C4—C3107.8 (4)C41—C40—H40A119.9
C5—C4—Mo173.9 (2)C40—C41—C42119.8 (5)
C3—C4—Mo171.9 (2)C40—C41—H41A120.1
C5—C4—H4A125.9C42—C41—H41A120.1
C3—C4—H4A125.9C37—C42—C41120.7 (4)
Mo1—C4—H4A125.9C37—C42—H42A119.7
C1—C5—C4107.8 (4)C41—C42—H42A119.7
C1—C5—Mo173.2 (2)C48—C43—C44117.8 (3)
C4—C5—Mo171.1 (2)C48—C43—P2120.8 (3)
C1—C5—H5A126.0C44—C43—P2121.4 (3)
C4—C5—H5A126.0C45—C44—C43121.1 (3)
Mo1—C5—H5A126.0C45—C44—H44A119.5
O1—C6—Mo1173.2 (3)C43—C44—H44A119.5
O2—C7—Mo1174.7 (3)C46—C45—C44119.8 (4)
C9—C8—C13118.7 (4)C46—C45—H45A120.1
C9—C8—P1121.0 (3)C44—C45—H45A120.1
C13—C8—P1120.0 (3)C47—C46—C45119.8 (4)
C10—C9—C8120.3 (5)C47—C46—H46A120.1
C10—C9—H9A119.9C45—C46—H46A120.1
C8—C9—H9A119.9C46—C47—C48120.6 (4)
C11—C10—C9120.2 (5)C46—C47—H47A119.7
C11—C10—H10A119.9C48—C47—H47A119.7
C9—C10—H10A119.9C47—C48—C43120.9 (4)
C12—C11—C10120.3 (4)C47—C48—H48A119.6
C12—C11—H11A119.9C43—C48—H48A119.6
C10—C11—H11A119.9C50—C49—P2115.2 (3)
C11—C12—C13120.4 (5)C50—C49—H49A108.5
C11—C12—H12A119.8P2—C49—H49A108.5
C13—C12—H12A119.8C50—C49—H49B108.5
C12—C13—C8120.2 (4)P2—C49—H49B108.5
C12—C13—H13A119.9H49A—C49—H49B107.5
C8—C13—H13A119.9C49—C50—C51111.6 (3)
C15—C14—C19118.2 (3)C49—C50—H50A109.3
C15—C14—P1120.2 (3)C51—C50—H50A109.3
C19—C14—P1121.6 (3)C49—C50—H50B109.3
C16—C15—C14121.2 (4)C51—C50—H50B109.3
C16—C15—H15A119.4H50A—C50—H50B108.0
C14—C15—H15A119.4C52—C51—C50114.2 (3)
C17—C16—C15119.3 (4)C52—C51—H51A108.7
C17—C16—H16A120.3C50—C51—H51A108.7
C15—C16—H16A120.3C52—C51—H51B108.7
C18—C17—C16120.6 (4)C50—C51—H51B108.7
C18—C17—H17A119.7H51A—C51—H51B107.6
C16—C17—H17A119.7C51—C52—C53115.9 (4)
C17—C18—C19120.2 (4)C51—C52—H52A108.3
C17—C18—H18A119.9C53—C52—H52A108.3
C19—C18—H18A119.9C51—C52—H52B108.3
C18—C19—C14120.3 (4)C53—C52—H52B108.3
C18—C19—H19A119.9H52A—C52—H52B107.4
C14—C19—H19A119.9C52—C53—C54113.9 (4)
C21—C20—P1120.8 (3)C52—C53—H53A108.8
C21—C20—H20A107.1C54—C53—H53A108.8
P1—C20—H20A107.1C52—C53—H53B108.8
C21—C20—H20B107.1C54—C53—H53B108.8
P1—C20—H20B107.1H53A—C53—H53B107.7
H20A—C20—H20B106.8C55—C54—C53114.9 (4)
C22—C21—C20109.8 (3)C55—C54—H54A108.5
