Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802002258/cf6148sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802002258/cf6148Isup2.hkl |
CCDC reference: 182575
The title compound was obtained by reaction of Li(Re2(µ-PEt2)2(CO)7{C(Ph)O)} with OEt3BF4 in CHCl3 solution at room temperature. The synthesis of the precursor Li salt has been described earlier (Haupt et al., 1998a).
H atoms were placed at calculated positions, riding on the attached C atoms, with isotropic displacement parameters Uiso(H) = 1.2Ueq(C) [1.5Ueq(C) for methyl groups].
Data collection: XSCANS (Bruker, 1996); cell refinement: XSCANS; data reduction: SHELXTL (Bruker, 1998); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Fig. 1. The molecular structure of (I) with H atoms omitted. Displacement ellipsoids are drawn at the 50% probability level. |
[Re2(C9H10O)(C4H10P)2(CO)7] | Z = 2 |
Mr = 880.82 | F(000) = 836 |
Triclinic, P1 | Dx = 1.994 Mg m−3 |
a = 8.425 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 10.504 (1) Å | Cell parameters from 29 reflections |
c = 17.674 (4) Å | θ = 7.8–23.7° |
α = 73.04 (1)° | µ = 8.40 mm−1 |
β = 78.82 (1)° | T = 200 K |
γ = 88.59 (1)° | Needle, colourless |
V = 1466.8 (5) Å3 | 0.38 × 0.15 × 0.06 mm |
Bruker P4 diffractometer | 5086 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.023 |
Graphite monochromator | θmax = 27.5°, θmin = 2.5° |
ω scans | h = −10→1 |
Absorption correction: ψ scan (North et al., 1968) | k = −13→13 |
Tmin = 0.083, Tmax = 0.608 | l = −22→22 |
8026 measured reflections | 3 standard reflections every 397 reflections |
6665 independent reflections | intensity decay: 1% |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.096 | H-atom parameters constrained |
S = 0.98 | w = 1/[σ2(Fo2) + (0.0575P)2] where P = (Fo2 + 2Fc2)/3 |
6665 reflections | (Δ/σ)max < 0.001 |
330 parameters | Δρmax = 0.94 e Å−3 |
0 restraints | Δρmin = −0.82 e Å−3 |
[Re2(C9H10O)(C4H10P)2(CO)7] | γ = 88.59 (1)° |
Mr = 880.82 | V = 1466.8 (5) Å3 |
Triclinic, P1 | Z = 2 |
a = 8.425 (2) Å | Mo Kα radiation |
b = 10.504 (1) Å | µ = 8.40 mm−1 |
c = 17.674 (4) Å | T = 200 K |
α = 73.04 (1)° | 0.38 × 0.15 × 0.06 mm |
