Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S010827010200865X/fr1372sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S010827010200865X/fr1372Isup2.hkl |
CCDC reference: 192941
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).
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.
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.
Fig. 1. The molecular structure of (I) showing 50% probability ellipsoids. H atoms have been omitted for clarity. |
[Mo2(C5H5)2(CH3O)2(C4H11Si)2(NO)2] | Dx = 1.542 Mg m−3 |
Mr = 618.58 | Mo Kα radiation, λ = 0.71069 Å |
Orthorhombic, Pna21 | Cell parameters from 16401 reflections |
a = 12.375 (2) Å | θ = 2.0–30.5° |
b = 15.248 (2) Å | µ = 1.06 mm−1 |
c = 14.119 (2) Å | T = 180 K |
V = 2664.1 (6) Å3 | Plate, orange |
Z = 4 | 0.30 × 0.20 × 0.03 mm |
F(000) = 1264.00 |
Rigaku ADSC CCD area-detector diffractometer | 7079 independent reflections |
Radiation source: X-ray tube | 4260 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.060 |
Detector resolution: 11.76 pixels mm-1 | θmax = 30.6°, θmin = 2.0° |
area detector scans | h = −15→17 |
Absorption correction: multi-scan D*TREK (Molecular Structure Corporation, 1997) | k = −21→16 |
Tmin = 0.775, Tmax = 0.969 | l = −16→18 |
24272 measured reflections |
Refinement on F2 | 0 constraints |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.037 | Weighting scheme based on measured s.u.'s w = 1/[σ2(Fo2)] |
wR(F2) = 0.063 | (Δ/σ)max = 0.002 |
S = 1.22 | Δρmax = 1.72 e Å−3 |
7078 reflections | Δρmin = −2.64 e Å−3 |
270 parameters | Absolute structure: Flack (1983), 2844 Friedel pairs |
0 restraints | Absolute structure parameter: 0.032 (4) |
[Mo2(C5H5)2(CH3O)2(C4H11Si)2(NO)2] | V = 2664.1 (6) Å3 |
Mr = 618.58 | Z = 4 |
Orthorhombic, Pna21 | Mo Kα radiation |
a = 12.375 (2) Å | µ = 1.06 mm−1 |
b = 15.248 (2) Å | T = 180 K |
c = 14.119 (2) Å | 0.30 × 0.20 × 0.03 mm |
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 = 0.969 | Rint = 0.060 |
24272 measured reflections |
R[F2 > 2σ(F2)] = 0.037 | H-atom parameters constrained |
wR(F2) = 0.063 | Δρmax = 1.72 e Å−3 |
S = 1.22 | Δρmin = −2.64 e Å−3 |
7078 reflections | Absolute structure: Flack (1983), 2844 Friedel pairs |
270 parameters | Absolute structure parameter: 0.032 (4) |
0 restraints |
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. |
x | y | z | Uiso*/Ueq | ||
Mo1 | 0.31576 (3) | 0.39487 (2) | 0.3891 | 0.01886 (9) | |
Mo2 | 0.25867 (3) | 0.57059 (2) | 0.53772 (5) | 0.01878 (9) | |
Si1 | 0.3084 (1) | 0.20452 (7) | 0.5286 (1) | 0.0270 (4) | |
Si2 | 0.2720 (1) | 0.78388 (8) | 0.4239 (1) | 0.0262 (4) | |
O1 | 0.1447 (3) | 0.2794 (2) | 0.3093 (3) | 0.037 (1) | |
O2 | 0.4758 (3) | 0.6528 (2) | 0.5445 (3) | 0.037 (1) | |
O3 | 0.2001 (3) | 0.4893 (2) | 0.4250 (2) | 0.0224 (9) | |
O4 | 0.3330 (2) | 0.4424 (2) | 0.5366 (3) | 0.0212 (7) | |
N1 | 0.2121 (3) | 0.3237 (2) | 0.3499 (3) | 0.026 (1) | |
N2 | 0.3891 (3) | 0.6190 (2) | 0.5331 (3) | 0.0199 (9) | |
