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Acta Cryst. (2008). E64, m1382    [ doi:10.1107/S1600536808032364 ]

[Bis(diphenylphosphino)methane-[kappa]2P,P'][bis(diphenylphosphinomethyl)diethoxysilane-[kappa]2P,P']bis(dinitrogen)molybdenum(0) benzene 0.7-solvate

K. Klatt, C. Näther and F. Tuczek

Abstract top

In the crystal structure of the title compound, [Mo(C25H22P2)(C30H34O2P2Si)(N2)2]·0.7C6H6, the Mo atoms are coordinated by four P atoms and two N atoms in a distorted octahedral mode. The two C atoms of one of the two ethoxy groups are disordered and were refined using a split model and site-occupation factors of 0.7:0.3. The crystal structure contains a benzene solvent molecule with a site occupation of 70%.

Comment top

The structure determination of this compound was undertaken as part of a project on grafting molybdenum(0) dinitrogen complexes to silica, in analogy to studies of Bluemel et al. on the immobilization of palladium phosphine complexes to silica for applications in catalysis (Bogza et al., 2005). Later these studies will be extended to semiconducting oxides like SnO2. In contrast to Leigh & Pickett who have attached Mo(0) dinitrogen complexes to SnO2 via an axial nitrile ligand (Leigh & Pickett, 1977). the title complex would allow this attachment via the equatorial bis(diphenylphosphinomethyl)-diethoxysilane ligand.

In the crystal structure of the title compound, C55H56MoN4O2P4Si . (C6H6)0.7 the Mo atoms are coordinated by each two P atoms of the dppm (dppm = diphenylphosphinomethane) and the (Ph2PCH2)2Si(OEt)2 ligand as well as two N atoms of two crystallographically independent N atoms of the dinitrogen ligand within distorted octahedra (Tab. 1 and Fig. 1).

Related literature top

For the coordination chemistry of dinitrogen, see: MacKay & Fryzuk (2004). For the synthesis of the ligand, see: Bogza et al. (2005); Leigh & Pickett (1977).

Experimental top

A suspension of 281 mg (0.44 mmol) MoCl4(dppm) and 260 mg (0.50 mmol) (Ph2PCH2)2Si(OEt)2 in 20 ml THF was added to sodium amalgam (200 mg Na, 30.0 g H g)and stirred for 3 h at 0 °C and 16 h at ambient temperature under N2. The solution was decanted, filtered and reduced in vacuo to 6 ml. 6 ml of methanol were added and the solvent was reduced in vacuo again. After addition of another 6 ml of methanol the formed precipitate was filtered off, washed four times with 4 ml of methanol and dried in vacuo.

Refinement top

All H atoms were positioned with idealized geometry and were refined with Ueq(H) = 1.2 Ueq of the parent atom (1.5 for methyl H atoms) using a riding model with C—H = 0.94–0.98 Å. The two carbon atoms of one of the two ethoxy groups are disordered and were refined using a split model. The site occupation factors refined to 0.7 and 0.3 but were fixed in the final refinement. The atoms on the site of lower occupancy were refined only isotropically. The positions of the benzene molecule are clearly not fully occupied. In the beginning the site occupation factors were refined but later, they were fixed at 0.7. Equivalent bond distances of the disordered ethoxy group and the bond distances in the solvent benzene ring were restrained to be equal with an effective standard deviation 0.02. In addition, the six atoms of the benzene ring were restrained to lie in a common plane.