β = 78.82 (1)° |
Bruker P4 diffractometer | 5086 reflections with I > 2σ(I) |
Absorption correction: ψ scan (North et al., 1968) | Rint = 0.023 |
Tmin = 0.083, Tmax = 0.608 | 3 standard reflections every 397 reflections |
8026 measured reflections | intensity decay: 1% |
6665 independent reflections |
R[F2 > 2σ(F2)] = 0.038 | 0 restraints |
wR(F2) = 0.096 | H-atom parameters constrained |
S = 0.98 | Δρmax = 0.94 e Å−3 |
6665 reflections | Δρmin = −0.82 e Å−3 |
330 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Re1 | −0.00177 (3) | 0.37089 (3) | 0.358736 (14) | 0.02719 (10) | |
Re2 | 0.29648 (3) | 0.26519 (2) | 0.186324 (13) | 0.02267 (9) | |
P1 | 0.0457 (2) | 0.39188 (17) | 0.21057 (9) | 0.0229 (3) | |
P2 | 0.2345 (2) | 0.22693 (18) | 0.33571 (10) | 0.0265 (4) | |
C1 | 0.1543 (10) | 0.5263 (8) | 0.3305 (5) | 0.0409 (18) | |
O1 | 0.2431 (8) | 0.6143 (6) | 0.3136 (4) | 0.0615 (18) | |
C2 | −0.0091 (10) | 0.3383 (8) | 0.4742 (5) | 0.0415 (19) | |
O2 | −0.0171 (8) | 0.3213 (7) | 0.5422 (3) | 0.0628 (19) | |
C3 | −0.1901 (10) | 0.4838 (8) | 0.3595 (5) | 0.045 (2) | |
O3 | −0.3029 (8) | 0.5454 (7) | 0.3635 (5) | 0.073 (2) | |
C4 | −0.1455 (9) | 0.2136 (7) | 0.3829 (4) | 0.0339 (16) | |
O4 | −0.2281 (6) | 0.1207 (6) | 0.3990 (3) | 0.0450 (14) | |
C5 | 0.4216 (8) | 0.4263 (7) | 0.1823 (4) | 0.0291 (15) | |
O5 | 0.4946 (6) | 0.5173 (5) | 0.1794 (3) | 0.0405 (13) | |
C6 | 0.4908 (8) | 0.1617 (7) | 0.1847 (4) | 0.0292 (15) | |
O6 | 0.6060 (6) | 0.0997 (6) | 0.1838 (3) | 0.0462 (14) | |
C7 | 0.3244 (9) | 0.3250 (7) | 0.0684 (4) | 0.0335 (16) | |
O7 | 0.3471 (8) | 0.3634 (6) | 0.0003 (3) | 0.0541 (16) | |
C8 | 0.1666 (8) | 0.0945 (7) | 0.1907 (4) | 0.0265 (14) | |
O8 | 0.0338 (6) | 0.0492 (5) | 0.2426 (3) | 0.0371 (12) | |
C9 | −0.0559 (10) | −0.0722 (8) | 0.2430 (5) | 0.050 (2) | |
H9A | −0.1004 | −0.0545 | 0.1932 | 0.060* | |
H9B | 0.0185 | −0.1470 | 0.2450 | 0.060* | |
C10 | −0.1868 (11) | −0.1067 (9) | 0.3133 (5) | 0.053 (2) | |
H10A | −0.2426 | −0.1890 | 0.3159 | 0.080* | |
H10B | −0.2635 | −0.0345 | 0.3092 | 0.080* | |
H10C | −0.1423 | −0.1198 | 0.3622 | 0.080* | |
C11 | 0.2245 (8) | 0.0148 (7) | 0.1321 (4) | 0.0296 (15) | |
