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Acta Crystallogr Sect E Struct Rep Online. 2010 July 1; 66(Pt 7): m786.
Published online 2010 June 16. doi:  10.1107/S1600536810021690
PMCID: PMC3006780

Trichloridobis(ethyl­diphenyl­phosphine)(tetra­hydro­furan)­molybdenum(III)

Abstract

In the mononuclear title compound, [MoCl3(C4H8O)(C14H15P)2], obtained by the reaction of trichloro­tris­(tetra­hydro­furan)­molybdenum(III) and ethyl­diphenyl­phosphine in tetra­hydro­furan (THF) solution, the MoIII atom is six-coordinated by one O atom of a THF mol­ecule, two P atoms from two ethyl­diphenyl­phosphine ligands and three Cl atoms in a distorted octa­hedral geometry. The C atoms of the THF molecule are disordered over two positions in a 0.55 (2):0.45 (2) ratio.

Related literature

For the structures of similar molybdenum complexes and for bond-length data, see: Cotton & Jianrui (1996 [triangle]); Cotton & Vidyasagar (1995 [triangle]); Hofacker et al. (1989 [triangle]); Borgmann et al. (1997 [triangle]). For the synthesis, see: Anker et al. (1975 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-0m786-scheme1.jpg

Experimental

Crystal data

  • [MoCl3(C4H8O)(C14H15P)2]
  • M r = 702.85
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-0m786-efi1.jpg
  • a = 15.437 Å
  • b = 13.356 Å
  • c = 20.229 Å
  • β = 128.87°
  • V = 3247.1 Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 0.77 mm−1
  • T = 120 K
  • 0.13 × 0.10 × 0.04 mm

Data collection

  • Oxford Diffraction KM-4/Xcalibur diffractometer with a Sapphire2 detector
  • Absorption correction: analytical [CrysAlis RED (Oxford Diffraction, 2006 [triangle]). based on expressions derived by Clark & Reid (1995 [triangle])] T min = 0.937, T max = 0.970
  • 25240 measured reflections
  • 7022 independent reflections
  • 2985 reflections with I > 2σ(I)
  • R int = 0.089

Refinement

  • R[F 2 > 2σ(F 2)] = 0.044
  • wR(F 2) = 0.115
  • S = 0.81
  • 7022 reflections
  • 385 parameters
  • H-atom parameters constrained
  • Δρmax = 0.70 e Å−3
  • Δρmin = −0.54 e Å−3

Data collection: CrysAlis CCD (Oxford Diffraction, 2006 [triangle]); cell refinement: CrysAlis RED (Oxford Diffraction, 2006 [triangle]); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 [triangle]); software used to prepare material for publication: WinGX (Farrugia, 1999 [triangle]).

Table 1
Selected bond lengths (Å)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810021690/ez2211sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810021690/ez2211Isup2.hkl

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

Acknowledgments

The work was undertaken with financial support from the Polish State Committee, grant No. NN204271535.

supplementary crystallographic information

Comment

The title molecule [MoCl3(PEtPh2)(THF)] was prepared as a potential adduct for synthesis with lithium phosphanides of the formula R2P—P(SiMe3)Li (R = tBu, iPr, Et2N, iPr2N).

The MoIII atom resides in a distorted MoCl3OP2 octahedral environment. The equatorial positions are occupied by three Cl atoms and one O atom from the THF, while the axial positions are occupied by P atoms from two ethyldiphenylphosphine residues. The Mo—Cl bond length [2.3871 (13) Å, 2.3822 (13) Å, 2.4126 (13) Å], the Mo—P bond length [2.5964 (14) Å, 2.5974 (13) Å] and the Mo—O bond length [2.206 (3) Å] are very similar to the previously reported molybdenum complexes (Cotton & Vidyasagar, 1995; Cotton & Jianrui, 1996; Hofacker et al., 1989; Borgmann et al., 1997).

Atoms C29, C30, C31, C32 from the THF molecule were disordered over two positions. During the refinement process the disorder models were refined with occupancies of 0.55 (2) and 0.45 (2).