Computing details top

Data collection: IPDS Program Package (Stoe & Cie, 1998); cell refinement: IPDS Program Package (Stoe & Cie, 1998); data reduction: IPDS Program Package (Stoe & Cie, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: CIFTAB in SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. : Crystal structure of the title compound with labelling and displacement ellipsoids drawn at the 30% probability level. The disorder of the carbon atoms is shown with full and open bonds.
[Bis(diphenylphosphino)methane- κ2P,P'][bis(diphenylphosphinomethyl)diethoxysilane- κ2P,P']bis(dinitrogen)molybdenum(0) benzene 0.7-solvate top
Crystal data top
[Mo(C25H22P2)(C30H34O2P2Si)(N2)2]·0.7C6H6F(000) = 4603
Mr = 1107.62Dx = 1.264 Mg m−3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 26.3512 (19) ÅCell parameters from 8000 reflections
b = 18.2414 (8) Åθ = 2–26°
c = 24.3498 (15) ŵ = 0.40 mm−1
β = 96.114 (8)°T = 220 K
V = 11638.0 (12) Å3Block, red
Z = 80.12 × 0.10 × 0.06 mm
Data collection top
Stoe IPDS-I
diffractometer		11012 independent reflections
Radiation source: fine-focus sealed tube8579 reflections with I > 2σ(I)
graphiteRint = 0.074
φ scansθmax = 26.0°, θmin = 2.4°
Absorption correction: numerical
(X-SHAPE; Stoe & Cie, 1998)		h = −32→32
Tmin = 0.864, Tmax = 0.966k = −22→22
45011 measured reflectionsl = −29→29
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.060H-atom parameters constrained
wR(F2) = 0.144 w = 1/[σ2(Fo2) + (0.0347P)2 + 93.4691P]
where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max = 0.001
11012 reflectionsΔρmax = 0.86 e Å−3
667 parametersΔρmin = −0.71 e Å−3
20 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00028 (7)
Crystal data top
[Mo(C25H22P2)(C30H34O2P2Si)(N2)2]·0.7C6H6V = 11638.0 (12) Å3
Mr = 1107.62Z = 8
Monoclinic, C2/cMo Kα radiation
a = 26.3512 (19) ŵ = 0.40 mm−1
b = 18.2414 (8) ÅT = 220 K
c = 24.3498 (15) Å0.12 × 0.10 × 0.06 mm
β = 96.114 (8)°
Data collection top
Stoe IPDS-I
diffractometer		11012 independent reflections
Absorption correction: numerical
(X-SHAPE; Stoe & Cie, 1998)		8579 reflections with I > 2σ(I)
Tmin = 0.864, Tmax = 0.966Rint = 0.074
45011 measured reflectionsθmax = 26.0°
Refinement top
R[F2 > 2σ(F2)] = 0.060 w = 1/[σ2(Fo2) + (0.0347P)2 + 93.4691P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.144Δρmax = 0.86 e Å−3
S = 1.09Δρmin = −0.71 e Å−3
11012 reflectionsAbsolute structure: ?
667 parametersFlack parameter: ?
20 restraintsRogers parameter: ?
H-atom parameters constrained
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*/UeqOcc. (<1)
Mo10.207010 (13)0.503577 (18)0.586610 (14)0.01918 (12)
N10.20784 (14)0.3935 (2)0.57550 (15)0.0266 (8)
N20.20844 (17)0.3324 (2)0.56985 (19)0.0409 (10)
N30.20929 (15)0.6111 (2)0.60433 (15)0.0281 (8)
N40.21203 (19)0.6703 (2)0.61769 (18)0.0435 (11)
C10.33665 (18)0.5687 (2)0.62864 (19)0.0307 (10)
H1A0.32790.62020.62110.037*