C12 | 0.1800 (10) | 0.0474 (8) | 0.0582 (4) | 0.0400 (18) | |
H12 | 0.1097 | 0.1188 | 0.0440 | 0.048* | |
C13 | 0.2379 (10) | −0.0239 (9) | 0.0043 (5) | 0.046 (2) | |
H13 | 0.2057 | −0.0024 | −0.0464 | 0.055* | |
C14 | 0.3422 (10) | −0.1259 (8) | 0.0244 (5) | 0.043 (2) | |
H14 | 0.3835 | −0.1736 | −0.0129 | 0.051* | |
C15 | 0.3859 (10) | −0.1583 (8) | 0.0976 (5) | 0.0416 (19) | |
H15 | 0.4569 | −0.2293 | 0.1112 | 0.050* | |
C16 | 0.3277 (9) | −0.0883 (7) | 0.1530 (4) | 0.0380 (17) | |
H16 | 0.3586 | −0.1112 | 0.2041 | 0.046* | |
C17 | 0.0751 (9) | 0.5669 (7) | 0.1445 (4) | 0.0317 (15) | |
H17A | 0.1675 | 0.6080 | 0.1570 | 0.038* | |
H17B | 0.1061 | 0.5649 | 0.0879 | 0.038* | |
C18 | −0.0674 (11) | 0.6565 (7) | 0.1501 (5) | 0.047 (2) | |
H18A | −0.1542 | 0.6261 | 0.1292 | 0.070* | |
H18B | −0.0334 | 0.7481 | 0.1182 | 0.070* | |
H18C | −0.1067 | 0.6533 | 0.2066 | 0.070* | |
C19 | −0.1352 (8) | 0.3378 (7) | 0.1830 (4) | 0.0313 (15) | |
H19A | −0.1599 | 0.2429 | 0.2136 | 0.038* | |
H19B | −0.2276 | 0.3895 | 0.2004 | 0.038* | |
C20 | −0.1223 (9) | 0.3529 (8) | 0.0934 (4) | 0.0398 (18) | |
H20A | −0.2211 | 0.3158 | 0.0852 | 0.060* | |
H20B | −0.0287 | 0.3051 | 0.0746 | 0.060* | |
H20C | −0.1090 | 0.4475 | 0.0628 | 0.060* | |
C21 | 0.4149 (8) | 0.2711 (9) | 0.3697 (4) | 0.0372 (18) | |
H21A | 0.5053 | 0.2165 | 0.3536 | 0.045* | |
H21B | 0.4463 | 0.3654 | 0.3404 | 0.045* | |
C22 | 0.3971 (11) | 0.2533 (10) | 0.4593 (4) | 0.056 (2) | |
H22A | 0.4998 | 0.2780 | 0.4704 | 0.084* | |
H22B | 0.3680 | 0.1600 | 0.4895 | 0.084* | |
H22C | 0.3120 | 0.3104 | 0.4760 | 0.084* | |
C23 | 0.1916 (9) | 0.0525 (7) | 0.3982 (4) | 0.0346 (16) | |
H23A | 0.1642 | 0.0509 | 0.4556 | 0.042* | |
H23B | 0.0949 | 0.0188 | 0.3850 | 0.042* | |
C24 | 0.3292 (10) | −0.0431 (8) | 0.3886 (5) | 0.049 (2) | |
H24A | 0.2955 | −0.1326 | 0.4244 | 0.074* | |
H24B | 0.4253 | −0.0124 | 0.4027 | 0.074* | |
H24C | 0.3548 | −0.0456 | 0.3326 | 0.074* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Re1 | 0.02897 (16) | 0.02844 (16) | 0.02476 (14) | 0.00114 (12) | −0.00087 (11) | −0.01157 (11) |
Re2 | 0.02382 (14) | 0.02338 (15) | 0.02012 (13) | 0.00128 (10) | −0.00226 (10) | −0.00667 (10) |