Experimental

The title compound was prepared according to the previously published method (Anker et al., 1975)

Refinement

Atoms C29, C30, C31, C32 were disordered over two positions. During the refinement process the disorder models were refined with occupancies of 0.55 (2) and 0.45 (2). H atoms bonded to C were included in calculated positions and refined as riding on their parent C atom with C—H = 0.95 Å, Uiso(H) = 1.2 Ueq(C) for aromatic; C—H = 0.99 Å, Uiso(H) = 1.2 Ueq(C) for methylene; and C—H = 0.98 Å, Uiso(H) = 1.5 Ueq(C) for methyl atoms.

Figures

Fig. 1.
The molecular structure of the title compound showing the atomic numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. For clarity, all H atoms and the minor component of the disorder have been omitted.

Crystal data

[MoCl3(C4H8O)(C14H15P)2]F(000) = 1444
Mr = 702.85Dx = 1.438 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 5220 reflections
a = 15.437 Åθ = 2.0–28.9°
b = 13.356 ŵ = 0.77 mm1
c = 20.229 ÅT = 120 K
β = 128.87°Block, orange
V = 3247.1 Å30.13 × 0.1 × 0.04 mm
Z = 4

Data collection

Oxford Diffraction KM-4/Xcalibur diffractometer with a Sapphire2 (large Be window) detector7022 independent reflections
graphite2985 reflections with I > 2σ(I)
Detector resolution: 8.1883 pixels mm-1Rint = 0.089
ω scansθmax = 27°, θmin = 2°
Absorption correction: analytical [CrysAlis RED (Oxford Diffraction, 2006). based on expressions derived by Clark & Reid (1995)]h = −15→19
Tmin = 0.937, Tmax = 0.97k = −16→17
25240 measured reflectionsl = −25→22

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)] = 0.044Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.115H-atom parameters constrained
S = 0.81w = 1/[σ2(Fo2) + (0.0551P)2] where P = (Fo2 + 2Fc2)/3
7022 reflections(Δ/σ)max = 0.001
385 parametersΔρmax = 0.70 e Å3
0 restraintsΔρmin = −0.54 e Å3

Special details

Experimental. CrysAlis RED (Oxford Diffraction, 2006) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by Clark & Reid (1995)
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)