H1B0.37240.56270.62180.037*
P10.29814 (4)0.51381 (6)0.57620 (5)0.0236 (2)
C20.26745 (18)0.5533 (2)0.72242 (18)0.0292 (10)
H2A0.26890.54380.76220.035*
H2B0.25360.60290.71610.035*
P20.22134 (4)0.48876 (6)0.68709 (4)0.0231 (2)
O10.36655 (13)0.48060 (19)0.72215 (14)0.0403 (8)
C30.3749 (2)0.4511 (3)0.7766 (2)0.0476 (14)
H3A0.34430.42500.78550.057*
H3B0.38190.49090.80340.057*
C40.4189 (3)0.4000 (5)0.7801 (4)0.088 (3)
H4A0.42450.37990.81710.132*
H4B0.44910.42620.77170.132*
H4C0.41170.36060.75370.132*
O20.36327 (16)0.6223 (2)0.73739 (17)0.0531 (11)
C50.3407 (4)0.6891 (4)0.7495 (4)0.054 (2)0.70
H5A0.30960.67810.76660.065*0.70
H5B0.33030.71390.71440.065*0.70
C60.3701 (6)0.7400 (6)0.7846 (6)0.095 (5)0.70
H6A0.34990.78360.78920.143*0.70
H6B0.40060.75330.76790.143*0.70
H6C0.37960.71750.82030.143*0.70
C5'0.3630 (16)0.6733 (17)0.7787 (13)0.134 (15)*0.30
H5C0.37460.65150.81470.161*0.30
H5D0.32870.69330.78010.161*0.30
C6'0.3982 (12)0.7304 (17)0.7648 (15)0.087 (10)*0.30
H6D0.39810.77020.79120.130*0.30
H6E0.38740.74880.72800.130*0.30
H6F0.43230.71030.76580.130*0.30
Si10.33400 (5)0.55386 (7)0.70401 (5)0.0304 (3)
C110.31535 (17)0.5657 (2)0.51541 (19)0.0291 (10)
C120.28563 (19)0.6258 (2)0.49781 (19)0.0333 (10)
H120.25740.63830.51650.040*
C130.2968 (2)0.6678 (3)0.4532 (2)0.0422 (13)
H130.27620.70830.44190.051*
C140.3382 (2)0.6502 (3)0.4252 (2)0.0530 (16)
H140.34580.67850.39490.064*
C150.3680 (2)0.5910 (4)0.4422 (3)0.0596 (17)
H150.39610.57890.42320.072*
C160.3571 (2)0.5483 (3)0.4872 (2)0.0439 (13)
H160.37790.50790.49830.053*
C210.33546 (17)0.4297 (2)0.56971 (19)0.0292 (10)
C220.31851 (19)0.3805 (3)0.5279 (2)0.0350 (11)
H220.28880.39150.50450.042*
C230.3442 (2)0.3162 (3)0.5200 (3)0.0484 (14)
H230.33270.28480.49070.058*
C240.3870 (2)0.2981 (3)0.5553 (3)0.0576 (17)
H240.40430.25390.55050.069*
C250.4040 (2)0.3454 (4)0.5973 (3)0.0605 (17)
H250.43320.33330.62130.073*
C260.3785 (2)0.4110 (3)0.6048 (2)0.0439 (13)
H260.39060.44280.63360.053*
C310.24594 (17)0.4021 (2)0.71857 (18)0.0265 (9)
C320.27744 (18)0.3571 (2)0.69038 (19)0.0309 (10)
H320.28370.36930.65420.037*
C330.2996 (2)0.2948 (3)0.7148 (2)0.0381 (12)
H330.32090.26550.69530.046*
C340.2904 (2)0.2757 (3)0.7676 (2)0.0391 (12)
H340.30540.23310.78400.047*
C350.25930 (19)0.3190 (3)0.7965 (2)0.0372 (11)
H350.25300.30570.83250.045*
C360.23744 (18)0.3820 (3)0.77250 (19)0.0312 (10)
H360.21670.41150.79250.037*
C410.16564 (17)0.5045 (3)0.72604 (17)0.0294 (9)
C420.12474 (18)0.4561 (3)0.7184 (2)0.0356 (11)
H420.12680.41500.69550.043*
C430.0808 (2)0.4678 (4)0.7441 (2)0.0500 (14)
H430.05380.43390.73890.060*
C440.0762 (2)0.5281 (4)0.7768 (2)0.0552 (16)
H440.04600.53650.79310.066*
C450.1165 (2)0.5762 (3)0.7855 (2)0.0514 (15)
H450.11390.61720.80850.062*
C460.1610 (2)0.5647 (3)0.7607 (2)0.0390 (12)
H460.18820.59790.76720.047*
P30.17645 (4)0.51372 (6)0.48719 (4)0.0226 (2)
P40.11254 (4)0.50224 (6)0.56937 (4)0.0252 (2)
