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The title complex, [Mo2(C5H5)2(CH3O)2(C4H11Si)2(NO)2], is formed in high yield by treating [CpMo(NO)(CH2SiMe3)2] (Cp is cyclo­penta­dienyl) with methanol. The nitro­syl ligands are nearly linear [O—N—Mo 170.1 (4) and 170.1 (5)°], with short Mo—N bonds [1.769 (4) and 1.776 (4) Å] and long N—O bonds [1.216 (5) and 1.201 (4) Å]. The central four-membered Mo2O2 ring exhibits an average Mo—O bond length of 2.15 Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S010827010200865X/fr1372sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S010827010200865X/fr1372Isup2.hkl
Contains datablock I

CCDC reference: 192941

Comment top

The title compound, [CpMo(NO)(CH2SiMe3)]2(µ-OMe)2, (I), is readily formed in high yield by protonation of an alkyl ligand in CpMo(NO)(CH2SiMe3)2 by MeOH. SiMe4 is generated as a byproduct. Only 30 min of reaction time in neat methanol are needed to effect complete conversion. Interestingly, no evidence for the formation of CpMo(NO)(OMe)2 is found, even with longer reaction times. Surprisingly, the title complex is isolated as an orange-yellow crystalline solid, even though it is bright red in solution. We have observed similar disparate colour differences before, the usual cause being dimer formation in the solid state. For instance, Cp*Mo(NO)Cl2 (Cp* is pentamethylcyclopentadienyl) exists as a green solution in CH2Cl2, presumably as a monomer, but is an orange-red dimer in the solid state, as confirmed by X-ray crystallography (Dryden et al., 1991). Similar to (I), Cp*Mo(NO)Me2 is red in solution and yellow in the solid state (Sharp et al., 2001), where it is likely to exist as a nitrosyl-bridged oligomer. \sch

X-ray crystallographic analysis confirms that (I) is dimeric in the solid state. The metal-nitrosyl linkages of (I) are both nearly linear [Mo1—N1—O1 170.1 (4)° and Mo2—N2—O2 170.1 (5)°], thereby indicating that the nitrosyl ligands are acting as 3 e donors. Both exhibit short Mo—N distances [Mo1—N1 1.769 (4) Å and Mo2—N2 1.776 (4) Å] and long N—O distances [N1—O1 1.216 (5) Å and N2—O2 1.201 (4) Å] relative to most nitrosyl complexes (Feltham & Enemark, 1981), due to strong π back-donation from the Mo centres. These NO-ligand metrical parameters are almost identical to those observed in CpMo(NO)(CH2SiMe3)(p-FC6H4O) (Hayton et al., 2002).

The most interesting structural feature of (I) is the central four-membered Mo2O2 ring. The four Mo—O distances are 2.093 (3) (Mo1—O3), 2.144 (3) (Mo2—O3), 2.160 (3) (Mo2—O4) and 2.216 (4) Å (Mo1—O4), with an average of 2.15 Å. These M—O distances are consistent with those reported for other bridging alkoxides, such as [W2(OPh)3(CO)6]3- [mean W—O 2.22 Å; Darensbourg et al., 1988] and [Mo2(OPh-4-Me)7(NHMe2)2]- [mean Mo—O(bridging) 2.11 Å; Coffindaffer et al., 1985]. The related nitrosyl complex CpMo(NO)(CH2SiMe3)(p-FC6H4O) exhibits an Mo—O distance of 1.945 (2) Å (Hayton et al., 2002), shorter than the values seen in (I). This is as expected, since the Mo—O bond in CpMo(NO)(CH2SiMe3)(p-FC6H4O) exhibits some multiple-bond character.

Experimental top

In a Schlenk tube, under anaerobic and anhydrous conditions, CpMo(NO)(CH2SiMe3)2 (356 mg, 0.97 mmol) was dissolved in MeOH (25 ml). After being stirred for 30 min at room temperature, the purple solution had turned bright red. The volume of the solution was reduced to 5 ml in vacuo, and the Schlenk tube was cooled to 243 K overnight to induce the deposition of orange crystals of (I) (235 mg, 80% yield) which were suitable for X-ray analysis. Compound (I) is moderately air- and temperature-sensitive and is best stored at 243 K under a dinitrogen atmosphere. Spectroscopic analysis: IR (Nujol): 1590 cm-1 (νNO); 1H NMR (200 MHz, CD3CN, δ, p.p.m.): 5.95 (s, 5H, C5H5), 4.74 (br s, 3H, OCH3), 1.79 (dd, 2H, CH2SiMe3), 0.03 (s, 9H, SiMe3); 13C NMR (200 MHz, CD3CN, δ, p.p.m.): 106.0 (C5H5), 79.6 (OCH3), 37.6 (CH2Si), 1.74 (SiCH3).

Refinement top

The positions of the H atoms on C12 were determined using the HFIX 137 function in SHELXL97 (Sheldrick, 1997). Subsequent refinements were carried out with the H atoms fixed in those positions, with C—H = 0.98 Å. Other H atoms? The absolute structure was determined by refinement of the Flack parameter (Flack, 1983) to 0.032 (4). The maximum and minimum peaks on the final difference Fourier map are adjacent to Mo2.