C1 | 0.3454 (5) | 0.4580 (4) | 0.2423 (4) | 0.037 (2) | |
C2 | 0.3974 (5) | 0.5177 (3) | 0.3062 (4) | 0.034 (2) | |
C3 | 0.4826 (4) | 0.4759 (3) | 0.3510 (4) | 0.038 (2) | |
C4 | 0.4887 (5) | 0.3879 (3) | 0.3136 (4) | 0.035 (2) | |
C5 | 0.4072 (5) | 0.3766 (3) | 0.2480 (4) | 0.037 (2) | |
C6 | 0.2429 (5) | 0.5645 (3) | 0.7022 (3) | 0.034 (1) | |
C7 | 0.1593 (5) | 0.5077 (3) | 0.6673 (4) | 0.036 (2) | |
C8 | 0.0841 (5) | 0.5635 (4) | 0.6209 (4) | 0.039 (2) | |
C9 | 0.1207 (5) | 0.6495 (4) | 0.6200 (4) | 0.040 (2) | |
C10 | 0.2196 (5) | 0.6521 (3) | 0.6736 (4) | 0.035 (2) | |
C11 | 0.1006 (4) | 0.4957 (3) | 0.3793 (5) | 0.031 (1) | |
C12 | 0.4243 (4) | 0.4290 (3) | 0.5925 (4) | 0.030 (1) | |
C13 | 0.3928 (4) | 0.2759 (3) | 0.4509 (4) | 0.030 (2) | |
C14 | 0.1887 (5) | 0.2616 (3) | 0.5845 (4) | 0.048 (2) | |
C15 | 0.3948 (6) | 0.1593 (4) | 0.6283 (4) | 0.052 (2) | |
C16 | 0.2570 (5) | 0.1089 (3) | 0.4577 (4) | 0.047 (2) | |
C17 | 0.2087 (4) | 0.6736 (3) | 0.4338 (4) | 0.024 (1) | |
C18 | 0.4039 (4) | 0.7742 (3) | 0.3597 (4) | 0.036 (2) | |
C19 | 0.1826 (5) | 0.8568 (3) | 0.3523 (4) | 0.042 (2) | |
C20 | 0.2971 (5) | 0.8400 (3) | 0.5398 (5) | 0.051 (2) | |
H1 | 0.2819 | 0.4694 | 0.2028 | 0.044* | |
H2 | 0.3757 | 0.5788 | 0.3167 | 0.040* | |
H3 | 0.5302 | 0.5014 | 0.3992 | 0.045* | |
H4 | 0.5420 | 0.3434 | 0.3318 | 0.042* | |
H5 | 0.3931 | 0.3231 | 0.2115 | 0.044* | |
H6 | 0.3057 | 0.5460 | 0.7393 | 0.041* | |
H7 | 0.1549 | 0.4439 | 0.6740 | 0.043* | |
H8 | 0.0156 | 0.5439 | 0.5932 | 0.046* | |
H9 | 0.0856 | 0.6993 | 0.5886 | 0.048* | |
H10 | 0.2628 | 0.7044 | 0.6878 | 0.042* | |
H11 | 0.1118 | 0.5148 | 0.3136 | 0.037* | |
H12 | 0.0551 | 0.5385 | 0.4122 | 0.037* | |
H13 | 0.0649 | 0.4383 | 0.3795 | 0.037* | |
H14 | 0.4894 | 0.4395 | 0.5546 | 0.036* | |
H15 | 0.4248 | 0.3685 | 0.6159 | 0.036* | |
H16 | 0.4230 | 0.4696 | 0.6463 | 0.036* | |
H17 | 0.4549 | 0.2956 | 0.4884 | 0.036* | |
H18 | 0.4182 | 0.2397 | 0.3980 | 0.036* | |
H19 | 0.2141 | 0.3109 | 0.6230 | 0.058* | |
H20 | 0.1494 | 0.2200 | 0.6248 | 0.058* | |
H21 | 0.1405 | 0.2833 | 0.5347 | 0.058* | |
H22 | 0.4568 | 0.1281 | 0.6015 | 0.062* | |
H23 | 0.3516 | 0.1188 | 0.6666 | 0.062* | |
H24 | 0.4203 | 0.2077 | 0.6680 | 0.062* | |
H25 | 0.2207 | 0.1305 | 0.4004 | 0.057* | |
H26 | 0.2056 | 0.0751 | 0.4957 | 0.057* | |
H27 | 0.3177 | 0.0712 | 0.4394 | 0.057* | |
H28 | 0.1320 | 0.6845 | 0.4463 | 0.028* | |
H29 | 0.2168 | 0.6467 | 0.3712 | 0.028* | |
H30 | 0.3923 | 0.7456 | 0.2984 | 0.044* | |
H31 | 0.4544 | 0.7392 | 0.3976 | 0.044* | |
H32 | 0.4343 | 0.8329 | 0.3495 | 0.044* | |
H33 | 0.2159 | 0.9149 | 0.3463 | 0.051* | |
H34 | 0.1122 | 0.8624 | 0.3836 | 0.051* | |
H35 | 0.1724 | 0.8314 | 0.2890 | 0.051* | |
H36 | 0.3284 | 0.8980 | 0.5282 | 0.061* | |
H37 | 0.3471 | 0.8049 | 0.5777 | 0.061* | |
H38 | 0.2285 | 0.8465 | 0.5739 | 0.061* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo1 | 0.0210 (2) | 0.0146 (1) | 0.0211 (2) | −0.0004 (2) | 0.0012 (3) | −0.0019 (2) |