C510.11108 (16)0.4821 (2)0.49459 (17)0.0274 (9)
H51A0.10650.42980.48640.033*
H51B0.08510.51080.47210.033*
C610.20347 (17)0.4523 (2)0.43829 (18)0.0272 (9)
C620.24413 (17)0.4761 (3)0.41067 (18)0.0302 (10)
H620.25320.52600.41160.036*
C630.2713 (2)0.4266 (3)0.3818 (2)0.0404 (12)
H630.29870.44330.36340.048*
C640.2586 (2)0.3531 (3)0.3798 (2)0.0480 (14)
H640.27730.32010.36020.058*
C650.2184 (2)0.3286 (3)0.4065 (2)0.0467 (14)
H650.20960.27870.40520.056*
C660.1908 (2)0.3778 (3)0.4357 (2)0.0354 (11)
H660.16330.36060.45370.042*
C710.16255 (16)0.5969 (2)0.44540 (18)0.0257 (9)
C720.15542 (19)0.6634 (3)0.4722 (2)0.0348 (11)
H720.16090.66580.51100.042*
C730.1404 (2)0.7256 (3)0.4423 (2)0.0408 (12)
H730.13520.76970.46080.049*
C740.13310 (19)0.7233 (3)0.3856 (2)0.0372 (11)
H740.12330.76580.36540.045*
C750.14024 (19)0.6582 (3)0.3584 (2)0.0351 (11)
H750.13560.65660.31960.042*
C760.15416 (18)0.5953 (3)0.38808 (18)0.0299 (10)
H760.15800.55090.36930.036*
C810.06569 (17)0.4360 (3)0.58982 (19)0.0326 (10)
C820.0772 (2)0.3616 (3)0.5871 (2)0.0448 (13)
H820.10830.34710.57470.054*
C830.0437 (2)0.3082 (3)0.6025 (3)0.0584 (17)
H830.05180.25820.60010.070*
C84−0.0016 (2)0.3297 (4)0.6215 (3)0.064 (2)
H84−0.02440.29410.63230.077*
C85−0.0137 (2)0.4024 (4)0.6247 (3)0.0606 (18)
H85−0.04470.41630.63760.073*
C860.01936 (18)0.4561 (3)0.6091 (2)0.0445 (13)
H860.01070.50590.61150.053*
C910.07932 (18)0.5888 (3)0.5757 (2)0.0341 (11)
C920.0885 (2)0.6268 (3)0.6251 (2)0.0465 (14)
H920.11110.60680.65360.056*
C930.0654 (3)0.6931 (4)0.6335 (3)0.0633 (19)
H930.07150.71700.66780.076*
C940.0333 (3)0.7241 (4)0.5917 (3)0.075 (2)
H940.01830.77000.59680.090*
C950.0233 (3)0.6878 (4)0.5423 (3)0.077 (2)
H950.00100.70860.51370.092*
C960.0458 (2)0.6207 (4)0.5345 (2)0.0547 (16)
H960.03830.59610.50070.066*
C1010.4698 (5)0.6214 (8)0.5784 (6)0.104 (5)0.70
H1010.43600.63710.56950.125*0.70
C1020.4863 (4)0.6103 (7)0.6313 (6)0.102 (5)0.70
H1020.46390.61360.65870.122*0.70
C1030.5348 (5)0.5946 (7)0.6440 (7)0.115 (5)0.70
H1030.54720.58410.68080.138*0.70
C1040.5668 (5)0.5936 (8)0.6041 (8)0.123 (7)0.70
H1040.60200.58760.61370.148*0.70
C1050.5483 (6)0.6012 (8)0.5501 (7)0.129 (7)0.70
H1050.57040.59920.52230.155*0.70
C1060.4987 (5)0.6113 (10)0.5373 (7)0.121 (6)0.70
H1060.48430.61140.50030.146*0.70
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.02565 (19)0.01740 (18)0.01462 (19)−0.00022 (14)0.00270 (12)−0.00092 (12)
N10.030 (2)0.030 (2)0.020 (2)−0.0030 (15)0.0036 (15)−0.0013 (14)
N20.055 (3)0.0183 (19)0.049 (3)−0.0003 (17)0.003 (2)−0.0048 (17)
N30.040 (2)0.0262 (19)0.0179 (19)0.0019 (16)0.0007 (16)0.0026 (14)
N40.074 (3)0.022 (2)0.033 (2)−0.0018 (19)−0.003 (2)−0.0049 (16)
C10.033 (2)0.029 (2)0.030 (3)−0.0038 (18)0.0031 (19)0.0028 (18)
P10.0267 (5)0.0229 (5)0.0210 (6)−0.0021 (4)0.0018 (4)0.0004 (4)
C20.042 (3)0.028 (2)0.017 (2)0.0002 (19)0.0041 (18)−0.0021 (16)