xyzUiso*/UeqOcc. (<1)
Mo10.57979 (3)0.74957 (4)0.63166 (2)0.03356 (12)
Cl10.53421 (13)0.92350 (10)0.61183 (10)0.0612 (4)
Cl20.62891 (9)0.74919 (11)0.76928 (7)0.0511 (3)
Cl30.62090 (10)0.57325 (9)0.64269 (9)0.0488 (3)
P10.78469 (10)0.78721 (10)0.69759 (9)0.0415 (3)
P20.37606 (10)0.70228 (10)0.56343 (8)0.0370 (3)
O10.5361 (2)0.7484 (3)0.50482 (18)0.0411 (7)
C10.8589 (4)0.8883 (4)0.7753 (3)0.0495 (14)
C20.8104 (5)0.9421 (5)0.8018 (4)0.075 (2)
H2A0.73580.92770.77850.09*
C30.8682 (6)1.0174 (6)0.8621 (5)0.099 (3)
H3A0.83341.05470.87970.118*
C40.9750 (6)1.0370 (5)0.8957 (4)0.084 (2)
H4A1.01611.08710.9380.101*
C51.0232 (5)0.9849 (5)0.8687 (4)0.0711 (19)
H5A1.097610.89180.085*
C60.9674 (4)0.9118 (4)0.8095 (4)0.0645 (17)
H6A1.00260.87650.79130.077*
C70.8016 (4)0.8198 (4)0.6187 (3)0.0462 (13)
C80.8262 (6)0.7500 (6)0.5828 (4)0.0873 (15)
H8A0.83890.68260.60180.105*
C90.8329 (5)0.7744 (6)0.5206 (4)0.084 (2)
H9A0.85070.72420.49770.101*
C100.8145 (5)0.8694 (6)0.4914 (4)0.080 (2)
H10A0.82080.88660.4490.096*
C110.7871 (6)0.9387 (5)0.5234 (4)0.0873 (15)
H11A0.77121.00520.50210.105*
C120.7820 (7)0.9141 (5)0.5872 (5)0.098 (2)
H12A0.76410.96490.60970.117*
C130.8800 (4)0.6808 (4)0.7548 (4)0.0563 (16)
H13A0.850.62210.71660.068*
H13B0.95290.69770.76980.068*
C140.8976 (5)0.6530 (5)0.8342 (4)0.084 (2)
H14A0.95620.60220.86540.126*
H14B0.82830.62610.81940.126*
H14C0.91980.71260.870.126*
C150.2980 (4)0.7756 (3)0.5873 (3)0.0414 (13)
C160.1881 (4)0.7565 (4)0.5442 (3)0.0572 (14)
H16A0.15260.7050.50260.069*
C170.1273 (5)0.8118 (5)0.5608 (4)0.0656 (17)
H17A0.0510.79720.53180.079*
C180.1780 (5)0.8869 (5)0.6187 (4)0.0639 (17)
H18A0.13640.92640.62910.077*
C190.2870 (5)0.9059 (5)0.6615 (4)0.0675 (18)
H19A0.32170.95840.70210.081*
C200.3483 (4)0.8502 (4)0.6471 (3)0.0524 (14)
H20A0.42550.86330.67850.063*
C210.2853 (4)0.7107 (4)0.4475 (3)0.0416 (13)
C220.2670 (4)0.6302 (4)0.3982 (3)0.0497 (14)
H22A0.29830.5670.42410.06*
C230.2041 (4)0.6398 (5)0.3121 (3)0.0594 (16)
H23A0.19270.58350.27870.071*
C240.1579 (4)0.7294 (5)0.2740 (3)0.0630 (18)
H24A0.11370.73570.21410.076*
C250.1750 (4)0.8081 (5)0.3209 (4)0.0621 (16)
H25A0.14270.87070.29420.075*
C260.2390 (4)0.8001 (4)0.4079 (4)0.0599 (16)
H26A0.25090.85740.44050.072*
C270.3571 (4)0.5747 (4)0.5836 (3)0.0466 (13)
H27A0.27650.55980.54680.056*
H27B0.39130.52810.56780.056*
C280.4074 (4)0.5557 (4)0.6752 (3)0.0624 (16)
H28A0.39790.4850.68240.094*
H28B0.36990.59770.69010.094*
H28C0.48680.57210.71230.094*
C290.542 (4)0.6602 (15)0.4672 (19)0.064 (3)0.55 (2)
H29A0.48190.61280.45020.077*0.55 (2)
H29B0.61460.62630.50770.077*0.55 (2)
C300.5284 (16)0.6963 (11)0.3911 (10)0.066 (3)0.55 (2)
H30A0.49190.64490.34580.079*0.55 (2)
H30B0.60120.71390.40620.079*0.55 (2)
C310.4556 (16)0.7877 (16)0.3635 (13)0.073 (5)0.55 (2)
H31A0.46970.83630.33430.088*0.55 (2)
H31B0.37580.76910.3250.088*0.55 (2)
C320.488 (5)0.8294 (17)0.4431 (19)0.068 (7)0.55 (2)
H32A0.54270.88380.46340.081*0.55 (2)
H32B0.42180.8570.43440.081*0.55 (2)
C29A0.541 (5)0.6650 (18)0.461 (2)0.056 (3)0.45 (2)
H29C0.50870.6040.46560.067*0.45 (2)