Mo2 | 0.0212 (2) | 0.0155 (1) | 0.0196 (2) | 0.0020 (2) | −0.0024 (3) | −0.0028 (2) |
Si1 | 0.0311 (8) | 0.0217 (6) | 0.0280 (9) | −0.0033 (6) | −0.0045 (9) | 0.0016 (7) |
Si2 | 0.0268 (9) | 0.0188 (6) | 0.0330 (9) | 0.0010 (6) | −0.0018 (7) | 0.0004 (6) |
O1 | 0.034 (2) | 0.037 (2) | 0.039 (3) | −0.012 (2) | −0.003 (2) | −0.019 (2) |
O2 | 0.024 (2) | 0.039 (2) | 0.048 (3) | −0.012 (2) | −0.015 (2) | 0.012 (2) |
O3 | 0.018 (2) | 0.021 (2) | 0.028 (2) | 0.003 (1) | −0.006 (2) | −0.006 (1) |
O4 | 0.024 (2) | 0.020 (1) | 0.020 (2) | 0.006 (1) | −0.008 (2) | −0.006 (2) |
N1 | 0.022 (2) | 0.018 (2) | 0.037 (3) | −0.005 (2) | 0.004 (2) | −0.006 (2) |
N2 | 0.020 (2) | 0.028 (2) | 0.012 (2) | 0.001 (1) | −0.007 (2) | 0.003 (2) |
C1 | 0.045 (4) | 0.045 (3) | 0.021 (3) | −0.006 (2) | 0.005 (3) | 0.011 (2) |
C2 | 0.041 (3) | 0.020 (2) | 0.041 (4) | −0.007 (2) | 0.023 (3) | 0.006 (2) |
C3 | 0.030 (3) | 0.035 (3) | 0.049 (4) | −0.017 (2) | 0.008 (3) | −0.004 (2) |
C4 | 0.033 (3) | 0.028 (2) | 0.046 (4) | 0.000 (3) | 0.025 (2) | 0.014 (2) |
C5 | 0.047 (4) | 0.034 (3) | 0.029 (3) | −0.010 (2) | 0.034 (2) | −0.008 (2) |
C6 | 0.049 (3) | 0.036 (2) | 0.018 (2) | 0.008 (3) | 0.014 (3) | −0.007 (2) |
C7 | 0.050 (4) | 0.038 (3) | 0.019 (3) | −0.007 (2) | 0.021 (3) | 0.008 (2) |
C8 | 0.036 (4) | 0.050 (3) | 0.030 (4) | −0.004 (3) | 0.017 (3) | −0.005 (3) |
C9 | 0.047 (4) | 0.039 (3) | 0.034 (4) | 0.027 (3) | 0.011 (3) | −0.008 (3) |
C10 | 0.053 (4) | 0.034 (2) | 0.018 (3) | −0.005 (3) | 0.012 (3) | −0.016 (2) |
C11 | 0.022 (3) | 0.030 (2) | 0.042 (4) | 0.002 (2) | −0.016 (3) | −0.010 (3) |
C12 | 0.030 (3) | 0.028 (2) | 0.031 (3) | 0.007 (3) | −0.007 (2) | 0.006 (3) |
C13 | 0.036 (3) | 0.013 (2) | 0.040 (4) | 0.008 (2) | 0.002 (3) | 0.005 (2) |
C14 | 0.032 (3) | 0.046 (3) | 0.066 (5) | 0.005 (3) | 0.013 (3) | −0.012 (3) |
C15 | 0.062 (5) | 0.048 (4) | 0.044 (4) | −0.002 (3) | −0.026 (3) | 0.019 (3) |
C16 | 0.061 (4) | 0.022 (2) | 0.059 (4) | −0.016 (3) | −0.003 (4) | 0.001 (2) |
C17 | 0.028 (3) | 0.017 (2) | 0.025 (3) | 0.004 (2) | −0.010 (2) | 0.002 (2) |
C18 | 0.028 (3) | 0.037 (3) | 0.045 (4) | −0.005 (3) | 0.001 (2) | −0.001 (3) |
C19 | 0.030 (3) | 0.026 (2) | 0.071 (5) | 0.005 (2) | −0.003 (3) | 0.022 (2) |
C20 | 0.082 (5) | 0.029 (2) | 0.041 (3) | −0.018 (3) | 0.002 (5) | −0.015 (3) |
Mo1—O3 | 2.093 (3) | C5—H5 | 0.98 |
Mo1—O4 | 2.216 (4) | C6—C7 | 1.436 (9) |
Mo1—N1 | 1.769 (4) | C6—C10 | 1.425 (7) |
Mo1—C1 | 2.315 (6) | C6—H6 | 0.98 |
Mo1—C2 | 2.428 (5) | C7—C8 | 1.421 (9) |
Mo1—C3 | 2.465 (6) | C7—H7 | 0.98 |
Mo1—C4 | 2.393 (6) | C8—C9 | 1.388 (8) |
Mo1—C5 | 2.307 (5) | C8—H8 | 0.98 |
Mo1—C13 | 2.227 (5) | C9—C10 | 1.441 (9) |
Mo2—O3 | 2.144 (3) | C9—H9 | 0.98 |
Mo2—O4 | 2.160 (3) | C10—H10 | 0.98 |
Mo2—N2 | 1.776 (4) | C11—H11 | 0.98 |
Mo2—C6 | 2.332 (5) | C11—H12 | 0.98 |
Mo2—C7 | 2.404 (5) | C11—H13 | 0.98 |
Mo2—C8 | 2.462 (6) | C12—H14 | 0.98 |
Mo2—C9 | 2.390 (6) | C12—H15 | 0.98 |