P1 | 0.0237 (8) | 0.0229 (8) | 0.0220 (7) | 0.0013 (7) | −0.0046 (6) | −0.0066 (6) |
P2 | 0.0268 (8) | 0.0310 (9) | 0.0214 (7) | 0.0013 (7) | −0.0059 (7) | −0.0066 (7) |
C1 | 0.044 (4) | 0.036 (4) | 0.041 (4) | 0.003 (4) | 0.004 (4) | −0.016 (3) |
O1 | 0.071 (4) | 0.051 (4) | 0.060 (4) | −0.024 (4) | 0.006 (3) | −0.023 (3) |
C2 | 0.044 (4) | 0.044 (5) | 0.037 (4) | −0.009 (4) | 0.000 (3) | −0.017 (3) |
O2 | 0.079 (5) | 0.084 (5) | 0.027 (3) | −0.009 (4) | −0.002 (3) | −0.023 (3) |
C3 | 0.039 (4) | 0.036 (4) | 0.056 (5) | 0.004 (4) | 0.001 (4) | −0.012 (4) |
O3 | 0.046 (4) | 0.050 (4) | 0.111 (6) | 0.014 (3) | 0.012 (4) | −0.021 (4) |
C4 | 0.029 (4) | 0.035 (4) | 0.032 (3) | 0.009 (3) | 0.000 (3) | −0.005 (3) |
O4 | 0.037 (3) | 0.041 (3) | 0.052 (3) | −0.007 (3) | −0.003 (3) | −0.008 (3) |
C5 | 0.022 (3) | 0.036 (4) | 0.029 (3) | 0.005 (3) | −0.006 (3) | −0.008 (3) |
O5 | 0.038 (3) | 0.029 (3) | 0.051 (3) | −0.007 (2) | −0.005 (2) | −0.009 (2) |
C6 | 0.028 (3) | 0.034 (4) | 0.025 (3) | 0.000 (3) | −0.006 (3) | −0.008 (3) |
O6 | 0.031 (3) | 0.042 (3) | 0.063 (4) | 0.010 (3) | −0.006 (3) | −0.015 (3) |
C7 | 0.037 (4) | 0.038 (4) | 0.025 (3) | 0.008 (3) | −0.003 (3) | −0.009 (3) |
O7 | 0.073 (4) | 0.055 (4) | 0.026 (3) | 0.010 (3) | −0.005 (3) | −0.003 (2) |
C8 | 0.031 (3) | 0.025 (3) | 0.024 (3) | 0.005 (3) | −0.008 (3) | −0.007 (2) |
O8 | 0.037 (3) | 0.033 (3) | 0.041 (3) | −0.007 (2) | 0.003 (2) | −0.016 (2) |
C9 | 0.040 (4) | 0.042 (5) | 0.069 (6) | −0.018 (4) | −0.001 (4) | −0.023 (4) |
C10 | 0.055 (5) | 0.039 (5) | 0.060 (5) | −0.010 (4) | −0.002 (4) | −0.011 (4) |
C11 | 0.030 (3) | 0.027 (3) | 0.033 (3) | −0.001 (3) | −0.002 (3) | −0.013 (3) |
C12 | 0.046 (4) | 0.045 (5) | 0.040 (4) | 0.006 (4) | −0.014 (3) | −0.026 (3) |
C13 | 0.047 (5) | 0.060 (5) | 0.038 (4) | −0.001 (4) | −0.003 (4) | −0.030 (4) |
C14 | 0.046 (5) | 0.038 (4) | 0.047 (4) | 0.002 (4) | 0.010 (4) | −0.030 (4) |
C15 | 0.046 (5) | 0.027 (4) | 0.054 (5) | 0.002 (3) | 0.001 (4) | −0.021 (3) |
C16 | 0.046 (4) | 0.032 (4) | 0.037 (4) | 0.004 (3) | −0.006 (3) | −0.012 (3) |
C17 | 0.039 (4) | 0.023 (3) | 0.031 (3) | −0.002 (3) | −0.011 (3) | −0.001 (3) |