H29D0.61910.65090.48570.067*0.45 (2)
C30A0.474 (2)0.6981 (14)0.3695 (13)0.075 (4)0.45 (2)
H30C0.49620.66170.33970.091*0.45 (2)
H30D0.3930.68950.33820.091*0.45 (2)
C31A0.506 (2)0.8069 (16)0.3820 (17)0.063 (4)0.45 (2)
H31C0.45020.84620.33040.076*0.45 (2)
H31D0.57970.81530.39590.076*0.45 (2)
C32A0.510 (6)0.839 (2)0.455 (3)0.064 (7)0.45 (2)
H32C0.56830.89060.49010.077*0.45 (2)
H32D0.43750.8670.43460.077*0.45 (2)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Mo10.0421 (2)0.0281 (2)0.0318 (2)0.00186 (18)0.02382 (17)0.0012 (2)
Cl10.0978 (11)0.0283 (8)0.0685 (10)0.0094 (7)0.0575 (9)0.0041 (7)
Cl20.0565 (7)0.0651 (8)0.0343 (6)−0.0004 (7)0.0297 (6)0.0013 (8)
Cl30.0583 (8)0.0320 (7)0.0577 (9)0.0070 (6)0.0372 (7)0.0059 (6)
P10.0426 (8)0.0390 (8)0.0446 (8)−0.0019 (5)0.0281 (7)−0.0007 (6)
P20.0405 (7)0.0363 (8)0.0323 (8)0.0025 (5)0.0220 (6)−0.0010 (6)
O10.0568 (19)0.0352 (18)0.0328 (16)0.0028 (17)0.0288 (15)0.0022 (19)
C10.057 (4)0.048 (4)0.045 (3)−0.008 (2)0.032 (3)−0.005 (3)
C20.076 (4)0.081 (5)0.086 (5)−0.033 (3)0.060 (4)−0.042 (4)
C30.109 (6)0.114 (6)0.105 (6)−0.055 (5)0.083 (5)−0.069 (5)
C40.088 (5)0.074 (5)0.069 (5)−0.040 (4)0.039 (4)−0.031 (4)
C50.055 (4)0.062 (5)0.075 (5)−0.018 (3)0.031 (4)−0.012 (4)
C60.060 (4)0.057 (4)0.080 (5)−0.013 (3)0.046 (4)−0.011 (3)
C70.049 (3)0.046 (4)0.053 (3)−0.004 (2)0.036 (3)−0.004 (3)
C80.154 (5)0.060 (3)0.093 (4)0.013 (3)0.099 (4)0.013 (3)
C90.100 (5)0.096 (6)0.086 (5)0.038 (4)0.073 (4)0.009 (4)
C100.114 (5)0.085 (6)0.089 (5)0.006 (4)0.087 (5)0.007 (4)
C110.154 (5)0.060 (3)0.093 (4)0.013 (3)0.099 (4)0.013 (3)
C120.204 (8)0.041 (4)0.116 (6)0.005 (4)0.133 (6)0.006 (4)
C130.048 (3)0.049 (4)0.066 (4)0.003 (2)0.033 (3)0.014 (3)
C140.074 (4)0.084 (5)0.067 (5)0.013 (3)0.031 (4)0.029 (4)
C150.046 (3)0.042 (4)0.033 (3)0.007 (2)0.024 (3)0.002 (2)
C160.051 (3)0.067 (4)0.057 (3)0.003 (3)0.036 (3)−0.008 (3)
C170.058 (4)0.086 (5)0.064 (4)0.018 (3)0.044 (4)0.009 (4)
C180.072 (4)0.069 (5)0.061 (4)0.028 (3)0.047 (4)0.010 (3)
C190.079 (5)0.070 (5)0.056 (4)0.011 (3)0.044 (4)−0.011 (3)
C200.051 (3)0.061 (4)0.042 (3)0.004 (3)0.028 (3)−0.005 (3)
C210.040 (3)0.044 (3)0.036 (3)0.002 (2)0.022 (3)−0.006 (2)
C220.054 (3)0.050 (4)0.048 (3)0.005 (2)0.033 (3)0.001 (3)
C230.060 (4)0.072 (5)0.035 (3)0.003 (3)0.024 (3)−0.012 (3)
C240.056 (4)0.089 (5)0.030 (3)0.013 (3)0.020 (3)−0.005 (3)
C250.067 (4)0.061 (4)0.047 (4)0.022 (3)0.030 (3)0.013 (3)
C260.076 (4)0.047 (4)0.047 (4)0.014 (3)0.034 (3)0.002 (3)
C270.051 (3)0.040 (3)0.052 (3)−0.004 (2)0.034 (3)0.001 (3)
C280.077 (4)0.059 (4)0.058 (4)−0.004 (3)0.045 (3)0.014 (3)
C290.089 (5)0.066 (4)0.053 (5)−0.004 (4)0.052 (5)−0.013 (4)
C300.084 (6)0.076 (5)0.053 (6)−0.004 (5)0.051 (6)−0.011 (4)
C310.086 (14)0.083 (10)0.040 (9)−0.014 (9)0.035 (11)0.004 (7)
C320.094 (19)0.057 (6)0.049 (8)0.010 (8)0.043 (12)0.020 (6)
C29A0.086 (5)0.055 (5)0.052 (5)−0.005 (4)0.056 (5)−0.012 (4)
C30A0.094 (7)0.077 (6)0.058 (6)−0.003 (6)0.049 (6)−0.014 (5)
C31A0.076 (14)0.085 (10)0.036 (10)−0.011 (9)0.039 (12)0.003 (7)
C32A0.092 (19)0.055 (6)0.047 (8)0.008 (8)0.044 (12)0.020 (6)