P20.0303 (5)0.0231 (5)0.0159 (5)0.0018 (4)0.0022 (4)0.0004 (4)
O10.0431 (19)0.045 (2)0.033 (2)0.0044 (16)0.0015 (15)0.0067 (15)
C30.044 (3)0.059 (3)0.036 (3)0.003 (3)−0.009 (2)0.008 (3)
C40.084 (6)0.095 (6)0.081 (6)0.037 (5)−0.007 (4)0.029 (5)
O20.055 (2)0.049 (2)0.052 (3)−0.0136 (19)−0.0077 (19)−0.0190 (19)
C50.094 (7)0.030 (4)0.036 (5)−0.014 (4)−0.004 (5)−0.004 (3)
C60.132 (12)0.045 (6)0.099 (10)−0.003 (7)−0.033 (9)−0.033 (6)
Si10.0339 (7)0.0310 (6)0.0252 (7)−0.0036 (5)−0.0027 (5)−0.0028 (5)
C110.034 (2)0.031 (2)0.021 (2)−0.0069 (18)0.0018 (18)−0.0018 (17)
C120.045 (3)0.028 (2)0.025 (3)−0.007 (2)−0.002 (2)0.0024 (18)
C130.057 (3)0.033 (3)0.035 (3)−0.013 (2)−0.003 (2)0.010 (2)
C140.060 (4)0.063 (4)0.036 (3)−0.020 (3)0.007 (3)0.023 (3)
C150.056 (4)0.086 (5)0.041 (4)−0.003 (3)0.023 (3)0.018 (3)
C160.041 (3)0.058 (3)0.034 (3)−0.001 (2)0.012 (2)0.010 (2)
C210.030 (2)0.032 (2)0.026 (3)0.0004 (18)0.0064 (18)0.0049 (18)
C220.037 (3)0.030 (2)0.039 (3)0.0019 (19)0.008 (2)−0.003 (2)
C230.057 (4)0.033 (3)0.057 (4)0.003 (2)0.014 (3)−0.012 (2)
C240.052 (4)0.043 (3)0.079 (5)0.019 (3)0.011 (3)−0.005 (3)
C250.053 (4)0.061 (4)0.065 (4)0.027 (3)−0.002 (3)−0.003 (3)
C260.038 (3)0.052 (3)0.041 (3)0.012 (2)−0.003 (2)−0.006 (2)
C310.031 (2)0.028 (2)0.020 (2)−0.0023 (17)0.0001 (17)0.0026 (17)
C320.041 (3)0.031 (2)0.021 (2)0.0034 (19)0.0008 (19)0.0029 (17)
C330.047 (3)0.027 (2)0.040 (3)0.008 (2)0.001 (2)−0.002 (2)
C340.053 (3)0.028 (2)0.035 (3)0.004 (2)−0.003 (2)0.011 (2)
C350.045 (3)0.042 (3)0.024 (3)0.002 (2)0.004 (2)0.014 (2)
C360.038 (3)0.035 (2)0.021 (2)0.0049 (19)0.0057 (19)0.0072 (18)
C410.038 (2)0.036 (2)0.015 (2)0.009 (2)0.0063 (17)0.0042 (18)
C420.037 (3)0.046 (3)0.024 (3)0.003 (2)0.001 (2)0.005 (2)
C430.038 (3)0.072 (4)0.041 (3)0.004 (3)0.007 (2)0.018 (3)
C440.045 (3)0.084 (5)0.040 (4)0.020 (3)0.020 (3)0.005 (3)
C450.056 (4)0.060 (4)0.040 (3)0.019 (3)0.017 (3)−0.005 (3)
C460.043 (3)0.045 (3)0.030 (3)0.008 (2)0.007 (2)−0.002 (2)
P30.0301 (5)0.0218 (5)0.0161 (5)−0.0007 (4)0.0033 (4)−0.0019 (4)
P40.0267 (5)0.0284 (5)0.0205 (6)−0.0004 (5)0.0031 (4)0.0003 (4)
C510.029 (2)0.034 (2)0.019 (2)−0.0031 (18)0.0037 (17)−0.0031 (17)
C610.039 (2)0.025 (2)0.017 (2)0.0018 (18)−0.0016 (18)−0.0010 (16)
C620.034 (2)0.035 (2)0.022 (2)0.0029 (18)0.0018 (18)0.0007 (17)
C630.044 (3)0.053 (3)0.026 (3)0.009 (2)0.009 (2)−0.004 (2)
C640.065 (4)0.047 (3)0.034 (3)0.016 (3)0.014 (3)−0.011 (2)
C650.076 (4)0.027 (2)0.038 (3)0.005 (2)0.010 (3)−0.008 (2)
C660.052 (3)0.030 (2)0.025 (3)−0.001 (2)0.007 (2)−0.0047 (18)
C710.028 (2)0.027 (2)0.022 (2)−0.0008 (17)0.0009 (17)0.0008 (17)
C720.043 (3)0.031 (2)0.028 (3)0.002 (2)−0.005 (2)−0.0050 (19)
C730.050 (3)0.026 (2)0.044 (3)0.001 (2)−0.006 (2)−0.004 (2)
C740.043 (3)0.030 (2)0.036 (3)−0.004 (2)−0.005 (2)0.010 (2)
C750.039 (3)0.037 (3)0.028 (3)0.000 (2)0.003 (2)0.009 (2)
C760.037 (2)0.033 (2)0.019 (2)0.0016 (19)0.0038 (18)0.0018 (17)