Mo2—C10 | 2.337 (5) | C12—H16 | 0.98 |
Mo2—C17 | 2.237 (5) | C13—H17 | 0.98 |
Si1—C13 | 1.865 (6) | C13—H18 | 0.98 |
Si1—C14 | 1.890 (6) | C14—H19 | 0.98 |
Si1—C15 | 1.897 (7) | C14—H20 | 0.98 |
Si1—C16 | 1.880 (5) | C14—H21 | 0.98 |
Si2—C17 | 1.860 (5) | C15—H22 | 0.98 |
Si2—C18 | 1.874 (6) | C15—H23 | 0.98 |
Si2—C19 | 1.866 (6) | C15—H24 | 0.98 |
Si2—C20 | 1.872 (7) | C16—H25 | 0.98 |
O1—N1 | 1.216 (5) | C16—H26 | 0.98 |
O2—N2 | 1.201 (4) | C16—H27 | 0.98 |
O3—C11 | 1.393 (6) | C17—H28 | 0.98 |
O4—C12 | 1.394 (6) | C17—H29 | 0.98 |
C1—C2 | 1.435 (8) | C18—H30 | 0.98 |
C1—C5 | 1.459 (8) | C18—H31 | 0.98 |
C1—H1 | 0.98 | C18—H32 | 0.98 |
C2—C3 | 1.385 (8) | C19—H33 | 0.98 |
C2—H2 | 0.98 | C19—H34 | 0.98 |
C3—C4 | 1.444 (8) | C19—H35 | 0.98 |
C3—H3 | 0.98 | C20—H36 | 0.98 |
C4—C5 | 1.380 (9) | C20—H37 | 0.98 |
C4—H4 | 0.98 | C20—H38 | 0.98 |
O1···C4i | 3.200 (7) | O2···C5iii | 3.249 (7) |
O1···C10ii | 3.203 (7) | C3···C19iv | 3.554 (8) |
O3—Mo1—O4 | 67.2 (1) | Mo1—C3—H3 | 123.4 |
O3—Mo1—N1 | 90.1 (2) | C2—C3—C4 | 107.5 (5) |
O3—Mo1—C1 | 92.2 (2) | C2—C3—H3 | 126.3 |
O3—Mo1—C2 | 82.5 (2) | C4—C3—H3 | 126.2 |
O3—Mo1—C3 | 106.3 (2) | Mo1—C4—C3 | 75.5 (3) |
O3—Mo1—C4 | 138.6 (2) | Mo1—C4—C5 | 69.5 (3) |
O3—Mo1—C5 | 128.9 (2) | Mo1—C4—H4 | 121.1 |
O3—Mo1—C13 | 139.3 (2) | C3—C4—C5 | 108.8 (5) |
O4—Mo1—N1 | 124.4 (2) | C3—C4—H4 | 125.6 |
O4—Mo1—C1 | 133.7 (2) | C5—C4—H4 | 125.6 |
O4—Mo1—C2 | 99.2 (2) | Mo1—C5—C1 | 71.9 (3) |
O4—Mo1—C3 | 87.8 (2) | Mo1—C5—C4 | 76.4 (4) |
O4—Mo1—C4 | 110.3 (2) | Mo1—C5—H5 | 117.9 |
O4—Mo1—C5 | 143.5 (2) | C1—C5—C4 | 108.3 (5) |
O4—Mo1—C13 | 81.8 (2) | C1—C5—H5 | 125.8 |
N1—Mo1—C1 | 95.2 (2) | C4—C5—H5 | 125.8 |
N1—Mo1—C2 | 128.6 (2) | Mo2—C6—C7 | 75.1 (3) |
N1—Mo1—C3 | 147.8 (2) | Mo2—C6—C10 | 72.4 (3) |
N1—Mo1—C4 | 118.8 (2) | Mo2—C6—H6 | 118.6 |
N1—Mo1—C5 | 90.7 (2) | C7—C6—C10 | 108.8 (6) |
N1—Mo1—C13 | 86.2 (2) | C7—C6—H6 | 125.6 |
C1—Mo1—C2 | 35.1 (2) | C10—C6—H6 | 125.6 |
C1—Mo1—C3 | 57.5 (2) | Mo2—C7—C6 | 69.6 (3) |
C1—Mo1—C4 | 58.5 (2) | Mo2—C7—C8 | 75.2 (3) |
C1—Mo1—C5 | 36.8 (2) | Mo2—C7—H7 | 119.9 |
C1—Mo1—C13 | 128.4 (2) | C6—C7—C8 | 105.6 (5) |
C2—Mo1—C3 | 32.9 (2) | C6—C7—H7 | 127.3 |
C2—Mo1—C4 | 56.5 (2) | C8—C7—H7 | 127.1 |
C2—Mo1—C5 | 58.2 (2) | Mo2—C8—C7 | 70.8 (3) |
C2—Mo1—C13 | 129.7 (2) | Mo2—C8—C9 | 70.6 (4) |
C3—Mo1—C4 | 34.5 (2) | Mo2—C8—H8 | 125.6 |
C3—Mo1—C5 | 57.4 (2) | C7—C8—C9 | 110.9 (6) |
C3—Mo1—C13 | 97.8 (2) | C7—C8—H8 | 124.6 |
C4—Mo1—C5 | 34.1 (2) | C9—C8—H8 | 124.6 |
C4—Mo1—C13 | 75.9 (2) | Mo2—C9—C8 | 76.2 (3) |
C5—Mo1—C13 | 91.7 (2) | Mo2—C9—C10 | 70.3 (3) |
O3—Mo2—O4 | 67.4 (1) | Mo2—C9—H9 | 119.1 |
O3—Mo2—N2 | 121.4 (2) | C8—C9—C10 | 107.4 (6) |
O3—Mo2—C6 | 133.5 (2) | C8—C9—H9 | 126.3 |
O3—Mo2—C7 | 99.3 (2) | C10—C9—H9 | 126.4 |
O3—Mo2—C8 | 91.8 (2) | Mo2—C10—C6 | 72.0 (3) |
O3—Mo2—C9 | 114.2 (2) | Mo2—C10—C9 | 74.3 (3) |
O3—Mo2—C10 | 147.9 (2) | Mo2—C10—H10 | 119.2 |
O3—Mo2—C17 | 79.9 (1) | C6—C10—C9 | 107.1 (5) |