Geometric parameters (Å, °)

Mo1—O12.206 (3)C16—H16A0.95
Mo1—Cl12.3871 (13)C17—C181.356 (8)
Mo1—Cl22.3822 (13)C17—H17A0.95
Mo1—Cl32.4126 (13)C18—C191.348 (7)
Mo1—P12.5964 (14)C18—H18A0.95
Mo1—P22.5974 (13)C19—C201.371 (7)
P1—C71.824 (6)C19—H19A0.95
P1—C11.830 (5)C20—H20A0.95
P1—C131.840 (5)C21—C261.364 (7)
P2—C271.818 (5)C21—C221.370 (7)
P2—C211.830 (5)C22—C231.368 (7)
P2—C151.838 (5)C22—H22A0.95
O1—C291.434 (15)C23—C241.358 (8)
O1—C29A1.453 (16)C23—H23A0.95
O1—C321.455 (15)C24—C251.326 (7)
O1—C32A1.459 (17)C24—H24A0.95
C1—C21.366 (7)C25—C261.380 (7)
C1—C61.389 (7)C25—H25A0.95
C2—C31.390 (8)C26—H26A0.95
C2—H2A0.95C27—C281.514 (7)
C3—C41.358 (9)C27—H27A0.99
C3—H3A0.95C27—H27B0.99
C4—C51.359 (9)C28—H28A0.98
C4—H4A0.95C28—H28B0.98
C5—C61.355 (8)C28—H28C0.98
C5—H5A0.95C29—C301.499 (17)
C6—H6A0.95C29—H29A0.99
C7—C121.358 (8)C29—H29B0.99
C7—C81.373 (8)C30—C311.510 (16)
C8—C91.364 (9)C30—H30A0.99
C8—H8A0.95C30—H30B0.99
C9—C101.352 (9)C31—C321.464 (16)
C9—H9A0.95C31—H31A0.99
C10—C111.341 (8)C31—H31B0.99
C10—H10A0.95C32—H32A0.99
C11—C121.381 (9)C32—H32B0.99
C11—H11A0.95C29A—C30A1.514 (18)
C12—H12A0.95C29A—H29C0.99
C13—C141.498 (8)C29A—H29D0.99
C13—H13A0.99C30A—C31A1.506 (17)
C13—H13B0.99C30A—H30C0.99
C14—H14A0.98C30A—H30D0.99
C14—H14B0.98C31A—C32A1.509 (18)
C14—H14C0.98C31A—H31C0.99
C15—C161.359 (7)C31A—H31D0.99
C15—C201.371 (7)C32A—H32C0.99
C16—C171.391 (7)C32A—H32D0.99
O1—Mo1—Cl2179.21 (10)C18—C17—H17A120.3
O1—Mo1—Cl188.22 (10)C16—C17—H17A120.3
Cl2—Mo1—Cl192.44 (5)C19—C18—C17120.3 (5)
O1—Mo1—Cl388.34 (10)C19—C18—H18A119.8
Cl2—Mo1—Cl391.01 (5)C17—C18—H18A119.8
Cl1—Mo1—Cl3176.50 (6)C18—C19—C20120.8 (6)
O1—Mo1—P189.05 (9)C18—C19—H19A119.6
Cl2—Mo1—P190.49 (5)C20—C19—H19A119.6
Cl1—Mo1—P191.92 (5)C19—C20—C15119.8 (5)
Cl3—Mo1—P188.66 (4)C19—C20—H20A120.1
O1—Mo1—P289.76 (8)C15—C20—H20A120.1
Cl2—Mo1—P290.67 (4)C26—C21—C22117.8 (5)
Cl1—Mo1—P290.94 (5)C26—C21—P2120.3 (4)