C22—C21—H21A109.7C53—C54—H54A108.5
C20—C21—H21A109.7C55—C54—H54B108.5
C22—C21—H21B109.7C53—C54—H54B108.5
C20—C21—H21B109.7H54A—C54—H54B107.5
H21A—C21—H21B108.2C54—C55—C56115.8 (5)
C23—C22—C21114.6 (4)C54—C55—H55A108.3
C23—C22—H22A108.6C56—C55—H55A108.3
C21—C22—H22A108.6C54—C55—H55B108.3
C23—C22—H22B108.6C56—C55—H55B108.3
C21—C22—H22B108.6H55A—C55—H55B107.4
H22A—C22—H22B107.6C57—C56—C55114.2 (5)
C22—C23—C24110.6 (4)C57—C56—H56A108.7
C22—C23—H23A109.5C55—C56—H56A108.7
C24—C23—H23A109.5C57—C56—H56B108.7
C22—C23—H23B109.5C55—C56—H56B108.7
C24—C23—H23B109.5H56A—C56—H56B107.6
H23A—C23—H23B108.1C58—C57—C56131.2 (9)
C25—C24—C23115.8 (4)C58—C57—H57A114.4
C25—C24—H24A108.3C56—C57—H57A114.4
C23—C24—H24A108.3C57—C58—H58A120.0
C25—C24—H24B108.3C57—C58—H58B120.0
C23—C24—H24B108.3H58A—C58—H58B120.0
H24A—C24—H24B107.4C4S—O1S—C1S109.4 (5)
C24—C25—C26115.3 (4)C8S—O2S—C5S108.2 (5)
C24—C25—H25A108.5O1S—C1S—C2S104.0 (6)
C26—C25—H25A108.5O1S—C1S—H1SA111.0
C24—C25—H25B108.5C2S—C1S—H1SA111.0
C26—C25—H25B108.5O1S—C1S—H1SB111.0
H25A—C25—H25B107.5C2S—C1S—H1SB111.0
C27—C26—C25114.5 (5)H1SA—C1S—H1SB109.0
C27—C26—H26A108.6C3S—C2S—C1S107.6 (7)
C25—C26—H26A108.6C3S—C2S—H2SA110.2
C27—C26—H26B108.6C1S—C2S—H2SA110.2
C25—C26—H26B108.6C3S—C2S—H2SB110.2
H26A—C26—H26B107.6C1S—C2S—H2SB110.2
C28—C27—C26115.4 (5)H2SA—C2S—H2SB108.5
C28—C27—H27A108.4C2S—C3S—C4S105.0 (6)
C26—C27—H27A108.4C2S—C3S—H3SA110.7
C28—C27—H27B108.4C4S—C3S—H3SA110.7
C26—C27—H27B108.4C2S—C3S—H3SB110.7
H27A—C27—H27B107.5C4S—C3S—H3SB110.7
C29—C28—C27128.2 (7)H3SA—C3S—H3SB108.8
C29—C28—H28A115.9O1S—C4S—C3S106.8 (6)
C27—C28—H28A115.9O1S—C4S—H4SA110.4
C28—C29—H29A120.0C3S—C4S—H4SA110.4
C28—C29—H29B120.0O1S—C4S—H4SB110.4
H29A—C29—H29B120.0C3S—C4S—H4SB110.4
C36—Mo2—C35105.41 (15)H4SA—C4S—H4SB108.6
C36—Mo2—C33103.58 (14)O2S—C5S—C6S107.9 (5)
C35—Mo2—C33147.55 (14)O2S—C5S—H5SA110.1
C36—Mo2—C32136.06 (14)C6S—C5S—H5SA110.1
C35—Mo2—C32112.24 (14)O2S—C5S—H5SB110.1
C33—Mo2—C3235.45 (13)C6S—C5S—H5SB110.1
C36—Mo2—C3498.15 (14)H5SA—C5S—H5SB108.4
C35—Mo2—C34148.90 (14)C7S—C6S—C5S103.4 (6)