O4—Mo2—N2 | 89.4 (1) | C6—C10—H10 | 126.5 |
O4—Mo2—C6 | 90.4 (2) | C9—C10—H10 | 126.4 |
O4—Mo2—C7 | 82.1 (2) | O3—C11—H11 | 109.5 |
O4—Mo2—C8 | 109.7 (2) | O3—C11—H12 | 109.5 |
O4—Mo2—C9 | 139.8 (2) | O3—C11—H13 | 109.6 |
O4—Mo2—C10 | 125.1 (2) | H11—C11—H12 | 109.4 |
O4—Mo2—C17 | 138.4 (2) | H11—C11—H13 | 109.4 |
N2—Mo2—C6 | 97.4 (2) | H12—C11—H13 | 109.5 |
N2—Mo2—C7 | 131.2 (2) | O4—C12—H14 | 109.5 |
N2—Mo2—C8 | 146.4 (2) | O4—C12—H15 | 109.5 |
N2—Mo2—C9 | 117.2 (2) | O4—C12—H16 | 109.5 |
N2—Mo2—C10 | 89.8 (2) | H14—C12—H15 | 109.5 |
N2—Mo2—C17 | 86.3 (2) | H14—C12—H16 | 109.4 |
C6—Mo2—C7 | 35.3 (2) | H15—C12—H16 | 109.5 |
C6—Mo2—C8 | 56.6 (2) | Mo1—C13—Si1 | 117.8 (3) |
C6—Mo2—C9 | 58.4 (2) | Mo1—C13—H17 | 107.3 |
C6—Mo2—C10 | 35.5 (2) | Mo1—C13—H18 | 107.3 |
C6—Mo2—C17 | 131.1 (2) | Si1—C13—H17 | 107.4 |
C7—Mo2—C8 | 33.9 (2) | Si1—C13—H18 | 107.4 |
C7—Mo2—C9 | 57.7 (2) | H17—C13—H18 | 109.4 |
C7—Mo2—C10 | 58.8 (2) | Si1—C14—H19 | 109.5 |
C7—Mo2—C17 | 129.6 (2) | Si1—C14—H20 | 109.5 |
C8—Mo2—C9 | 33.2 (2) | Si1—C14—H21 | 109.5 |
C8—Mo2—C10 | 56.6 (2) | H19—C14—H20 | 109.5 |
C8—Mo2—C17 | 95.8 (2) | H19—C14—H21 | 109.5 |
C9—Mo2—C10 | 35.5 (2) | H20—C14—H21 | 109.4 |
C9—Mo2—C17 | 76.5 (2) | Si1—C15—H22 | 109.4 |
C10—Mo2—C17 | 96.2 (2) | Si1—C15—H23 | 109.4 |
C13—Si1—C14 | 114.6 (2) | Si1—C15—H24 | 109.4 |
C13—Si1—C15 | 109.5 (3) | H22—C15—H23 | 109.5 |
C13—Si1—C16 | 109.1 (3) | H22—C15—H24 | 109.6 |
C14—Si1—C15 | 107.4 (3) | H23—C15—H24 | 109.6 |
C14—Si1—C16 | 108.3 (3) | Si1—C16—H25 | 109.5 |
C15—Si1—C16 | 107.7 (3) | Si1—C16—H26 | 109.6 |
C17—Si2—C18 | 109.4 (3) | Si1—C16—H27 | 109.6 |
C17—Si2—C19 | 109.3 (3) | H25—C16—H26 | 109.3 |
C17—Si2—C20 | 114.7 (3) | H25—C16—H27 | 109.3 |
C18—Si2—C19 | 107.6 (3) | H26—C16—H27 | 109.5 |
C18—Si2—C20 | 108.3 (3) | Mo2—C17—Si2 | 124.6 (3) |
C19—Si2—C20 | 107.4 (3) | Mo2—C17—H28 | 105.6 |
Mo1—O3—Mo2 | 110.2 (2) | Mo2—C17—H29 | 105.6 |
Mo1—O3—C11 | 122.7 (3) | Si2—C17—H28 | 105.6 |
Mo2—O3—C11 | 127.1 (3) | Si2—C17—H29 | 105.5 |
Mo1—O4—Mo2 | 105.2 (2) | H28—C17—H29 | 109.4 |
Mo1—O4—C12 | 124.2 (3) | Si2—C18—H30 | 109.5 |
Mo2—O4—C12 | 118.3 (3) | Si2—C18—H31 | 109.5 |
Mo1—N1—O1 | 170.1 (4) | Si2—C18—H32 | 109.5 |
Mo2—N2—O2 | 170.1 (5) | H30—C18—H31 | 109.5 |
Mo1—C1—C2 | 76.8 (4) | H30—C18—H32 | 109.4 |
Mo1—C1—C5 | 71.3 (3) | H31—C18—H32 | 109.4 |
Mo1—C1—H1 | 117.1 | Si2—C19—H33 | 109.6 |
C2—C1—C5 | 105.7 (6) | Si2—C19—H34 | 109.6 |
C2—C1—H1 | 127.2 | Si2—C19—H35 | 109.5 |
C5—C1—H1 | 127.1 | H33—C19—H34 | 109.5 |
Mo1—C2—C1 | 68.1 (3) | H33—C19—H35 | 109.3 |
Mo1—C2—C3 | 75.0 (3) | H34—C19—H35 | 109.3 |
Mo1—C2—H2 | 123.1 | Si2—C20—H36 | 109.4 |
C1—C2—C3 | 109.6 (5) | Si2—C20—H37 | 109.4 |
C1—C2—H2 | 125.2 | Si2—C20—H38 | 109.3 |
C3—C2—H2 | 125.2 | H36—C20—H37 | 109.6 |
Mo1—C3—C2 | 72.1 (3) | H36—C20—H38 | 109.5 |
Mo1—C3—C4 | 70.0 (3) | H37—C20—H38 | 109.6 |
Mo1—O3—Mo2—O4 | −25.4 (1) | N1—Mo1—C5—C1 | 97.7 (4) |
Mo1—O3—Mo2—N2 | 49.1 (2) | N1—Mo1—C5—C4 | −147.5 (4) |