Cl3—Mo1—P288.41 (4)C22—C21—P2121.8 (4)
P1—Mo1—P2176.87 (5)C23—C22—C21120.8 (5)
C7—P1—C1102.7 (2)C23—C22—H22A119.6
C7—P1—C13103.8 (3)C21—C22—H22A119.6
C1—P1—C13101.9 (3)C24—C23—C22120.4 (6)
C7—P1—Mo1113.20 (16)C24—C23—H23A119.8
C1—P1—Mo1119.23 (19)C22—C23—H23A119.8
C13—P1—Mo1114.15 (18)C25—C24—C23119.6 (6)
C27—P2—C21104.1 (2)C25—C24—H24A120.2
C27—P2—C15102.5 (2)C23—C24—H24A120.2
C21—P2—C15101.7 (2)C24—C25—C26120.9 (6)
C27—P2—Mo1114.84 (16)C24—C25—H25A119.6
C21—P2—Mo1111.36 (16)C26—C25—H25A119.6
C15—P2—Mo1120.40 (17)C21—C26—C25120.6 (6)
C29—O1—C32108.9 (15)C21—C26—H26A119.7
C29A—O1—C32104.0 (14)C25—C26—H26A119.7
C29—O1—C32A113.6 (15)C28—C27—P2113.6 (4)
C29A—O1—C32A108.5 (16)C28—C27—H27A108.8
C29—O1—Mo1123.2 (9)P2—C27—H27A108.8
C29A—O1—Mo1128.2 (10)C28—C27—H27B108.8
C32—O1—Mo1127.6 (11)P2—C27—H27B108.8
C32A—O1—Mo1122.9 (12)H27A—C27—H27B107.7
C2—C1—C6118.3 (5)C27—C28—H28A109.5
C2—C1—P1121.5 (4)C27—C28—H28B109.5
C6—C1—P1120.2 (4)H28A—C28—H28B109.5
C1—C2—C3121.1 (6)C27—C28—H28C109.5
C1—C2—H2A119.5H28A—C28—H28C109.5
C3—C2—H2A119.5H28B—C28—H28C109.5
C4—C3—C2119.2 (7)O1—C29—C30105.5 (14)
C4—C3—H3A120.4O1—C29—H29A110.6
C2—C3—H3A120.4C30—C29—H29A110.6
C5—C4—C3120.0 (6)O1—C29—H29B110.6
C5—C4—H4A120C30—C29—H29B110.6
C3—C4—H4A120H29A—C29—H29B108.8
C6—C5—C4121.3 (6)C29—C30—C31103.3 (18)
C6—C5—H5A119.3C29—C30—H30A111.1
C4—C5—H5A119.3C31—C30—H30A111.1
C5—C6—C1120.1 (6)C29—C30—H30B111.1
C5—C6—H6A120C31—C30—H30B111.1
C1—C6—H6A120H30A—C30—H30B109.1
C12—C7—C8115.8 (6)C32—C31—C30104.0 (19)
C12—C7—P1121.3 (5)C32—C31—H31A111
C8—C7—P1122.7 (4)C30—C31—H31A111
C9—C8—C7122.1 (7)C32—C31—H31B111
C9—C8—H8A118.9C30—C31—H31B111
C7—C8—H8A118.9H31A—C31—H31B109
C10—C9—C8120.7 (7)O1—C32—C31107.4 (17)
C10—C9—H9A119.7O1—C32—H32A110.2
C8—C9—H9A119.7C31—C32—H32A110.2
C11—C10—C9118.7 (7)O1—C32—H32B110.2
C11—C10—H10A120.7C31—C32—H32B110.2
C9—C10—H10A120.7H32A—C32—H32B108.5