C33—Mo2—C3434.96 (12)C7S—C6S—H6SA111.1
C32—Mo2—C3458.37 (13)C5S—C6S—H6SA111.1
C36—Mo2—C30124.24 (14)C7S—C6S—H6SB111.1
C35—Mo2—C30114.15 (14)C5S—C6S—H6SB111.1
C33—Mo2—C3057.91 (13)H6SA—C6S—H6SB109.1
C32—Mo2—C3057.76 (13)C8S—C7S—C6S105.7 (6)
C34—Mo2—C3034.78 (13)C8S—C7S—H7SA110.6
C36—Mo2—C31156.08 (14)C6S—C7S—H7SA110.6
C35—Mo2—C3196.64 (14)C8S—C7S—H7SB110.6
C33—Mo2—C3158.36 (13)C6S—C7S—H7SB110.6
C32—Mo2—C3134.95 (12)H7SA—C7S—H7SB108.7
C34—Mo2—C3157.97 (13)O2S—C8S—C7S108.5 (6)
C30—Mo2—C3134.42 (12)O2S—C8S—H8SA110.0
C36—Mo2—P280.78 (10)C7S—C8S—H8SA110.0
C35—Mo2—P281.04 (10)O2S—C8S—H8SB110.0
C33—Mo2—P289.57 (9)C7S—C8S—H8SB110.0
C32—Mo2—P283.46 (9)H8SA—C8S—H8SB108.4
C7—Mo1—P1—C8−66.73 (18)C30—Mo2—P2—C4360.8 (2)
C6—Mo1—P1—C8−172.92 (17)C31—Mo2—P2—C4336.68 (17)
C3—Mo1—P1—C874.75 (18)C36—Mo2—P2—C3776.37 (18)
C4—Mo1—P1—C839.47 (18)C35—Mo2—P2—C37−176.29 (17)
C2—Mo1—P1—C893.12 (19)C33—Mo2—P2—C37−27.47 (17)
C5—Mo1—P1—C826.34 (19)C32—Mo2—P2—C37−62.47 (17)
C1—Mo1—P1—C864.1 (2)C34—Mo2—P2—C37−17.38 (19)
C7—Mo1—P1—C2052.75 (18)C30—Mo2—P2—C37−58.6 (2)
C6—Mo1—P1—C20−53.44 (17)C31—Mo2—P2—C37−82.73 (18)
C3—Mo1—P1—C20−165.77 (18)C36—Mo2—P2—C49−39.88 (19)
C4—Mo1—P1—C20158.96 (17)C35—Mo2—P2—C4967.47 (18)
C2—Mo1—P1—C20−147.39 (18)C33—Mo2—P2—C49−143.71 (18)
C5—Mo1—P1—C20145.83 (18)C32—Mo2—P2—C49−178.71 (18)
C1—Mo1—P1—C20−176.5 (2)C34—Mo2—P2—C49−133.63 (19)
C7—Mo1—P1—C14172.30 (17)C30—Mo2—P2—C49−174.9 (2)
C6—Mo1—P1—C1466.11 (16)C31—Mo2—P2—C49161.03 (18)
C3—Mo1—P1—C14−46.22 (17)C36—Mo2—C30—C31−164.4 (2)
C4—Mo1—P1—C14−81.49 (17)C35—Mo2—C30—C3164.5 (3)
C2—Mo1—P1—C14−27.84 (18)C33—Mo2—C30—C31−79.6 (2)
C5—Mo1—P1—C14−94.62 (18)C32—Mo2—C30—C31−37.5 (2)
C1—Mo1—P1—C14−56.9 (2)C34—Mo2—C30—C31−117.2 (3)
C7—Mo1—C1—C551.8 (3)P2—Mo2—C30—C31−42.0 (3)
C6—Mo1—C1—C5−178.5 (2)C36—Mo2—C30—C34−47.2 (3)
C3—Mo1—C1—C5−79.5 (3)C35—Mo2—C30—C34−178.3 (2)
C4—Mo1—C1—C5−37.4 (2)C33—Mo2—C30—C3437.5 (2)
C2—Mo1—C1—C5−117.0 (4)C32—Mo2—C30—C3479.7 (2)
P1—Mo1—C1—C5−66.9 (3)C31—Mo2—C30—C34117.2 (3)
C7—Mo1—C1—C2168.8 (2)P2—Mo2—C30—C3475.2 (3)
C6—Mo1—C1—C2−61.6 (3)C34—C30—C31—C32−0.7 (4)