C810.029 (2)0.045 (3)0.023 (3)−0.009 (2)0.0001 (18)0.0031 (19)
C820.035 (3)0.046 (3)0.053 (4)−0.009 (2)0.003 (2)0.011 (2)
C830.053 (4)0.049 (3)0.071 (5)−0.016 (3)−0.005 (3)0.019 (3)
C840.043 (3)0.087 (5)0.062 (4)−0.029 (3)−0.001 (3)0.026 (4)
C850.035 (3)0.096 (5)0.051 (4)−0.017 (3)0.010 (3)0.006 (3)
C860.029 (3)0.068 (4)0.037 (3)−0.006 (2)0.007 (2)0.001 (3)
C910.033 (2)0.043 (3)0.026 (3)0.006 (2)0.0038 (19)0.002 (2)
C920.051 (3)0.052 (3)0.035 (3)0.019 (3)−0.001 (2)−0.008 (2)
C930.072 (4)0.061 (4)0.054 (4)0.029 (3)−0.004 (3)−0.019 (3)
C940.079 (5)0.065 (4)0.079 (5)0.044 (4)0.005 (4)−0.008 (4)
C950.078 (5)0.086 (5)0.064 (5)0.050 (4)−0.010 (4)0.001 (4)
C960.058 (4)0.066 (4)0.037 (3)0.031 (3)−0.008 (3)−0.001 (3)
C1010.060 (7)0.139 (13)0.111 (12)−0.025 (8)−0.002 (8)0.018 (10)
C1020.058 (7)0.133 (12)0.113 (12)−0.033 (7)0.004 (7)0.011 (9)
C1030.127 (13)0.102 (11)0.106 (12)0.029 (10)−0.029 (10)0.029 (9)
C1040.063 (8)0.095 (10)0.21 (2)0.030 (7)0.009 (11)0.033 (13)
C1050.151 (17)0.082 (10)0.172 (19)0.023 (10)0.102 (14)0.015 (11)
C1060.074 (9)0.187 (18)0.104 (12)−0.027 (10)0.013 (8)0.002 (11)
Geometric parameters (Å, °) top
Mo1—N32.007 (4)C41—C421.390 (7)
Mo1—N12.027 (4)C41—C461.398 (7)
Mo1—P12.4485 (11)C42—C431.391 (7)
Mo1—P22.4506 (11)C42—H420.9400
Mo1—P32.4755 (11)C43—C441.371 (9)
Mo1—P42.4801 (11)C43—H430.9400
N1—N21.124 (5)C44—C451.376 (9)
N3—N41.129 (5)C44—H440.9400
C1—P11.840 (5)C45—C461.391 (7)
C1—Si11.864 (5)C45—H450.9400
C1—H1A0.9800C46—H460.9400
C1—H1B0.9800P3—C611.833 (5)
P1—C211.839 (5)P3—C711.842 (4)
P1—C111.854 (5)P3—C511.844 (4)
C2—P21.839 (4)P4—C911.820 (5)
C2—Si11.856 (5)P4—C811.834 (5)
C2—H2A0.9800P4—C511.854 (4)
C2—H2B0.9800C51—H51A0.9800
P2—C311.844 (4)C51—H51B0.9800
P2—C411.853 (4)C61—C621.394 (6)
O1—C31.427 (6)C61—C661.399 (6)
O1—Si11.624 (4)C62—C631.389 (7)
C3—C41.481 (9)C62—H620.9400
C3—H3A0.9800C63—C641.381 (8)
C3—H3B0.9800C63—H630.9400
C4—H4A0.9700C64—C651.375 (8)
C4—H4B0.9700C64—H640.9400
C4—H4C0.9700C65—C661.396 (7)
O2—C5'1.372 (19)C65—H650.9400
O2—C51.401 (9)C66—H660.9400
O2—Si11.637 (4)C71—C761.390 (6)
C5—C61.431 (11)C71—C721.400 (6)
C5—H5A0.9800C72—C731.384 (7)
C5—H5B0.9800C72—H720.9400
C6—H6A0.9700C73—C741.373 (7)
C6—H6B0.9700C73—H730.9400
C6—H6C0.9700C74—C751.383 (7)
C5'—C6'1.46 (2)C74—H740.9400
C5'—H5C0.9800C75—C761.385 (6)
C5'—H5D0.9800C75—H750.9400
C6'—H6D0.9700C76—H760.9400
C6'—H6E0.9700C81—C821.394 (7)
C6'—H6F0.9700C81—C861.403 (7)
C11—C121.389 (6)C82—C831.392 (7)
C11—C161.396 (7)C82—H820.9400
C12—C131.386 (7)C83—C841.384 (10)
C12—H120.9400C83—H830.9400
C13—C141.383 (8)C84—C851.369 (10)
C13—H130.9400C84—H840.9400
C14—C151.373 (9)C85—C861.390 (8)
C14—H140.9400C85—H850.9400
C15—C161.398 (7)C86—H860.9400
C15—H150.9400C91—C921.387 (7)
C16—H160.9400C91—C961.391 (7)
C21—C261.387 (7)C92—C931.379 (8)
C21—C221.394 (7)C92—H920.9400
C22—C231.378 (7)C93—C941.375 (9)
C22—H220.9400C93—H930.9400
C23—C241.382 (9)C94—C951.374 (10)