C18 | 0.060 (5) | 0.025 (4) | 0.054 (5) | 0.012 (4) | −0.011 (4) | −0.012 (3) |
C19 | 0.027 (3) | 0.035 (4) | 0.033 (3) | 0.001 (3) | −0.006 (3) | −0.013 (3) |
C20 | 0.037 (4) | 0.043 (4) | 0.043 (4) | −0.005 (4) | −0.014 (3) | −0.014 (3) |
C21 | 0.028 (4) | 0.059 (5) | 0.031 (3) | −0.005 (4) | −0.012 (3) | −0.017 (3) |
C22 | 0.051 (5) | 0.088 (7) | 0.034 (4) | −0.007 (5) | −0.015 (4) | −0.021 (4) |
C23 | 0.041 (4) | 0.030 (4) | 0.027 (3) | 0.002 (3) | −0.005 (3) | 0.000 (3) |
C24 | 0.052 (5) | 0.040 (5) | 0.045 (4) | 0.017 (4) | −0.007 (4) | 0.001 (4) |
Re1—C2 | 1.956 (8) | C12—C13 | 1.387 (10) |
Re1—C3 | 1.958 (9) | C12—H12 | 0.950 |
Re1—C4 | 1.966 (8) | C13—C14 | 1.377 (12) |
Re1—C1 | 2.004 (8) | C13—H13 | 0.950 |
Re1—P2 | 2.5122 (19) | C14—C15 | 1.358 (11) |
Re1—P1 | 2.5154 (17) | C14—H14 | 0.950 |
Re2—C6 | 1.943 (7) | C15—C16 | 1.399 (10) |
Re2—C7 | 1.962 (7) | C15—H15 | 0.950 |
Re2—C5 | 1.993 (7) | C16—H16 | 0.950 |
Re2—C8 | 2.098 (7) | C17—C18 | 1.513 (11) |
Re2—P2 | 2.5023 (17) | C17—H17A | 0.990 |
Re2—P1 | 2.5024 (18) | C17—H17B | 0.990 |
P1—C19 | 1.837 (7) | C18—H18A | 0.980 |
P1—C17 | 1.861 (6) | C18—H18B | 0.980 |
P2—C23 | 1.846 (7) | C18—H18C | 0.980 |
P2—C21 | 1.854 (7) | C19—C20 | 1.529 (9) |
C1—O1 | 1.136 (9) | C19—H19A | 0.990 |
C2—O2 | 1.152 (9) | C19—H19B | 0.990 |
C3—O3 | 1.139 (10) | C20—H20A | 0.980 |
C4—O4 | 1.145 (9) | C20—H20B | 0.980 |
C5—O5 | 1.132 (8) | C20—H20C | 0.980 |
C6—O6 | 1.155 (8) | C21—C22 | 1.518 (9) |
C7—O7 | 1.130 (8) | C21—H21A | 0.990 |
C8—O8 | 1.300 (8) | C21—H21B | 0.990 |
C8—C11 | 1.517 (9) | C22—H22A | 0.980 |
O8—C9 | 1.495 (9) | C22—H22B | 0.980 |
C9—C10 | 1.455 (11) | C22—H22C | 0.980 |
C9—H9A | 0.990 | C23—C24 | 1.532 (10) |
C9—H9B | 0.990 | C23—H23A | 0.990 |
C10—H10A | 0.980 | C23—H23B | 0.990 |
C10—H10B | 0.980 | C24—H24A | 0.980 |
C10—H10C | 0.980 | C24—H24B | 0.980 |
C11—C12 | 1.374 (10) | C24—H24C | 0.980 |
C11—C16 | 1.382 (10) | ||
C2—Re1—C3 | 92.9 (4) | C12—C11—C8 | 120.7 (7) |
C2—Re1—C4 | 89.8 (3) | C16—C11—C8 | 119.0 (6) |
C3—Re1—C4 | 89.9 (3) | C11—C12—C13 | 120.0 (8) |
C2—Re1—C1 | 91.8 (3) | C11—C12—H12 | 120.0 |
C3—Re1—C1 | 92.8 (3) | C13—C12—H12 | 120.0 |