C3—Mo1—C1—C237.5 (3)Mo2—C30—C31—C3262.5 (2)
C4—Mo1—C1—C279.5 (3)C34—C30—C31—Mo2−63.1 (3)
C5—Mo1—C1—C2117.0 (4)C36—Mo2—C31—C3033.4 (4)
P1—Mo1—C1—C250.1 (3)C35—Mo2—C31—C30−124.0 (2)
C5—C1—C2—C30.7 (4)C33—Mo2—C31—C3078.2 (2)
Mo1—C1—C2—C3−63.0 (3)C32—Mo2—C31—C30116.1 (3)
C5—C1—C2—Mo163.6 (3)C34—Mo2—C31—C3036.8 (2)
C7—Mo1—C2—C392.7 (4)P2—Mo2—C31—C30153.0 (2)
C6—Mo1—C2—C3−116.2 (3)C36—Mo2—C31—C32−82.8 (4)
C4—Mo1—C2—C337.9 (2)C35—Mo2—C31—C32119.9 (2)
C5—Mo1—C2—C379.4 (3)C33—Mo2—C31—C32−37.9 (2)
C1—Mo1—C2—C3115.9 (4)C34—Mo2—C31—C32−79.4 (2)
P1—Mo1—C2—C3−33.3 (3)C30—Mo2—C31—C32−116.1 (3)
C7—Mo1—C2—C1−23.2 (5)P2—Mo2—C31—C3236.9 (2)
C6—Mo1—C2—C1127.9 (3)C30—C31—C32—C330.9 (4)
C3—Mo1—C2—C1−115.9 (4)Mo2—C31—C32—C3364.8 (2)
C4—Mo1—C2—C1−78.0 (3)C30—C31—C32—Mo2−63.9 (2)
C5—Mo1—C2—C1−36.5 (2)C36—Mo2—C32—C31144.6 (2)
P1—Mo1—C2—C1−149.2 (2)C35—Mo2—C32—C31−68.5 (2)
C1—C2—C3—C4−0.7 (4)C33—Mo2—C32—C31115.5 (3)
Mo1—C2—C3—C4−65.2 (3)C34—Mo2—C32—C3178.1 (2)
C1—C2—C3—Mo164.5 (3)C30—Mo2—C32—C3136.9 (2)
C7—Mo1—C3—C2−140.3 (3)P2—Mo2—C32—C31−146.0 (2)
C6—Mo1—C3—C272.5 (3)C36—Mo2—C32—C3329.1 (3)
C4—Mo1—C3—C2−115.5 (4)C35—Mo2—C32—C33176.0 (2)
C5—Mo1—C3—C2−78.0 (3)C34—Mo2—C32—C33−37.4 (2)
C1—Mo1—C3—C2−37.2 (2)C30—Mo2—C32—C33−78.6 (2)
P1—Mo1—C3—C2150.4 (2)C31—Mo2—C32—C33−115.5 (3)
C7—Mo1—C3—C4−24.9 (4)P2—Mo2—C32—C3398.5 (2)
C6—Mo1—C3—C4−172.1 (2)C31—C32—C33—C34−0.8 (4)
C2—Mo1—C3—C4115.5 (4)Mo2—C32—C33—C3465.5 (3)
C5—Mo1—C3—C437.5 (2)C31—C32—C33—Mo2−66.3 (3)
C1—Mo1—C3—C478.3 (3)C36—Mo2—C33—C3484.8 (2)
P1—Mo1—C3—C4−94.1 (2)C35—Mo2—C33—C34−122.4 (3)
C2—C3—C4—C50.4 (4)C32—Mo2—C33—C34−115.5 (3)
Mo1—C3—C4—C5−65.8 (3)C30—Mo2—C33—C34−37.3 (2)
C2—C3—C4—Mo166.2 (3)C31—Mo2—C33—C34−78.1 (2)
C7—Mo1—C4—C5−81.2 (3)P2—Mo2—C33—C34165.2 (2)
C6—Mo1—C4—C5128.7 (3)C36—Mo2—C33—C32−159.7 (2)
C3—Mo1—C4—C5115.4 (4)C35—Mo2—C33—C32−6.9 (4)
C2—Mo1—C4—C578.0 (3)C34—Mo2—C33—C32115.5 (3)
C1—Mo1—C4—C536.8 (2)C30—Mo2—C33—C3278.2 (2)
P1—Mo1—C4—C5−160.3 (2)C31—Mo2—C33—C3237.4 (2)
C7—Mo1—C4—C3163.4 (2)P2—Mo2—C33—C32−79.3 (2)
C6—Mo1—C4—C313.3 (4)C32—C33—C34—C300.4 (4)