Computing details top

Data collection: D*TREK (Molecular Structure Corporation, 1997); cell refinement: D*TREK; data reduction: D*TREK; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: TEXSAN (Molecular Structure Corporation, 1997) and SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: TEXSAN.

Figures top
[Figure 1] Fig. 1. The molecular structure of (I) showing 50% probability ellipsoids. H atoms have been omitted for clarity.
Di-µ-methoxy-bis[(η5-cyclopentadienyl)(nitrosyl- κN)(trimethylsilylmethyl)molybdenum(III)] top
Crystal data top
[Mo2(C5H5)2(CH3O)2(C4H11Si)2(NO)2]Dx = 1.542 Mg m3
Mr = 618.58Mo Kα radiation, λ = 0.71069 Å
Orthorhombic, Pna21Cell parameters from 16401 reflections
a = 12.375 (2) Åθ = 2.0–30.5°
b = 15.248 (2) ŵ = 1.06 mm1
c = 14.119 (2) ÅT = 180 K
V = 2664.1 (6) Å3Plate, orange
Z = 40.30 × 0.20 × 0.03 mm
F(000) = 1264.00
Data collection top
Rigaku ADSC CCD area-detector
diffractometer
7079 independent reflections
Radiation source: X-ray tube4260 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.060
Detector resolution: 11.76 pixels mm-1θmax = 30.6°, θmin = 2.0°
area detector scansh = 1517
Absorption correction: multi-scan
D*TREK (Molecular Structure Corporation, 1997)
k = 2116
Tmin = 0.775, Tmax = 0.969l = 1618
24272 measured reflections
Refinement top
Refinement on F20 constraints
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.037Weighting scheme based on measured s.u.'s w = 1/[σ2(Fo2)]
wR(F2) = 0.063(Δ/σ)max = 0.002
S = 1.22Δρmax = 1.72 e Å3
7078 reflectionsΔρmin = 2.64 e Å3
270 parametersAbsolute structure: Flack (1983), 2844 Friedel pairs
0 restraintsAbsolute structure parameter: 0.032 (4)
Crystal data top
[Mo2(C5H5)2(CH3O)2(C4H11Si)2(NO)2]V = 2664.1 (6) Å3
Mr = 618.58Z = 4
Orthorhombic, Pna21Mo Kα radiation
a = 12.375 (2) ŵ = 1.06 mm1
b = 15.248 (2) ÅT = 180 K
c = 14.119 (2) Å0.30 × 0.20 × 0.03 mm
Data collection top
Rigaku ADSC CCD area-detector
diffractometer
7079 independent reflections
Absorption correction: multi-scan
D*TREK (Molecular Structure Corporation, 1997)
4260 reflections with I > 3σ(I)
Tmin = 0.775, Tmax = 0.969Rint = 0.060
24272 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.037H-atom parameters constrained
wR(F2) = 0.063Δρmax = 1.72 e Å3
S = 1.22Δρmin = 2.64 e Å3
7078 reflectionsAbsolute structure: Flack (1983), 2844 Friedel pairs
270 parametersAbsolute structure parameter: 0.032 (4)
0 restraints
Special details top