Mo1—O3—Mo2—C6 | −92.8 (3) | N2—Mo2—O3—C11 | −130.6 (4) |
Mo1—O3—Mo2—C7 | −102.7 (2) | N2—Mo2—O4—C12 | 42.4 (4) |
Mo1—O3—Mo2—C8 | −136.0 (2) | N2—Mo2—C6—C7 | −165.1 (4) |
Mo1—O3—Mo2—C9 | −161.4 (2) | N2—Mo2—C6—C10 | 79.2 (4) |
Mo1—O3—Mo2—C10 | −146.0 (3) | N2—Mo2—C7—C6 | 19.8 (5) |
Mo1—O3—Mo2—C17 | 128.4 (2) | N2—Mo2—C7—C8 | 133.1 (4) |
Mo1—O4—Mo2—O3 | 23.2 (1) | N2—Mo2—C8—C7 | −83.9 (5) |
Mo1—O4—Mo2—N2 | −101.5 (2) | N2—Mo2—C8—C9 | 37.6 (6) |
Mo1—O4—Mo2—C6 | 161.1 (2) | N2—Mo2—C9—C8 | −157.7 (4) |
Mo1—O4—Mo2—C7 | 126.8 (2) | N2—Mo2—C9—C10 | −43.2 (4) |
Mo1—O4—Mo2—C8 | 106.7 (2) | N2—Mo2—C10—C6 | −103.1 (4) |
Mo1—O4—Mo2—C9 | 124.5 (3) | N2—Mo2—C10—C9 | 142.5 (4) |
Mo1—O4—Mo2—C10 | 169.2 (2) | C1—Mo1—O3—C11 | 67.3 (4) |
Mo1—O4—Mo2—C17 | −17.8 (3) | C1—Mo1—O4—C12 | −94.9 (4) |
Mo1—C1—C2—C3 | 64.0 (5) | C1—Mo1—C2—C3 | −118.8 (5) |
Mo1—C1—C5—C4 | −68.3 (4) | C1—Mo1—C3—C2 | 36.7 (4) |
Mo1—C2—C1—C5 | −65.9 (4) | C1—Mo1—C3—C4 | −80.4 (4) |
Mo1—C2—C3—C4 | 61.4 (4) | C1—Mo1—C4—C3 | 77.3 (4) |
Mo1—C3—C2—C1 | −59.7 (4) | C1—Mo1—C4—C5 | −39.6 (3) |
Mo1—C3—C4—C5 | 62.0 (4) | C1—Mo1—C5—C4 | 114.8 (5) |
Mo1—C4—C3—C2 | −62.7 (4) | C1—C2—Mo1—C3 | 118.8 (5) |
Mo1—C4—C5—C1 | 65.3 (4) | C1—C2—Mo1—C4 | 81.5 (4) |
Mo1—C5—C1—C2 | 69.8 (4) | C1—C2—Mo1—C5 | 40.8 (4) |
Mo1—C5—C4—C3 | −65.8 (4) | C1—C2—Mo1—C13 | 102.9 (4) |
Mo1—C13—Si1—C14 | −23.0 (4) | C1—C2—C3—C4 | 1.7 (7) |
Mo1—C13—Si1—C15 | −143.7 (3) | C1—C5—Mo1—C2 | −38.9 (4) |
Mo1—C13—Si1—C16 | 98.6 (3) | C1—C5—Mo1—C3 | −77.9 (4) |
Mo2—O3—Mo1—O4 | 24.7 (1) | C1—C5—Mo1—C4 | −114.8 (5) |
Mo2—O3—Mo1—N1 | 152.4 (2) | C1—C5—Mo1—C13 | −176.1 (4) |
Mo2—O3—Mo1—C1 | −112.4 (2) | C1—C5—C4—C3 | −0.4 (7) |
Mo2—O3—Mo1—C2 | −78.6 (2) | C2—Mo1—O3—C11 | 101.1 (4) |
Mo2—O3—Mo1—C3 | −55.7 (2) | C2—Mo1—O4—C12 | −87.1 (4) |
Mo2—O3—Mo1—C4 | −70.6 (3) | C2—Mo1—C1—C5 | 111.9 (6) |
Mo2—O3—Mo1—C5 | −116.7 (2) | C2—Mo1—C3—C4 | −117.0 (5) |
Mo2—O3—Mo1—C13 | 68.2 (3) | C2—Mo1—C4—C3 | 35.4 (3) |
Mo2—O4—Mo1—O3 | −23.8 (1) | C2—Mo1—C4—C5 | −81.5 (4) |
Mo2—O4—Mo1—N1 | −97.2 (2) | C2—Mo1—C5—C4 | 75.9 (4) |
Mo2—O4—Mo1—C1 | 46.2 (3) | C2—C1—Mo1—C3 | −34.3 (3) |
Mo2—O4—Mo1—C2 | 54.0 (2) | C2—C1—Mo1—C4 | −75.3 (4) |
Mo2—O4—Mo1—C3 | 84.9 (2) | C2—C1—Mo1—C5 | −111.9 (6) |
Mo2—O4—Mo1—C4 | 111.6 (2) | C2—C1—Mo1—C13 | −106.8 (4) |
Mo2—O4—Mo1—C5 | 101.4 (3) | C2—C1—C5—C4 | 1.4 (7) |
Mo2—O4—Mo1—C13 | −176.9 (2) | C2—C3—Mo1—C4 | 117.0 (5) |
Mo2—C6—C7—C8 | −67.3 (4) | C2—C3—Mo1—C5 | 80.7 (4) |
Mo2—C6—C10—C9 | 66.5 (4) | C2—C3—Mo1—C13 | 167.7 (4) |
Mo2—C7—C6—C10 | 65.1 (4) | C2—C3—C4—C5 | −0.8 (7) |
Mo2—C7—C8—C9 | −59.4 (5) | C3—Mo1—O3—C11 | 124.0 (4) |
Mo2—C8—C7—C6 | 63.4 (4) | C3—Mo1—O4—C12 | −56.2 (4) |
Mo2—C8—C9—C10 | −63.8 (4) | C3—Mo1—C1—C5 | 77.6 (4) |
Mo2—C9—C8—C7 | 59.5 (5) | C3—Mo1—C4—C5 | −116.9 (5) |
Mo2—C9—C10—C6 | −65.0 (4) | C3—Mo1—C5—C4 | 36.9 (3) |
Mo2—C10—C6—C7 | −66.9 (4) | C3—C2—Mo1—C4 | −37.3 (4) |
Mo2—C10—C9—C8 | 67.8 (5) | C3—C2—Mo1—C5 | −78.0 (4) |
Mo2—C17—Si2—C18 | 77.5 (4) | C3—C2—Mo1—C13 | −15.9 (5) |