C4—Re1—C1 | 176.8 (3) | C14—C13—C12 | 120.0 (8) |
C2—Re1—P2 | 96.0 (3) | C14—C13—H13 | 120.0 |
C3—Re1—P2 | 170.9 (3) | C12—C13—H13 | 120.0 |
C4—Re1—P2 | 88.3 (2) | C15—C14—C13 | 120.1 (7) |
C1—Re1—P2 | 88.7 (2) | C15—C14—H14 | 120.0 |
C2—Re1—P1 | 171.2 (3) | C13—C14—H14 | 120.0 |
C3—Re1—P1 | 95.9 (3) | C14—C15—C16 | 120.8 (8) |
C4—Re1—P1 | 90.6 (2) | C14—C15—H15 | 119.6 |
C1—Re1—P1 | 87.4 (2) | C16—C15—H15 | 119.6 |
P2—Re1—P1 | 75.23 (5) | C11—C16—C15 | 118.9 (7) |
C6—Re2—C7 | 93.4 (3) | C11—C16—H16 | 120.6 |
C6—Re2—C5 | 91.4 (3) | C15—C16—H16 | 120.6 |
C7—Re2—C5 | 89.8 (3) | C18—C17—P1 | 117.0 (5) |
C6—Re2—C8 | 88.1 (3) | C18—C17—H17A | 108.1 |
C7—Re2—C8 | 90.3 (3) | P1—C17—H17A | 108.1 |
C5—Re2—C8 | 179.5 (3) | C18—C17—H17B | 108.1 |
C6—Re2—P2 | 95.78 (19) | P1—C17—H17B | 108.1 |
C7—Re2—P2 | 169.7 (2) | H17A—C17—H17B | 107.3 |
C5—Re2—P2 | 85.28 (19) | C17—C18—H18A | 109.5 |
C8—Re2—P2 | 94.66 (17) | C17—C18—H18B | 109.5 |
C6—Re2—P1 | 171.38 (19) | H18A—C18—H18B | 109.5 |
C7—Re2—P1 | 95.1 (2) | C17—C18—H18C | 109.5 |
C5—Re2—P1 | 87.2 (2) | H18A—C18—H18C | 109.5 |
C8—Re2—P1 | 93.27 (19) | H18B—C18—H18C | 109.5 |
P2—Re2—P1 | 75.63 (6) | C20—C19—P1 | 115.5 (5) |
C19—P1—C17 | 101.3 (3) | C20—C19—H19A | 108.4 |
C19—P1—Re2 | 116.5 (2) | P1—C19—H19A | 108.4 |
C17—P1—Re2 | 110.2 (2) | C20—C19—H19B | 108.4 |
C19—P1—Re1 | 111.1 (2) | P1—C19—H19B | 108.4 |
C17—P1—Re1 | 113.8 (2) | H19A—C19—H19B | 107.5 |
Re2—P1—Re1 | 104.30 (6) | C19—C20—H20A | 109.5 |
C23—P2—C21 | 101.7 (4) | C19—C20—H20B | 109.5 |
C23—P2—Re2 | 116.1 (2) | H20A—C20—H20B | 109.5 |
C21—P2—Re2 | 110.0 (2) | C19—C20—H20C | 109.5 |
C23—P2—Re1 | 111.7 (2) | H20A—C20—H20C | 109.5 |
C21—P2—Re1 | 113.2 (3) | H20B—C20—H20C | 109.5 |
Re2—P2—Re1 | 104.40 (6) | C22—C21—P2 | 116.6 (5) |
O1—C1—Re1 | 179.3 (7) | C22—C21—H21A | 108.2 |
O2—C2—Re1 | 178.1 (8) | P2—C21—H21A | 108.2 |
O3—C3—Re1 | 176.7 (8) | C22—C21—H21B | 108.2 |
O4—C4—Re1 | 178.2 (7) | P2—C21—H21B | 108.2 |
O5—C5—Re2 | 178.9 (6) | H21A—C21—H21B | 107.3 |
O6—C6—Re2 | 179.7 (6) | C21—C22—H22A | 109.5 |
O7—C7—Re2 | 176.5 (7) | C21—C22—H22B | 109.5 |
O8—C8—C11 | 115.4 (6) | H22A—C22—H22B | 109.5 |