Experimental. Data were collected in 0.50° oscillations with 60.0 s exposures. A sweep of data was done using ϕ oscillations from 0.0 to 190.0° at χ = -90° and a second sweep was performed using ω oscillations between -23.0 and 18.0° at χ = 90.0°. The crystal-to-detector distance was 38.83 mm. The detector swing angle was -10.0°. The absorption correction is based on a three-dimensional analysis of symmetry-equivalent data and is performed along with batch scaling in a single step. The resulting transmission factors, therefore, include contributions from absorption, crystal decay, and detectable variations in beam intensity.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mo10.31576 (3)0.39487 (2)0.38910.01886 (9)
Mo20.25867 (3)0.57059 (2)0.53772 (5)0.01878 (9)
Si10.3084 (1)0.20452 (7)0.5286 (1)0.0270 (4)
Si20.2720 (1)0.78388 (8)0.4239 (1)0.0262 (4)
O10.1447 (3)0.2794 (2)0.3093 (3)0.037 (1)
O20.4758 (3)0.6528 (2)0.5445 (3)0.037 (1)
O30.2001 (3)0.4893 (2)0.4250 (2)0.0224 (9)
O40.3330 (2)0.4424 (2)0.5366 (3)0.0212 (7)
N10.2121 (3)0.3237 (2)0.3499 (3)0.026 (1)
N20.3891 (3)0.6190 (2)0.5331 (3)0.0199 (9)
C10.3454 (5)0.4580 (4)0.2423 (4)0.037 (2)
C20.3974 (5)0.5177 (3)0.3062 (4)0.034 (2)
C30.4826 (4)0.4759 (3)0.3510 (4)0.038 (2)
C40.4887 (5)0.3879 (3)0.3136 (4)0.035 (2)
C50.4072 (5)0.3766 (3)0.2480 (4)0.037 (2)
C60.2429 (5)0.5645 (3)0.7022 (3)0.034 (1)
C70.1593 (5)0.5077 (3)0.6673 (4)0.036 (2)
C80.0841 (5)0.5635 (4)0.6209 (4)0.039 (2)
C90.1207 (5)0.6495 (4)0.6200 (4)0.040 (2)
C100.2196 (5)0.6521 (3)0.6736 (4)0.035 (2)
C110.1006 (4)0.4957 (3)0.3793 (5)0.031 (1)
C120.4243 (4)0.4290 (3)0.5925 (4)0.030 (1)
C130.3928 (4)0.2759 (3)0.4509 (4)0.030 (2)
C140.1887 (5)0.2616 (3)0.5845 (4)0.048 (2)
C150.3948 (6)0.1593 (4)0.6283 (4)0.052 (2)
C160.2570 (5)0.1089 (3)0.4577 (4)0.047 (2)
C170.2087 (4)0.6736 (3)0.4338 (4)0.024 (1)
C180.4039 (4)0.7742 (3)0.3597 (4)0.036 (2)
C190.1826 (5)0.8568 (3)0.3523 (4)0.042 (2)
C200.2971 (5)0.8400 (3)0.5398 (5)0.051 (2)
H10.28190.46940.20280.044*
H20.37570.57880.31670.040*
H30.53020.50140.39920.045*
H40.54200.34340.33180.042*
H50.39310.32310.21150.044*
H60.30570.54600.73930.041*
H70.15490.44390.67400.043*
H80.01560.54390.59320.046*
H90.08560.69930.58860.048*
H100.26280.70440.68780.042*
H110.11180.51480.31360.037*
H120.05510.53850.41220.037*
H130.06490.43830.37950.037*
H140.48940.43950.55460.036*
H150.42480.36850.61590.036*
H160.42300.46960.64630.036*
H170.45490.29560.48840.036*
H180.41820.23970.39800.036*
H190.21410.31090.62300.058*
H200.14940.22000.62480.058*
H210.14050.28330.53470.058*
H220.45680.12810.60150.062*
H230.35160.11880.66660.062*
H240.42030.20770.66800.062*
H250.22070.13050.40040.057*
H260.20560.07510.49570.057*
H270.31770.07120.43940.057*
H280.13200.68450.44630.028*
H290.21680.64670.37120.028*
H300.39230.74560.29840.044*
H310.45440.73920.39760.044*
H320.43430.83290.34950.044*
H330.21590.91490.34630.051*
H340.11220.86240.38360.051*
H350.17240.83140.28900.051*
H360.32840.89800.52820.061*
H370.34710.80490.57770.061*