C2—Mo1—C4—C3−37.5 (2)Mo2—C33—C34—C3065.1 (3)
C5—Mo1—C4—C3−115.4 (4)C32—C33—C34—Mo2−64.7 (3)
C1—Mo1—C4—C3−78.6 (3)C31—C30—C34—C330.1 (4)
P1—Mo1—C4—C384.3 (2)Mo2—C30—C34—C33−63.8 (3)
C2—C1—C5—C4−0.4 (4)C31—C30—C34—Mo263.9 (3)
Mo1—C1—C5—C463.1 (2)C36—Mo2—C34—C33−102.1 (2)
C2—C1—C5—Mo1−63.4 (3)C35—Mo2—C34—C33118.7 (3)
C3—C4—C5—C10.0 (4)C32—Mo2—C34—C3337.9 (2)
Mo1—C4—C5—C1−64.5 (2)C30—Mo2—C34—C33115.7 (3)
C3—C4—C5—Mo164.4 (3)C31—Mo2—C34—C3379.3 (2)
C7—Mo1—C5—C1−137.6 (2)P2—Mo2—C34—C33−17.8 (3)
C6—Mo1—C5—C12.7 (4)C36—Mo2—C34—C30142.2 (2)
C3—Mo1—C5—C178.3 (3)C35—Mo2—C34—C303.0 (4)
C4—Mo1—C5—C1116.2 (4)C33—Mo2—C34—C30−115.7 (3)
C2—Mo1—C5—C136.8 (2)C32—Mo2—C34—C30−77.8 (2)
P1—Mo1—C5—C1139.5 (2)C31—Mo2—C34—C30−36.4 (2)
C7—Mo1—C5—C4106.2 (3)P2—Mo2—C34—C30−133.51 (19)
C6—Mo1—C5—C4−113.5 (3)C36—Mo2—C35—O3158 (2)
C3—Mo1—C5—C4−37.9 (3)C33—Mo2—C35—O36(2)
C2—Mo1—C5—C4−79.4 (3)C32—Mo2—C35—O31(2)
C1—Mo1—C5—C4−116.2 (4)C34—Mo2—C35—O3−64 (2)
P1—Mo1—C5—C423.3 (3)C30—Mo2—C35—O3−62 (2)
C7—Mo1—C6—O1−146 (3)C31—Mo2—C35—O3−31 (2)
C3—Mo1—C6—O112 (3)P2—Mo2—C35—O380 (2)
C4—Mo1—C6—O14(3)C35—Mo2—C36—O4−152 (3)
C2—Mo1—C6—O146 (3)C33—Mo2—C36—O414 (3)
C5—Mo1—C6—O174 (3)C32—Mo2—C36—O4−3(3)
C1—Mo1—C6—O176 (3)C34—Mo2—C36—O449 (3)
P1—Mo1—C6—O1−70 (3)C30—Mo2—C36—O474 (3)
C6—Mo1—C7—O2141 (3)C31—Mo2—C36—O452 (3)
C3—Mo1—C7—O2−8(4)P2—Mo2—C36—O4−74 (3)
C4—Mo1—C7—O2−22 (3)C43—P2—C37—C42−26.9 (4)
C2—Mo1—C7—O2−69 (3)C49—P2—C37—C42−131.6 (3)
C5—Mo1—C7—O2−57 (3)Mo2—P2—C37—C42101.3 (3)
C1—Mo1—C7—O2−84 (3)C43—P2—C37—C38158.5 (3)
P1—Mo1—C7—O264 (3)C49—P2—C37—C3853.9 (3)
C20—P1—C8—C9−34.2 (4)Mo2—P2—C37—C38−73.3 (3)
C14—P1—C8—C9−140.7 (3)C42—C37—C38—C391.1 (6)
Mo1—P1—C8—C989.2 (3)P2—C37—C38—C39175.9 (3)
C20—P1—C8—C13152.0 (3)C37—C38—C39—C400.2 (7)
C14—P1—C8—C1345.6 (3)C38—C39—C40—C41−1.3 (8)
Mo1—P1—C8—C13−84.6 (3)C39—C40—C41—C421.0 (8)
C13—C8—C9—C100.4 (6)C38—C37—C42—C41−1.4 (6)
P1—C8—C9—C10−173.5 (3)P2—C37—C42—C41−176.1 (3)
C8—C9—C10—C111.1 (7)C40—C41—C42—C370.4 (7)
C9—C10—C11—C12−1.9 (8)C37—P2—C43—C48−53.8 (3)
C10—C11—C12—C131.2 (8)C49—P2—C43—C4849.3 (4)