C23—H230.9400C94—H940.9400
C24—C251.377 (9)C95—C961.381 (8)
C24—H240.9400C95—H950.9400
C25—C261.394 (8)C96—H960.9400
C25—H250.9400C101—C1021.330 (12)
C26—H260.9400C101—C1061.332 (12)
C31—C321.399 (6)C101—H1010.9400
C31—C361.404 (6)C102—C1031.315 (12)
C32—C331.381 (6)C102—H1020.9400
C32—H320.9400C103—C1041.353 (12)
C33—C341.379 (7)C103—H1030.9400
C33—H330.9400C104—C1051.358 (13)
C34—C351.384 (7)C104—H1040.9400
C34—H340.9400C105—C1061.323 (13)
C35—C361.387 (6)C105—H1050.9400
C35—H350.9400C106—H1060.9400
C36—H360.9400
N3—Mo1—N1174.95 (15)C35—C34—H34119.9
N3—Mo1—P186.59 (12)C34—C35—C36120.0 (5)
N1—Mo1—P192.12 (11)C34—C35—H35120.0
N3—Mo1—P283.99 (11)C36—C35—H35120.0
N1—Mo1—P291.22 (11)C35—C36—C31120.7 (5)
P1—Mo1—P293.63 (4)C35—C36—H36119.6
N3—Mo1—P397.83 (10)C31—C36—H36119.6
N1—Mo1—P387.16 (10)C42—C41—C46117.6 (4)
P1—Mo1—P396.52 (4)C42—C41—P2118.6 (4)
P2—Mo1—P3169.78 (4)C46—C41—P2123.8 (4)
N3—Mo1—P493.01 (11)C41—C42—C43120.9 (5)
N1—Mo1—P489.57 (11)C41—C42—H42119.5
P1—Mo1—P4163.94 (4)C43—C42—H42119.5
P2—Mo1—P4102.30 (4)C44—C43—C42120.8 (6)
P3—Mo1—P467.61 (4)C44—C43—H43119.6
N2—N1—Mo1179.3 (4)C42—C43—H43119.6
N4—N3—Mo1175.4 (4)C43—C44—C45119.2 (5)
P1—C1—Si1121.9 (2)C43—C44—H44120.4
P1—C1—H1A106.9C45—C44—H44120.4
Si1—C1—H1A106.9C44—C45—C46120.5 (5)
P1—C1—H1B106.9C44—C45—H45119.7
Si1—C1—H1B106.9C46—C45—H45119.7
H1A—C1—H1B106.7C45—C46—C41120.9 (5)
C21—P1—C1104.7 (2)C45—C46—H46119.6
C21—P1—C11100.3 (2)C41—C46—H46119.6
C1—P1—C1196.5 (2)C61—P3—C71102.3 (2)
C21—P1—Mo1118.99 (15)C61—P3—C51107.7 (2)
C1—P1—Mo1116.36 (16)C71—P3—C51100.3 (2)
C11—P1—Mo1116.60 (15)C61—P3—Mo1118.75 (14)
P2—C2—Si1119.0 (2)C71—P3—Mo1128.81 (14)
P2—C2—H2A107.6C51—P3—Mo195.22 (14)
Si1—C2—H2A107.6C91—P4—C81101.8 (2)
P2—C2—H2B107.6C91—P4—C51107.2 (2)
Si1—C2—H2B107.6C81—P4—C51101.1 (2)
H2A—C2—H2B107.0C91—P4—Mo1117.41 (17)
C2—P2—C3199.7 (2)C81—P4—Mo1130.77 (16)
C2—P2—C41100.4 (2)C51—P4—Mo194.80 (14)
C31—P2—C41100.5 (2)P3—C51—P496.4 (2)
C2—P2—Mo1114.86 (15)P3—C51—H51A112.5
C31—P2—Mo1121.30 (15)P4—C51—H51A112.5
C41—P2—Mo1116.60 (14)P3—C51—H51B112.5
C3—O1—Si1126.0 (3)P4—C51—H51B112.5
O1—C3—C4109.4 (5)H51A—C51—H51B110.0
O1—C3—H3A109.8C62—C61—C66118.2 (4)
C4—C3—H3A109.8C62—C61—P3119.6 (3)
O1—C3—H3B109.8C66—C61—P3121.1 (4)
C4—C3—H3B109.8C63—C62—C61120.4 (5)
H3A—C3—H3B108.2C63—C62—H62119.8
C3—C4—H4A109.5C61—C62—H62119.8
C3—C4—H4B109.5C64—C63—C62120.8 (5)
H4A—C4—H4B109.5C64—C63—H63119.6
C3—C4—H4C109.5C62—C63—H63119.6
H4A—C4—H4C109.5C65—C64—C63119.7 (5)
H4B—C4—H4C109.5C65—C64—H64120.2
C5'—O2—C538.7 (19)C63—C64—H64120.2
C5'—O2—Si1147.5 (15)C64—C65—C66120.1 (5)
C5—O2—Si1125.5 (5)C64—C65—H65119.9
O2—C5—C6118.4 (9)C66—C65—H65119.9
O2—C5—H5A107.7C65—C66—C61120.8 (5)
C6—C5—H5A107.7C65—C66—H66119.6
O2—C5—H5B107.7C61—C66—H66119.6
C6—C5—H5B107.7C76—C71—C72118.2 (4)
H5A—C5—H5B107.1C76—C71—P3122.6 (3)
C5—C6—H6A109.5C72—C71—P3119.0 (3)
C5—C6—H6B109.5C73—C72—C71120.7 (5)
H6A—C6—H6B109.5C73—C72—H72119.7