H380.22850.84650.57390.061*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.0210 (2)0.0146 (1)0.0211 (2)0.0004 (2)0.0012 (3)0.0019 (2)
Mo20.0212 (2)0.0155 (1)0.0196 (2)0.0020 (2)0.0024 (3)0.0028 (2)
Si10.0311 (8)0.0217 (6)0.0280 (9)0.0033 (6)0.0045 (9)0.0016 (7)
Si20.0268 (9)0.0188 (6)0.0330 (9)0.0010 (6)0.0018 (7)0.0004 (6)
O10.034 (2)0.037 (2)0.039 (3)0.012 (2)0.003 (2)0.019 (2)
O20.024 (2)0.039 (2)0.048 (3)0.012 (2)0.015 (2)0.012 (2)
O30.018 (2)0.021 (2)0.028 (2)0.003 (1)0.006 (2)0.006 (1)
O40.024 (2)0.020 (1)0.020 (2)0.006 (1)0.008 (2)0.006 (2)
N10.022 (2)0.018 (2)0.037 (3)0.005 (2)0.004 (2)0.006 (2)
N20.020 (2)0.028 (2)0.012 (2)0.001 (1)0.007 (2)0.003 (2)
C10.045 (4)0.045 (3)0.021 (3)0.006 (2)0.005 (3)0.011 (2)
C20.041 (3)0.020 (2)0.041 (4)0.007 (2)0.023 (3)0.006 (2)
C30.030 (3)0.035 (3)0.049 (4)0.017 (2)0.008 (3)0.004 (2)
C40.033 (3)0.028 (2)0.046 (4)0.000 (3)0.025 (2)0.014 (2)
C50.047 (4)0.034 (3)0.029 (3)0.010 (2)0.034 (2)0.008 (2)
C60.049 (3)0.036 (2)0.018 (2)0.008 (3)0.014 (3)0.007 (2)
C70.050 (4)0.038 (3)0.019 (3)0.007 (2)0.021 (3)0.008 (2)
C80.036 (4)0.050 (3)0.030 (4)0.004 (3)0.017 (3)0.005 (3)
C90.047 (4)0.039 (3)0.034 (4)0.027 (3)0.011 (3)0.008 (3)
C100.053 (4)0.034 (2)0.018 (3)0.005 (3)0.012 (3)0.016 (2)
C110.022 (3)0.030 (2)0.042 (4)0.002 (2)0.016 (3)0.010 (3)
C120.030 (3)0.028 (2)0.031 (3)0.007 (3)0.007 (2)0.006 (3)
C130.036 (3)0.013 (2)0.040 (4)0.008 (2)0.002 (3)0.005 (2)
C140.032 (3)0.046 (3)0.066 (5)0.005 (3)0.013 (3)0.012 (3)
C150.062 (5)0.048 (4)0.044 (4)0.002 (3)0.026 (3)0.019 (3)
C160.061 (4)0.022 (2)0.059 (4)0.016 (3)0.003 (4)0.001 (2)
C170.028 (3)0.017 (2)0.025 (3)0.004 (2)0.010 (2)0.002 (2)
C180.028 (3)0.037 (3)0.045 (4)0.005 (3)0.001 (2)0.001 (3)
C190.030 (3)0.026 (2)0.071 (5)0.005 (2)0.003 (3)0.022 (2)
C200.082 (5)0.029 (2)0.041 (3)0.018 (3)0.002 (5)0.015 (3)
Geometric parameters (Å, º) top
Mo1—O32.093 (3)C5—H50.98
Mo1—O42.216 (4)C6—C71.436 (9)
Mo1—N11.769 (4)C6—C101.425 (7)
Mo1—C12.315 (6)C6—H60.98
Mo1—C22.428 (5)C7—C81.421 (9)
Mo1—C32.465 (6)C7—H70.98
Mo1—C42.393 (6)C8—C91.388 (8)
Mo1—C52.307 (5)C8—H80.98
Mo1—C132.227 (5)C9—C101.441 (9)
Mo2—O32.144 (3)C9—H90.98
Mo2—O42.160 (3)C10—H100.98
Mo2—N21.776 (4)C11—H110.98
Mo2—C62.332 (5)C11—H120.98
Mo2—C72.404 (5)C11—H130.98
Mo2—C82.462 (6)C12—H140.98
Mo2—C92.390 (6)C12—H150.98
Mo2—C102.337 (5)C12—H160.98
Mo2—C172.237 (5)C13—H170.98
Si1—C131.865 (6)C13—H180.98
Si1—C141.890 (6)C14—H190.98
Si1—C151.897 (7)C14—H200.98
Si1—C161.880 (5)C14—H210.98
Si2—C171.860 (5)C15—H220.98
Si2—C181.874 (6)C15—H230.98
Si2—C191.866 (6)C15—H240.98
Si2—C201.872 (7)C16—H250.98
O1—N11.216 (5)C16—H260.98
O2—N21.201 (4)C16—H270.98
O3—C111.393 (6)C17—H280.98
O4—C121.394 (6)C17—H290.98
C1—C21.435 (8)C18—H300.98
C1—C51.459 (8)C18—H310.98
C1—H10.98C18—H320.98
C2—C31.385 (8)C19—H330.98
C2—H20.98C19—H340.98
C3—C41.444 (8)C19—H350.98
C3—H30.98C20—H360.98
C4—C51.380 (9)C20—H370.98
C4—H40.98C20—H380.98
O1···C4i3.200 (7)O2···C5iii3.249 (7)
O1···C10ii3.203 (7)C3···C19iv3.554 (8)
O3—Mo1—O467.2 (1)Mo1—C3—H3123.4
O3—Mo1—N190.1 (2)C2—C3—C4107.5 (5)
O3—Mo1—C192.2 (2)C2—C3—H3126.3
O3—Mo1—C282.5 (2)C4—C3—H3126.2