C10—C11—C12120.4 (6)O1—C29A—C30A105.3 (18)
C10—C11—H11A119.8O1—C29A—H29C110.7
C12—C11—H11A119.8C30A—C29A—H29C110.7
C7—C12—C11122.2 (7)O1—C29A—H29D110.7
C7—C12—H12A118.9C30A—C29A—H29D110.7
C11—C12—H12A118.9H29C—C29A—H29D108.8
C14—C13—P1113.7 (4)C31A—C30A—C29A100 (2)
C14—C13—H13A108.8C31A—C30A—H30C111.8
P1—C13—H13A108.8C29A—C30A—H30C111.8
C14—C13—H13B108.8C31A—C30A—H30D111.8
P1—C13—H13B108.8C29A—C30A—H30D111.8
H13A—C13—H13B107.7H30C—C30A—H30D109.5
C13—C14—H14A109.5C30A—C31A—C32A104 (2)
C13—C14—H14B109.5C30A—C31A—H31C110.9
H14A—C14—H14B109.5C32A—C31A—H31C110.9
C13—C14—H14C109.5C30A—C31A—H31D110.9
H14A—C14—H14C109.5C32A—C31A—H31D110.9
H14B—C14—H14C109.5H31C—C31A—H31D108.9
C16—C15—C20119.4 (5)O1—C32A—C31A105 (2)
C16—C15—P2119.5 (4)O1—C32A—H32C110.7
C20—C15—P2121.1 (4)C31A—C32A—H32C110.7
C15—C16—C17120.3 (6)O1—C32A—H32D110.7
C15—C16—H16A119.8C31A—C32A—H32D110.7
C17—C16—H16A119.8H32C—C32A—H32D108.8
C18—C17—C16119.4 (6)
O1—Mo1—P1—C711.0 (2)P1—C7—C8—C9176.5 (5)
Cl2—Mo1—P1—C7−169.7 (2)C7—C8—C9—C10−0.5 (12)
Cl1—Mo1—P1—C7−77.2 (2)C8—C9—C10—C11−1.4 (11)
Cl3—Mo1—P1—C799.3 (2)C9—C10—C11—C122.3 (11)
O1—Mo1—P1—C1131.9 (2)C8—C7—C12—C11−0.5 (11)
Cl2—Mo1—P1—C1−48.8 (2)P1—C7—C12—C11−175.6 (6)
Cl1—Mo1—P1—C143.7 (2)C10—C11—C12—C7−1.4 (12)
Cl3—Mo1—P1—C1−139.8 (2)C7—P1—C13—C14168.8 (4)
O1—Mo1—P1—C13−107.4 (2)C1—P1—C13—C1462.4 (5)
Cl2—Mo1—P1—C1371.9 (2)Mo1—P1—C13—C14−67.6 (5)
Cl1—Mo1—P1—C13164.4 (2)C27—P2—C15—C16−58.1 (5)
Cl3—Mo1—P1—C13−19.1 (2)C21—P2—C15—C1649.4 (5)
O1—Mo1—P2—C27108.1 (2)Mo1—P2—C15—C16173.0 (4)
Cl2—Mo1—P2—C27−71.3 (2)C27—P2—C15—C20122.9 (4)
Cl1—Mo1—P2—C27−163.7 (2)C21—P2—C15—C20−129.7 (4)
Cl3—Mo1—P2—C2719.7 (2)Mo1—P2—C15—C20−6.1 (5)
O1—Mo1—P2—C21−9.9 (2)C20—C15—C16—C17−0.2 (8)
Cl2—Mo1—P2—C21170.76 (18)P2—C15—C16—C17−179.3 (4)
Cl1—Mo1—P2—C2178.31 (18)C15—C16—C17—C181.8 (9)
Cl3—Mo1—P2—C21−98.26 (18)C16—C17—C18—C19−1.9 (9)
O1—Mo1—P2—C15−128.8 (2)C17—C18—C19—C200.3 (9)