C5—C6—H6C109.5C71—C72—H72119.7
H6A—C6—H6C109.5C74—C73—C72120.4 (5)
H6B—C6—H6C109.5C74—C73—H73119.8
O2—C5'—C6'105 (2)C72—C73—H73119.8
O2—C5'—H5C110.7C73—C74—C75119.8 (4)
C6'—C5'—H5C110.7C73—C74—H74120.1
O2—C5'—H5D110.7C75—C74—H74120.1
C6'—C5'—H5D110.7C74—C75—C76120.2 (5)
H5C—C5'—H5D108.8C74—C75—H75119.9
C5'—C6'—H6D109.5C76—C75—H75119.9
C5'—C6'—H6E109.5C75—C76—C71120.8 (4)
H6D—C6'—H6E109.5C75—C76—H76119.6
C5'—C6'—H6F109.5C71—C76—H76119.6
H6D—C6'—H6F109.5C82—C81—C86118.2 (5)
H6E—C6'—H6F109.5C82—C81—P4118.2 (4)
O1—Si1—O2106.6 (2)C86—C81—P4123.6 (4)
O1—Si1—C2114.6 (2)C83—C82—C81121.4 (6)
O2—Si1—C2106.9 (2)C83—C82—H82119.3
O1—Si1—C1108.3 (2)C81—C82—H82119.3
O2—Si1—C1108.3 (2)C84—C83—C82119.1 (6)
C2—Si1—C1112.0 (2)C84—C83—H83120.4
C12—C11—C16118.5 (4)C82—C83—H83120.4
C12—C11—P1118.2 (4)C85—C84—C83120.5 (6)
C16—C11—P1123.4 (4)C85—C84—H84119.7
C13—C12—C11121.2 (5)C83—C84—H84119.7
C13—C12—H12119.4C84—C85—C86120.8 (6)
C11—C12—H12119.4C84—C85—H85119.6
C14—C13—C12120.2 (5)C86—C85—H85119.6
C14—C13—H13119.9C85—C86—C81120.0 (6)
C12—C13—H13119.9C85—C86—H86120.0
C15—C14—C13119.3 (5)C81—C86—H86120.0
C15—C14—H14120.3C92—C91—C96117.0 (5)
C13—C14—H14120.3C92—C91—P4117.8 (4)
C14—C15—C16121.1 (6)C96—C91—P4125.2 (4)
C14—C15—H15119.5C93—C92—C91122.0 (5)
C16—C15—H15119.5C93—C92—H92119.0
C11—C16—C15119.8 (5)C91—C92—H92119.0
C11—C16—H16120.1C94—C93—C92119.8 (6)
C15—C16—H16120.1C94—C93—H93120.1
C26—C21—C22118.0 (4)C92—C93—H93120.1
C26—C21—P1124.2 (4)C95—C94—C93119.7 (6)
C22—C21—P1117.8 (3)C95—C94—H94120.1
C23—C22—C21121.7 (5)C93—C94—H94120.1
C23—C22—H22119.2C94—C95—C96120.1 (6)
C21—C22—H22119.2C94—C95—H95120.0
C22—C23—C24119.9 (5)C96—C95—H95120.0
C22—C23—H23120.1C95—C96—C91121.5 (6)
C24—C23—H23120.1C95—C96—H96119.3
C25—C24—C23119.4 (5)C91—C96—H96119.3
C25—C24—H24120.3C102—C101—C106123.5 (14)
C23—C24—H24120.3C102—C101—H101118.2
C24—C25—C26120.8 (6)C106—C101—H101118.2
C24—C25—H25119.6C103—C102—C101118.1 (13)
C26—C25—H25119.6C103—C102—H102121.0
C21—C26—C25120.3 (5)C101—C102—H102121.0
C21—C26—H26119.9C102—C103—C104119.8 (13)
C25—C26—H26119.9C102—C103—H103120.1
C32—C31—C36117.8 (4)C104—C103—H103120.1
C32—C31—P2120.0 (3)C103—C104—C105120.5 (14)
C36—C31—P2121.9 (3)C103—C104—H104119.7
C33—C32—C31121.1 (5)C105—C104—H104119.7
C33—C32—H32119.4C106—C105—C104119.0 (14)
C31—C32—H32119.4C106—C105—H105120.5
C34—C33—C32120.1 (5)C104—C105—H105120.5
C34—C33—H33119.9C105—C106—C101118.1 (14)
C32—C33—H33119.9C105—C106—H106120.9
C33—C34—C35120.2 (4)C101—C106—H106120.9
C33—C34—H34119.9
references
References top

Bogza, M., Oeser, T. & Bluemel, J. (2005). J. Organomet. Chem. pp. 3383–3389.

Leigh, G. J. & Pickett, C. J. (1977). J. Chem. Soc. Dalton Trans. pp. 1797–1800.

MacKay, A. & Fryzuk, M. D. (2004). Chem. Rev. pp. 385–401.

Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122.

Stoe & Cie (1998). X-SHAPE and IPDS Program Package. Stoe & Cie, Darmstadt, Germany.