O3—Mo1—C3106.3 (2)Mo1—C4—C375.5 (3)
O3—Mo1—C4138.6 (2)Mo1—C4—C569.5 (3)
O3—Mo1—C5128.9 (2)Mo1—C4—H4121.1
O3—Mo1—C13139.3 (2)C3—C4—C5108.8 (5)
O4—Mo1—N1124.4 (2)C3—C4—H4125.6
O4—Mo1—C1133.7 (2)C5—C4—H4125.6
O4—Mo1—C299.2 (2)Mo1—C5—C171.9 (3)
O4—Mo1—C387.8 (2)Mo1—C5—C476.4 (4)
O4—Mo1—C4110.3 (2)Mo1—C5—H5117.9
O4—Mo1—C5143.5 (2)C1—C5—C4108.3 (5)
O4—Mo1—C1381.8 (2)C1—C5—H5125.8
N1—Mo1—C195.2 (2)C4—C5—H5125.8
N1—Mo1—C2128.6 (2)Mo2—C6—C775.1 (3)
N1—Mo1—C3147.8 (2)Mo2—C6—C1072.4 (3)
N1—Mo1—C4118.8 (2)Mo2—C6—H6118.6
N1—Mo1—C590.7 (2)C7—C6—C10108.8 (6)
N1—Mo1—C1386.2 (2)C7—C6—H6125.6
C1—Mo1—C235.1 (2)C10—C6—H6125.6
C1—Mo1—C357.5 (2)Mo2—C7—C669.6 (3)
C1—Mo1—C458.5 (2)Mo2—C7—C875.2 (3)
C1—Mo1—C536.8 (2)Mo2—C7—H7119.9
C1—Mo1—C13128.4 (2)C6—C7—C8105.6 (5)
C2—Mo1—C332.9 (2)C6—C7—H7127.3
C2—Mo1—C456.5 (2)C8—C7—H7127.1
C2—Mo1—C558.2 (2)Mo2—C8—C770.8 (3)
C2—Mo1—C13129.7 (2)Mo2—C8—C970.6 (4)
C3—Mo1—C434.5 (2)Mo2—C8—H8125.6
C3—Mo1—C557.4 (2)C7—C8—C9110.9 (6)
C3—Mo1—C1397.8 (2)C7—C8—H8124.6
C4—Mo1—C534.1 (2)C9—C8—H8124.6
C4—Mo1—C1375.9 (2)Mo2—C9—C876.2 (3)
C5—Mo1—C1391.7 (2)Mo2—C9—C1070.3 (3)
O3—Mo2—O467.4 (1)Mo2—C9—H9119.1
O3—Mo2—N2121.4 (2)C8—C9—C10107.4 (6)
O3—Mo2—C6133.5 (2)C8—C9—H9126.3
O3—Mo2—C799.3 (2)C10—C9—H9126.4
O3—Mo2—C891.8 (2)Mo2—C10—C672.0 (3)
O3—Mo2—C9114.2 (2)Mo2—C10—C974.3 (3)
O3—Mo2—C10147.9 (2)Mo2—C10—H10119.2
O3—Mo2—C1779.9 (1)C6—C10—C9107.1 (5)
O4—Mo2—N289.4 (1)C6—C10—H10126.5
O4—Mo2—C690.4 (2)C9—C10—H10126.4
O4—Mo2—C782.1 (2)O3—C11—H11109.5
O4—Mo2—C8109.7 (2)O3—C11—H12109.5
O4—Mo2—C9139.8 (2)O3—C11—H13109.6
O4—Mo2—C10125.1 (2)H11—C11—H12109.4
O4—Mo2—C17138.4 (2)H11—C11—H13109.4
N2—Mo2—C697.4 (2)H12—C11—H13109.5
N2—Mo2—C7131.2 (2)O4—C12—H14109.5
N2—Mo2—C8146.4 (2)O4—C12—H15109.5
N2—Mo2—C9117.2 (2)O4—C12—H16109.5
N2—Mo2—C1089.8 (2)H14—C12—H15109.5
N2—Mo2—C1786.3 (2)H14—C12—H16109.4
C6—Mo2—C735.3 (2)H15—C12—H16109.5
C6—Mo2—C856.6 (2)Mo1—C13—Si1117.8 (3)
C6—Mo2—C958.4 (2)Mo1—C13—H17107.3
C6—Mo2—C1035.5 (2)Mo1—C13—H18107.3
C6—Mo2—C17131.1 (2)Si1—C13—H17107.4
C7—Mo2—C833.9 (2)Si1—C13—H18107.4
C7—Mo2—C957.7 (2)H17—C13—H18109.4
C7—Mo2—C1058.8 (2)Si1—C14—H19109.5
C7—Mo2—C17129.6 (2)Si1—C14—H20109.5
C8—Mo2—C933.2 (2)Si1—C14—H21109.5
C8—Mo2—C1056.6 (2)H19—C14—H20109.5
C8—Mo2—C1795.8 (2)H19—C14—H21109.5
C9—Mo2—C1035.5 (2)H20—C14—H21109.4
C9—Mo2—C1776.5 (2)Si1—C15—H22109.4
C10—Mo2—C1796.2 (2)Si1—C15—H23109.4
C13—Si1—C14114.6 (2)Si1—C15—H24109.4
C13—Si1—C15109.5 (3)H22—C15—H23109.5
C13—Si1—C16109.1 (3)H22—C15—H24109.6
C14—Si1—C15107.4 (3)H23—C15—H24109.6
C14—Si1—C16108.3 (3)Si1—C16—H25109.5
C15—Si1—C16107.7 (3)Si1—C16—H26109.6
C17—Si2—C18109.4 (3)Si1—C16—H27109.6
C17—Si2—C19109.3 (3)H25—C16—H26109.3
C17—Si2—C20114.7 (3)H25—C16—H27109.3
C18—Si2—C19107.6 (3)H26—C16—H27109.5
C18—Si2—C20108.3 (3)Mo2—C17—Si2124.6 (3)
C19—Si2—C20107.4 (3)Mo2—C17—H28105.6
Mo1—O3—Mo2110.2 (2)Mo2—C17—H29105.6
Mo1—O3—C11122.7 (3)Si2—C17—H28105.6
Mo2—O3—C11127.1 (3)Si2—C17—H29105.5
Mo1—O4—Mo2105.2 (2)H28—C17—H29109.4
Mo1—O4—C12124.2 (3)Si2—C18—H30109.5
Mo2—O4—C12118.3 (3)Si2—C18—H31109.5
Mo1—N1—O1170.1 (4)Si2—C18—H32109.5