C11—C12—C13—C80.3 (7)Mo2—P2—C43—C48−178.3 (3)
C9—C8—C13—C12−1.1 (6)C37—P2—C43—C44127.6 (3)
P1—C8—C13—C12172.9 (3)C49—P2—C43—C44−129.3 (3)
C8—P1—C14—C15−149.5 (3)Mo2—P2—C43—C443.0 (4)
C20—P1—C14—C15101.8 (3)C48—C43—C44—C451.1 (6)
Mo1—P1—C14—C15−22.8 (3)P2—C43—C44—C45179.8 (3)
C8—P1—C14—C1932.1 (3)C43—C44—C45—C46−0.8 (6)
C20—P1—C14—C19−76.6 (3)C44—C45—C46—C470.1 (6)
Mo1—P1—C14—C19158.9 (3)C45—C46—C47—C480.3 (7)
C19—C14—C15—C16−0.5 (6)C46—C47—C48—C430.0 (7)
P1—C14—C15—C16−179.0 (3)C44—C43—C48—C47−0.7 (6)
C14—C15—C16—C170.0 (6)P2—C43—C48—C47−179.4 (3)
C15—C16—C17—C180.7 (7)C43—P2—C49—C5059.4 (3)
C16—C17—C18—C19−1.0 (7)C37—P2—C49—C50164.6 (3)
C17—C18—C19—C140.4 (6)Mo2—P2—C49—C50−72.6 (3)
C15—C14—C19—C180.3 (6)P2—C49—C50—C51177.2 (3)
P1—C14—C19—C18178.7 (3)C49—C50—C51—C52178.4 (3)
C8—P1—C20—C21−58.2 (3)C50—C51—C52—C5367.8 (5)
C14—P1—C20—C2148.1 (4)C51—C52—C53—C54170.8 (4)
Mo1—P1—C20—C21177.3 (3)C52—C53—C54—C55−176.4 (5)
P1—C20—C21—C22−175.1 (3)C53—C54—C55—C56−176.6 (5)
C20—C21—C22—C23173.3 (4)C54—C55—C56—C57−167.0 (6)
C21—C22—C23—C24−175.5 (4)C55—C56—C57—C58−116.9 (9)
C22—C23—C24—C25−178.8 (4)C4S—O1S—C1S—C2S5.7 (9)
C23—C24—C25—C26−60.4 (6)O1S—C1S—C2S—C3S−20.8 (12)
C24—C25—C26—C27−57.7 (7)C1S—C2S—C3S—C4S27.5 (12)
C25—C26—C27—C28−58.8 (7)C1S—O1S—C4S—C3S10.8 (9)
C26—C27—C28—C29118.3 (9)C2S—C3S—C4S—O1S−23.7 (11)
C36—Mo2—P2—C43−164.23 (18)C8S—O2S—C5S—C6S−3.4 (8)
C35—Mo2—P2—C43−56.88 (17)O2S—C5S—C6S—C7S17.6 (9)
C33—Mo2—P2—C4391.94 (17)C5S—C6S—C7S—C8S−24.7 (10)
C32—Mo2—P2—C4356.93 (17)C5S—O2S—C8S—C7S−12.7 (9)
C34—Mo2—P2—C43102.02 (18)C6S—C7S—C8S—O2S23.9 (10)
Table 1
Selected geometric parameters (Å) top
Mo1—P12.4337 (10)Mo2—P22.4191 (9)
Acknowledgements top

Acknowledgment is made to the Petroleum Research Fund, administered by the American Chemical Society, and to the National Science Foundation for the support of this research. This research was also supported by the National Science Foundation IGERT Fellowship Program under grant No. DGE-0549503.

references
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