Cl2—Mo1—P2—C1551.90 (18)C18—C19—C20—C151.3 (9)
Cl1—Mo1—P2—C15−40.55 (18)C16—C15—C20—C19−1.3 (8)
Cl3—Mo1—P2—C15142.89 (18)P2—C15—C20—C19177.8 (4)
Cl1—Mo1—O1—C29−180 (2)C27—P2—C21—C26150.8 (5)
Cl3—Mo1—O1—C290(2)C15—P2—C21—C2644.6 (5)
P1—Mo1—O1—C2989 (2)Mo1—P2—C21—C26−84.9 (5)
P2—Mo1—O1—C29−89 (2)C27—P2—C21—C22−33.3 (5)
Cl1—Mo1—O1—C29A179 (3)C15—P2—C21—C22−139.5 (4)
Cl3—Mo1—O1—C29A−2(3)Mo1—P2—C21—C2291.0 (4)
P1—Mo1—O1—C29A87 (3)C26—C21—C22—C23−0.1 (8)
P2—Mo1—O1—C29A−90 (3)P2—C21—C22—C23−176.1 (4)
Cl1—Mo1—O1—C32−6(3)C21—C22—C23—C24−0.6 (9)
Cl3—Mo1—O1—C32173 (3)C22—C23—C24—C250.7 (9)
P1—Mo1—O1—C32−98 (3)C23—C24—C25—C26−0.1 (9)
P2—Mo1—O1—C3285 (3)C22—C21—C26—C250.7 (8)
Cl1—Mo1—O1—C32A7(4)P2—C21—C26—C25176.7 (4)
Cl3—Mo1—O1—C32A−173 (4)C24—C25—C26—C21−0.6 (9)
P1—Mo1—O1—C32A−85 (4)C21—P2—C27—C28−169.0 (4)
P2—Mo1—O1—C32A98 (4)C15—P2—C27—C28−63.3 (4)
C7—P1—C1—C2128.5 (5)Mo1—P2—C27—C2869.0 (4)
C13—P1—C1—C2−124.3 (5)C32—O1—C29—C3017 (4)
Mo1—P1—C1—C22.4 (6)C32A—O1—C29—C305(5)
C7—P1—C1—C6−52.0 (5)Mo1—O1—C29—C30−168.8 (15)
C13—P1—C1—C655.3 (5)O1—C29—C30—C31−30 (4)
Mo1—P1—C1—C6−178.0 (4)C29—C30—C31—C3233 (4)
C6—C1—C2—C3−0.9 (10)C29—O1—C32—C314(5)
P1—C1—C2—C3178.7 (6)C29A—O1—C32—C316(5)
C1—C2—C3—C4−0.6 (12)C32A—O1—C32—C31120 (18)
C2—C3—C4—C51.6 (12)Mo1—O1—C32—C31−170.0 (17)
C3—C4—C5—C6−1.2 (11)C30—C31—C32—O1−23 (4)
C4—C5—C6—C1−0.3 (10)C32—O1—C29A—C30A−11 (4)
C2—C1—C6—C51.3 (9)C32A—O1—C29A—C30A−22 (5)
P1—C1—C6—C5−178.2 (5)Mo1—O1—C29A—C30A165.2 (15)
C1—P1—C7—C12−47.7 (6)O1—C29A—C30A—C31A38 (4)
C13—P1—C7—C12−153.6 (5)C29A—C30A—C31A—C32A−39 (4)
Mo1—P1—C7—C1282.1 (5)C29—O1—C32A—C31A−4(6)
C1—P1—C7—C8137.5 (5)C29A—O1—C32A—C31A−3(6)
C13—P1—C7—C831.6 (6)C32—O1—C32A—C31A−73 (13)
Mo1—P1—C7—C8−92.7 (5)Mo1—O1—C32A—C31A170 (2)
C12—C7—C8—C91.4 (10)C30A—C31A—C32A—O127 (5)

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: EZ2211).

References

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