Mo2—N2—O2170.1 (5)H30—C18—H31109.5
Mo1—C1—C276.8 (4)H30—C18—H32109.4
Mo1—C1—C571.3 (3)H31—C18—H32109.4
Mo1—C1—H1117.1Si2—C19—H33109.6
C2—C1—C5105.7 (6)Si2—C19—H34109.6
C2—C1—H1127.2Si2—C19—H35109.5
C5—C1—H1127.1H33—C19—H34109.5
Mo1—C2—C168.1 (3)H33—C19—H35109.3
Mo1—C2—C375.0 (3)H34—C19—H35109.3
Mo1—C2—H2123.1Si2—C20—H36109.4
C1—C2—C3109.6 (5)Si2—C20—H37109.4
C1—C2—H2125.2Si2—C20—H38109.3
C3—C2—H2125.2H36—C20—H37109.6
Mo1—C3—C272.1 (3)H36—C20—H38109.5
Mo1—C3—C470.0 (3)H37—C20—H38109.6
Mo1—O3—Mo2—O425.4 (1)N1—Mo1—C5—C197.7 (4)
Mo1—O3—Mo2—N249.1 (2)N1—Mo1—C5—C4147.5 (4)
Mo1—O3—Mo2—C692.8 (3)N2—Mo2—O3—C11130.6 (4)
Mo1—O3—Mo2—C7102.7 (2)N2—Mo2—O4—C1242.4 (4)
Mo1—O3—Mo2—C8136.0 (2)N2—Mo2—C6—C7165.1 (4)
Mo1—O3—Mo2—C9161.4 (2)N2—Mo2—C6—C1079.2 (4)
Mo1—O3—Mo2—C10146.0 (3)N2—Mo2—C7—C619.8 (5)
Mo1—O3—Mo2—C17128.4 (2)N2—Mo2—C7—C8133.1 (4)
Mo1—O4—Mo2—O323.2 (1)N2—Mo2—C8—C783.9 (5)
Mo1—O4—Mo2—N2101.5 (2)N2—Mo2—C8—C937.6 (6)
Mo1—O4—Mo2—C6161.1 (2)N2—Mo2—C9—C8157.7 (4)
Mo1—O4—Mo2—C7126.8 (2)N2—Mo2—C9—C1043.2 (4)
Mo1—O4—Mo2—C8106.7 (2)N2—Mo2—C10—C6103.1 (4)
Mo1—O4—Mo2—C9124.5 (3)N2—Mo2—C10—C9142.5 (4)
Mo1—O4—Mo2—C10169.2 (2)C1—Mo1—O3—C1167.3 (4)
Mo1—O4—Mo2—C1717.8 (3)C1—Mo1—O4—C1294.9 (4)
Mo1—C1—C2—C364.0 (5)C1—Mo1—C2—C3118.8 (5)
Mo1—C1—C5—C468.3 (4)C1—Mo1—C3—C236.7 (4)
Mo1—C2—C1—C565.9 (4)C1—Mo1—C3—C480.4 (4)
Mo1—C2—C3—C461.4 (4)C1—Mo1—C4—C377.3 (4)
Mo1—C3—C2—C159.7 (4)C1—Mo1—C4—C539.6 (3)
Mo1—C3—C4—C562.0 (4)C1—Mo1—C5—C4114.8 (5)
Mo1—C4—C3—C262.7 (4)C1—C2—Mo1—C3118.8 (5)
Mo1—C4—C5—C165.3 (4)C1—C2—Mo1—C481.5 (4)
Mo1—C5—C1—C269.8 (4)C1—C2—Mo1—C540.8 (4)
Mo1—C5—C4—C365.8 (4)C1—C2—Mo1—C13102.9 (4)
Mo1—C13—Si1—C1423.0 (4)C1—C2—C3—C41.7 (7)
Mo1—C13—Si1—C15143.7 (3)C1—C5—Mo1—C238.9 (4)
Mo1—C13—Si1—C1698.6 (3)C1—C5—Mo1—C377.9 (4)
Mo2—O3—Mo1—O424.7 (1)C1—C5—Mo1—C4114.8 (5)
Mo2—O3—Mo1—N1152.4 (2)C1—C5—Mo1—C13176.1 (4)
Mo2—O3—Mo1—C1112.4 (2)C1—C5—C4—C30.4 (7)
Mo2—O3—Mo1—C278.6 (2)C2—Mo1—O3—C11101.1 (4)
Mo2—O3—Mo1—C355.7 (2)C2—Mo1—O4—C1287.1 (4)
Mo2—O3—Mo1—C470.6 (3)C2—Mo1—C1—C5111.9 (6)
Mo2—O3—Mo1—C5116.7 (2)C2—Mo1—C3—C4117.0 (5)
Mo2—O3—Mo1—C1368.2 (3)C2—Mo1—C4—C335.4 (3)
Mo2—O4—Mo1—O323.8 (1)C2—Mo1—C4—C581.5 (4)
Mo2—O4—Mo1—N197.2 (2)C2—Mo1—C5—C475.9 (4)
Mo2—O4—Mo1—C146.2 (3)C2—C1—Mo1—C334.3 (3)
Mo2—O4—Mo1—C254.0 (2)C2—C1—Mo1—C475.3 (4)
Mo2—O4—Mo1—C384.9 (2)C2—C1—Mo1—C5111.9 (6)
Mo2—O4—Mo1—C4111.6 (2)C2—C1—Mo1—C13106.8 (4)
Mo2—O4—Mo1—C5101.4 (3)C2—C1—C5—C41.4 (7)
Mo2—O4—Mo1—C13176.9 (2)C2—C3—Mo1—C4117.0 (5)
Mo2—C6—C7—C867.3 (4)C2—C3—Mo1—C580.7 (4)
Mo2—C6—C10—C966.5 (4)C2—C3—Mo1—C13167.7 (4)
Mo2—C7—C6—C1065.1 (4)C2—C3—C4—C50.8 (7)
Mo2—C7—C8—C959.4 (5)C3—Mo1—O3—C11124.0 (4)
Mo2—C8—C7—C663.4 (4)C3—Mo1—O4—C1256.2 (4)
Mo2—C8—C9—C1063.8 (4)C3—Mo1—C1—C577.6 (4)
Mo2—C9—C8—C759.5 (5)C3—Mo1—C4—C5116.9 (5)
Mo2—C9—C10—C665.0 (4)C3—Mo1—C5—C436.9 (3)
Mo2—C10—C6—C766.9 (4)C3—C2—Mo1—C437.3 (4)
Mo2—C10—C9—C867.8 (5)C3—C2—Mo1—C578.0 (4)
Mo2—C17—Si2—C1877.5 (4)C3—C2—Mo1—C1315.9 (5)
Mo2—C17—Si2—C19165.0 (3)C3—C2—C1—C51.9 (7)
Mo2—C17—Si2—C2044.3 (4)C3—C4—Mo1—C5116.9 (5)
Si1—C13—Mo1—O334.1 (5)C3—C4—Mo1—C13127.8 (4)
Si1—C13—Mo1—O474.0 (3)C4—Mo1—O3—C11109.1 (5)