Mo2—C17—Si2—C19 | −165.0 (3) | C3—C2—C1—C5 | −1.9 (7) |
Mo2—C17—Si2—C20 | −44.3 (4) | C3—C4—Mo1—C5 | 116.9 (5) |
Si1—C13—Mo1—O3 | 34.1 (5) | C3—C4—Mo1—C13 | −127.8 (4) |
Si1—C13—Mo1—O4 | 74.0 (3) | C4—Mo1—O3—C11 | 109.1 (5) |
Si1—C13—Mo1—N1 | −51.6 (3) | C4—Mo1—O4—C12 | −29.5 (4) |
Si1—C13—Mo1—C1 | −145.1 (3) | C4—Mo1—C1—C5 | 36.6 (3) |
Si1—C13—Mo1—C2 | 169.2 (2) | C4—C3—Mo1—C5 | −36.4 (4) |
Si1—C13—Mo1—C3 | 160.5 (3) | C4—C3—Mo1—C13 | 50.7 (4) |
Si1—C13—Mo1—C4 | −172.6 (4) | C4—C5—Mo1—C13 | −61.3 (4) |
Si1—C13—Mo1—C5 | −142.1 (3) | C5—Mo1—O3—C11 | 63.0 (5) |
Si2—C17—Mo2—O3 | −150.9 (4) | C5—Mo1—O4—C12 | −39.7 (5) |
Si2—C17—Mo2—O4 | −113.0 (3) | C5—C1—Mo1—C13 | 5.0 (5) |
Si2—C17—Mo2—N2 | −28.1 (3) | C5—C4—Mo1—C13 | 115.3 (4) |
Si2—C17—Mo2—C6 | 68.5 (4) | C6—Mo2—O3—C11 | 87.6 (5) |
Si2—C17—Mo2—C7 | 115.3 (3) | C6—Mo2—O4—C12 | −55.0 (4) |
Si2—C17—Mo2—C8 | 118.2 (3) | C6—Mo2—C7—C8 | 113.3 (5) |
Si2—C17—Mo2—C9 | 91.0 (4) | C6—Mo2—C8—C7 | −39.4 (3) |
Si2—C17—Mo2—C10 | 61.3 (3) | C6—Mo2—C8—C9 | 82.1 (4) |
O3—Mo1—O4—C12 | −164.9 (4) | C6—Mo2—C9—C8 | −76.1 (4) |
O3—Mo1—C1—C2 | 73.6 (4) | C6—Mo2—C9—C10 | 38.4 (3) |
O3—Mo1—C1—C5 | −174.5 (4) | C6—Mo2—C10—C9 | −114.4 (6) |
O3—Mo1—C2—C1 | −104.8 (4) | C6—C7—Mo2—C8 | −113.3 (5) |
O3—Mo1—C2—C3 | 136.4 (4) | C6—C7—Mo2—C9 | −79.7 (4) |
O3—Mo1—C3—C2 | −45.4 (4) | C6—C7—Mo2—C10 | −37.8 (3) |
O3—Mo1—C3—C4 | −162.4 (3) | C6—C7—Mo2—C17 | −108.0 (4) |
O3—Mo1—C4—C3 | 26.0 (5) | C6—C7—C8—C9 | 4.0 (7) |
O3—Mo1—C4—C5 | −90.9 (4) | C6—C10—Mo2—C7 | 37.5 (4) |
O3—Mo1—C5—C1 | 7.1 (5) | C6—C10—Mo2—C8 | 77.8 (4) |
O3—Mo1—C5—C4 | 121.9 (4) | C6—C10—Mo2—C9 | 114.4 (6) |
O3—Mo2—O4—C12 | 167.1 (4) | C6—C10—Mo2—C17 | 170.7 (4) |
O3—Mo2—C6—C7 | −17.2 (5) | C6—C10—C9—C8 | 2.8 (7) |
O3—Mo2—C6—C10 | −133.0 (4) | C7—Mo2—O3—C11 | 77.6 (5) |
O3—Mo2—C7—C6 | 167.4 (3) | C7—Mo2—O4—C12 | −89.4 (4) |
O3—Mo2—C7—C8 | −79.3 (4) | C7—Mo2—C6—C10 | −115.7 (6) |
O3—Mo2—C8—C7 | 104.0 (4) | C7—Mo2—C8—C9 | 121.5 (6) |
O3—Mo2—C8—C9 | −134.5 (4) | C7—Mo2—C9—C8 | −34.3 (4) |
O3—Mo2—C9—C8 | 51.5 (5) | C7—Mo2—C9—C10 | 80.2 (4) |
O3—Mo2—C9—C10 | 166.0 (3) | C7—Mo2—C10—C9 | −76.9 (4) |
O3—Mo2—C10—C6 | 89.8 (5) | C7—C6—Mo2—C8 | 37.9 (3) |
O3—Mo2—C10—C9 | −24.6 (6) | C7—C6—Mo2—C9 | 77.4 (4) |
O4—Mo1—O3—C11 | −155.6 (5) | C7—C6—Mo2—C10 | 115.7 (6) |
O4—Mo1—C1—C2 | 13.5 (5) | C7—C6—Mo2—C17 | 103.4 (4) |
O4—Mo1—C1—C5 | 125.4 (4) | C7—C6—C10—C9 | −0.3 (7) |
O4—Mo1—C2—C1 | −170.1 (4) | C7—C8—Mo2—C9 | −121.5 (6) |
O4—Mo1—C2—C3 | 71.0 (4) | C7—C8—Mo2—C10 | −82.3 (4) |
O4—Mo1—C3—C2 | −110.9 (4) | C7—C8—Mo2—C17 | −175.9 (4) |
O4—Mo1—C3—C4 | 132.1 (4) | C7—C8—C9—C10 | −4.3 (8) |
O4—Mo1—C4—C3 | −52.3 (4) | C8—Mo2—O3—C11 | 44.3 (5) |
O4—Mo1—C4—C5 | −169.2 (3) | C8—Mo2—O4—C12 | −109.4 (4) |
O4—Mo1—C5—C1 | −97.6 (5) | C8—Mo2—C6—C10 | −77.8 (4) |
O4—Mo1—C5—C4 | 17.2 (5) | C8—Mo2—C9—C10 | 114.5 (6) |
O4—Mo2—O3—C11 | 154.9 (5) | C8—Mo2—C10—C9 | −36.6 (4) |
O4—Mo2—C6—C7 | −75.7 (4) | C8—C7—Mo2—C9 | 33.5 (4) |