Si1—C13—Mo1—N151.6 (3)C4—Mo1—O4—C1229.5 (4)
Si1—C13—Mo1—C1145.1 (3)C4—Mo1—C1—C536.6 (3)
Si1—C13—Mo1—C2169.2 (2)C4—C3—Mo1—C536.4 (4)
Si1—C13—Mo1—C3160.5 (3)C4—C3—Mo1—C1350.7 (4)
Si1—C13—Mo1—C4172.6 (4)C4—C5—Mo1—C1361.3 (4)
Si1—C13—Mo1—C5142.1 (3)C5—Mo1—O3—C1163.0 (5)
Si2—C17—Mo2—O3150.9 (4)C5—Mo1—O4—C1239.7 (5)
Si2—C17—Mo2—O4113.0 (3)C5—C1—Mo1—C135.0 (5)
Si2—C17—Mo2—N228.1 (3)C5—C4—Mo1—C13115.3 (4)
Si2—C17—Mo2—C668.5 (4)C6—Mo2—O3—C1187.6 (5)
Si2—C17—Mo2—C7115.3 (3)C6—Mo2—O4—C1255.0 (4)
Si2—C17—Mo2—C8118.2 (3)C6—Mo2—C7—C8113.3 (5)
Si2—C17—Mo2—C991.0 (4)C6—Mo2—C8—C739.4 (3)
Si2—C17—Mo2—C1061.3 (3)C6—Mo2—C8—C982.1 (4)
O3—Mo1—O4—C12164.9 (4)C6—Mo2—C9—C876.1 (4)
O3—Mo1—C1—C273.6 (4)C6—Mo2—C9—C1038.4 (3)
O3—Mo1—C1—C5174.5 (4)C6—Mo2—C10—C9114.4 (6)
O3—Mo1—C2—C1104.8 (4)C6—C7—Mo2—C8113.3 (5)
O3—Mo1—C2—C3136.4 (4)C6—C7—Mo2—C979.7 (4)
O3—Mo1—C3—C245.4 (4)C6—C7—Mo2—C1037.8 (3)
O3—Mo1—C3—C4162.4 (3)C6—C7—Mo2—C17108.0 (4)
O3—Mo1—C4—C326.0 (5)C6—C7—C8—C94.0 (7)
O3—Mo1—C4—C590.9 (4)C6—C10—Mo2—C737.5 (4)
O3—Mo1—C5—C17.1 (5)C6—C10—Mo2—C877.8 (4)
O3—Mo1—C5—C4121.9 (4)C6—C10—Mo2—C9114.4 (6)
O3—Mo2—O4—C12167.1 (4)C6—C10—Mo2—C17170.7 (4)
O3—Mo2—C6—C717.2 (5)C6—C10—C9—C82.8 (7)
O3—Mo2—C6—C10133.0 (4)C7—Mo2—O3—C1177.6 (5)
O3—Mo2—C7—C6167.4 (3)C7—Mo2—O4—C1289.4 (4)
O3—Mo2—C7—C879.3 (4)C7—Mo2—C6—C10115.7 (6)
O3—Mo2—C8—C7104.0 (4)C7—Mo2—C8—C9121.5 (6)
O3—Mo2—C8—C9134.5 (4)C7—Mo2—C9—C834.3 (4)
O3—Mo2—C9—C851.5 (5)C7—Mo2—C9—C1080.2 (4)
O3—Mo2—C9—C10166.0 (3)C7—Mo2—C10—C976.9 (4)
O3—Mo2—C10—C689.8 (5)C7—C6—Mo2—C837.9 (3)
O3—Mo2—C10—C924.6 (6)C7—C6—Mo2—C977.4 (4)
O4—Mo1—O3—C11155.6 (5)C7—C6—Mo2—C10115.7 (6)
O4—Mo1—C1—C213.5 (5)C7—C6—Mo2—C17103.4 (4)
O4—Mo1—C1—C5125.4 (4)C7—C6—C10—C90.3 (7)
O4—Mo1—C2—C1170.1 (4)C7—C8—Mo2—C9121.5 (6)
O4—Mo1—C2—C371.0 (4)C7—C8—Mo2—C1082.3 (4)
O4—Mo1—C3—C2110.9 (4)C7—C8—Mo2—C17175.9 (4)
O4—Mo1—C3—C4132.1 (4)C7—C8—C9—C104.3 (8)
O4—Mo1—C4—C352.3 (4)C8—Mo2—O3—C1144.3 (5)
O4—Mo1—C4—C5169.2 (3)C8—Mo2—O4—C12109.4 (4)
O4—Mo1—C5—C197.6 (5)C8—Mo2—C6—C1077.8 (4)
O4—Mo1—C5—C417.2 (5)C8—Mo2—C9—C10114.5 (6)
O4—Mo2—O3—C11154.9 (5)C8—Mo2—C10—C936.6 (4)
O4—Mo2—C6—C775.7 (4)C8—C7—Mo2—C933.5 (4)
O4—Mo2—C6—C10168.6 (4)C8—C7—Mo2—C1075.5 (4)
O4—Mo2—C7—C6102.0 (4)C8—C7—Mo2—C175.3 (5)
O4—Mo2—C7—C8144.7 (4)C8—C7—C6—C102.2 (7)
O4—Mo2—C8—C737.4 (4)C8—C9—Mo2—C10114.5 (6)
O4—Mo2—C8—C9158.9 (4)C8—C9—Mo2—C17123.7 (5)
O4—Mo2—C9—C831.6 (6)C9—Mo2—O3—C1118.9 (5)
O4—Mo2—C9—C1082.9 (5)C9—Mo2—O4—C1291.7 (4)
O4—Mo2—C10—C614.0 (5)C9—Mo2—C6—C1038.3 (4)
O4—Mo2—C10—C9128.4 (4)C9—C8—Mo2—C1039.2 (4)
N1—Mo1—O3—C1127.9 (4)C9—C8—Mo2—C1754.4 (4)
N1—Mo1—O4—C12121.6 (4)C9—C10—Mo2—C1756.3 (4)
N1—Mo1—C1—C2163.9 (4)C10—Mo2—O3—C1134.3 (6)
N1—Mo1—C1—C584.2 (4)C10—Mo2—O4—C1246.9 (4)
N1—Mo1—C2—C120.7 (5)C10—C6—Mo2—C1712.4 (5)
N1—Mo1—C2—C3139.5 (4)C10—C9—Mo2—C17121.8 (4)
N1—Mo1—C3—C272.5 (5)C11—O3—Mo1—C13112.1 (4)
N1—Mo1—C3—C444.6 (6)C11—O3—Mo2—C1751.3 (4)
N1—Mo1—C4—C3154.8 (4)C12—O4—Mo1—C1342.0 (4)
N1—Mo1—C4—C537.9 (4)C12—O4—Mo2—C17126.1 (4)
Symmetry codes: (i) x1/2, y+1/2, z; (ii) x+1/2, y1/2, z1/2; (iii) x+1, y+1, z+1/2; (iv) x+1/2, y+3/2, z.