O4—Mo2—C6—C10 | 168.6 (4) | C8—C7—Mo2—C10 | 75.5 (4) |
O4—Mo2—C7—C6 | 102.0 (4) | C8—C7—Mo2—C17 | 5.3 (5) |
O4—Mo2—C7—C8 | −144.7 (4) | C8—C7—C6—C10 | −2.2 (7) |
O4—Mo2—C8—C7 | 37.4 (4) | C8—C9—Mo2—C10 | −114.5 (6) |
O4—Mo2—C8—C9 | 158.9 (4) | C8—C9—Mo2—C17 | 123.7 (5) |
O4—Mo2—C9—C8 | −31.6 (6) | C9—Mo2—O3—C11 | 18.9 (5) |
O4—Mo2—C9—C10 | 82.9 (5) | C9—Mo2—O4—C12 | −91.7 (4) |
O4—Mo2—C10—C6 | −14.0 (5) | C9—Mo2—C6—C10 | −38.3 (4) |
O4—Mo2—C10—C9 | −128.4 (4) | C9—C8—Mo2—C10 | 39.2 (4) |
N1—Mo1—O3—C11 | −27.9 (4) | C9—C8—Mo2—C17 | −54.4 (4) |
N1—Mo1—O4—C12 | 121.6 (4) | C9—C10—Mo2—C17 | 56.3 (4) |
N1—Mo1—C1—C2 | 163.9 (4) | C10—Mo2—O3—C11 | 34.3 (6) |
N1—Mo1—C1—C5 | −84.2 (4) | C10—Mo2—O4—C12 | −46.9 (4) |
N1—Mo1—C2—C1 | −20.7 (5) | C10—C6—Mo2—C17 | −12.4 (5) |
N1—Mo1—C2—C3 | −139.5 (4) | C10—C9—Mo2—C17 | −121.8 (4) |
N1—Mo1—C3—C2 | 72.5 (5) | C11—O3—Mo1—C13 | −112.1 (4) |
N1—Mo1—C3—C4 | −44.6 (6) | C11—O3—Mo2—C17 | −51.3 (4) |
N1—Mo1—C4—C3 | 154.8 (4) | C12—O4—Mo1—C13 | 42.0 (4) |
N1—Mo1—C4—C5 | 37.9 (4) | C12—O4—Mo2—C17 | 126.1 (4) |
Symmetry codes: (i) x−1/2, −y+1/2, z; (ii) −x+1/2, y−1/2, z−1/2; (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] |
Mr | 618.58 |
Crystal system, space group | Orthorhombic, Pna21 |
Temperature (K) | 180 |
a, b, c (Å) | 12.375 (2), 15.248 (2), 14.119 (2) |
V (Å3) | 2664.1 (6) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.06 |
Crystal size (mm) | 0.30 × 0.20 × 0.03 |
Data collection | |
Diffractometer | Rigaku ADSC CCD area-detector diffractometer |
Absorption correction | Multi-scan D*TREK (Molecular Structure Corporation, 1997) |
Tmin, Tmax | 0.775, 0.969 |
No. of measured, independent and observed [I > 3σ(I)] reflections | 24272, 7079, 4260 |
Rint | 0.060 |
(sin θ/λ)max (Å−1) | 0.715 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.037, 0.063, 1.22 |
No. of reflections | 7078 |
No. of parameters | 270 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.72, −2.64 |
Absolute structure | Flack (1983), 2844 Friedel pairs |
Absolute structure parameter | 0.032 (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.
Mo1—O3 | 2.093 (3) | Mo2—O4 | 2.160 (3) |
Mo1—O4 | 2.216 (4) | Mo2—N2 | 1.776 (4) |
Mo1—N1 | 1.769 (4) | Mo2—C17 | 2.237 (5) |
Mo1—C13 | 2.227 (5) | O1—N1 | 1.216 (5) |
Mo2—O3 | 2.144 (3) | O2—N2 | 1.201 (4) |
O3—Mo1—O4 | 67.2 (1) | N2—Mo2—C17 | 86.3 (2) |
O3—Mo1—N1 | 90.1 (2) | Mo1—O3—Mo2 | 110.2 (2) |
O3—Mo1—C13 | 139.3 (2) | Mo1—O3—C11 | 122.7 (3) |
O4—Mo1—N1 | 124.4 (2) | Mo2—O3—C11 | 127.1 (3) |
O4—Mo1—C13 | 81.8 (2) | Mo1—O4—Mo2 | 105.2 (2) |
N1—Mo1—C13 | 86.2 (2) | Mo1—O4—C12 | 124.2 (3) |
O3—Mo2—O4 | 67.4 (1) | Mo2—O4—C12 | 118.3 (3) |
O3—Mo2—N2 | 121.4 (2) | Mo1—N1—O1 | 170.1 (4) |
O3—Mo2—C17 | 79.9 (1) | Mo2—N2—O2 | 170.1 (5) |
O4—Mo2—N2 | 89.4 (1) | Mo1—C13—Si1 | 117.8 (3) |
O4—Mo2—C17 | 138.4 (2) | Mo2—C17—Si2 | 124.6 (3) |
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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.