Experimental details

Crystal data
Chemical formula[Mo2(C5H5)2(CH3O)2(C4H11Si)2(NO)2]
Mr618.58
Crystal system, space groupOrthorhombic, Pna21
Temperature (K)180
a, b, c (Å)12.375 (2), 15.248 (2), 14.119 (2)
V3)2664.1 (6)
Z4
Radiation typeMo Kα
µ (mm1)1.06
Crystal size (mm)0.30 × 0.20 × 0.03
Data collection
DiffractometerRigaku ADSC CCD area-detector
diffractometer
Absorption correctionMulti-scan
D*TREK (Molecular Structure Corporation, 1997)
Tmin, Tmax0.775, 0.969
No. of measured, independent and
observed [I > 3σ(I)] reflections
24272, 7079, 4260
Rint0.060
(sin θ/λ)max1)0.715
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.037, 0.063, 1.22
No. of reflections7078
No. of parameters270
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.72, 2.64
Absolute structureFlack (1983), 2844 Friedel pairs
Absolute structure parameter0.032 (4)

Computer programs: D*TREK (Molecular Structure Corporation, 1997), D*TREK, SIR97 (Altomare et al., 1999), TEXSAN (Molecular Structure Corporation, 1997) and SHELXL97 (Sheldrick, 1997), TEXSAN.

Selected geometric parameters (Å, º) top
Mo1—O32.093 (3)Mo2—O42.160 (3)
Mo1—O42.216 (4)Mo2—N21.776 (4)
Mo1—N11.769 (4)Mo2—C172.237 (5)
Mo1—C132.227 (5)O1—N11.216 (5)
Mo2—O32.144 (3)O2—N21.201 (4)
O3—Mo1—O467.2 (1)N2—Mo2—C1786.3 (2)
O3—Mo1—N190.1 (2)Mo1—O3—Mo2110.2 (2)
O3—Mo1—C13139.3 (2)Mo1—O3—C11122.7 (3)
O4—Mo1—N1124.4 (2)Mo2—O3—C11127.1 (3)
O4—Mo1—C1381.8 (2)Mo1—O4—Mo2105.2 (2)
N1—Mo1—C1386.2 (2)Mo1—O4—C12124.2 (3)
O3—Mo2—O467.4 (1)Mo2—O4—C12118.3 (3)
O3—Mo2—N2121.4 (2)Mo1—N1—O1170.1 (4)
O3—Mo2—C1779.9 (1)Mo2—N2—O2170.1 (5)
O4—Mo2—N289.4 (1)Mo1—C13—Si1117.8 (3)
O4—Mo2—C17138.4 (2)Mo2—C17—Si2124.6 (3)
 

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