O8—C8—Re2 | 123.6 (5) | C21—C22—H22C | 109.5 |
C11—C8—Re2 | 121.0 (4) | H22A—C22—H22C | 109.5 |
C8—O8—C9 | 121.8 (6) | H22B—C22—H22C | 109.5 |
C10—C9—O8 | 108.7 (7) | C24—C23—P2 | 115.5 (5) |
C10—C9—H9A | 109.9 | C24—C23—H23A | 108.4 |
O8—C9—H9A | 109.9 | P2—C23—H23A | 108.4 |
C10—C9—H9B | 109.9 | C24—C23—H23B | 108.4 |
O8—C9—H9B | 109.9 | P2—C23—H23B | 108.4 |
H9A—C9—H9B | 108.3 | H23A—C23—H23B | 107.5 |
C9—C10—H10A | 109.5 | C23—C24—H24A | 109.5 |
C9—C10—H10B | 109.5 | C23—C24—H24B | 109.5 |
H10A—C10—H10B | 109.5 | H24A—C24—H24B | 109.5 |
C9—C10—H10C | 109.5 | C23—C24—H24C | 109.5 |
H10A—C10—H10C | 109.5 | H24A—C24—H24C | 109.5 |
H10B—C10—H10C | 109.5 | H24B—C24—H24C | 109.5 |
C12—C11—C16 | 120.3 (7) | ||
C7—Re2—P1—C19 | 66.8 (3) | C1—Re1—P2—C21 | 37.1 (3) |
C5—Re2—P1—C19 | 156.4 (3) | P1—Re1—P2—C21 | 124.7 (3) |
C8—Re2—P1—C19 | −23.8 (3) | C2—Re1—P2—Re2 | −174.3 (2) |
P2—Re2—P1—C19 | −117.8 (2) | C4—Re1—P2—Re2 | 96.1 (2) |
C7—Re2—P1—C17 | −47.8 (3) | C1—Re1—P2—Re2 | −82.6 (2) |
C5—Re2—P1—C17 | 41.7 (3) | P1—Re1—P2—Re2 | 5.04 (6) |
C8—Re2—P1—C17 | −138.4 (3) | C6—Re2—C8—O8 | 130.5 (6) |
P2—Re2—P1—C17 | 127.6 (3) | C7—Re2—C8—O8 | −136.2 (6) |
C7—Re2—P1—Re1 | −170.4 (2) | P2—Re2—C8—O8 | 34.8 (6) |
C5—Re2—P1—Re1 | −80.79 (19) | P1—Re2—C8—O8 | −41.0 (5) |
C8—Re2—P1—Re1 | 99.03 (17) | C6—Re2—C8—C11 | −49.3 (5) |
P2—Re2—P1—Re1 | 5.05 (6) | C7—Re2—C8—C11 | 44.0 (6) |
C3—Re1—P1—C19 | −56.9 (4) | P2—Re2—C8—C11 | −145.0 (5) |
C4—Re1—P1—C19 | 33.1 (3) | P1—Re2—C8—C11 | 139.2 (5) |
C1—Re1—P1—C19 | −149.4 (3) | C11—C8—O8—C9 | −0.8 (10) |
P2—Re1—P1—C19 | 121.2 (3) | Re2—C8—O8—C9 | 179.4 (6) |
C3—Re1—P1—C17 | 56.7 (4) | C8—O8—C9—C10 | 173.1 (7) |
C4—Re1—P1—C17 | 146.7 (3) | O8—C8—C11—C12 | 92.7 (8) |
C1—Re1—P1—C17 | −35.8 (3) | Re2—C8—C11—C12 | −87.5 (8) |
P2—Re1—P1—C17 | −125.2 (3) | O8—C8—C11—C16 | −89.7 (8) |
C3—Re1—P1—Re2 | 176.9 (2) | Re2—C8—C11—C16 | 90.1 (7) |
C4—Re1—P1—Re2 | −93.1 (2) | C16—C11—C12—C13 | 0.5 (11) |
C1—Re1—P1—Re2 | 84.3 (2) | C8—C11—C12—C13 | 178.1 (7) |
P2—Re1—P1—Re2 | −5.04 (6) | C11—C12—C13—C14 | −1.1 (12) |
C6—Re2—P2—C23 | −62.5 (3) | C12—C13—C14—C15 | 1.2 (12) |
C5—Re2—P2—C23 | −153.4 (3) | C13—C14—C15—C16 | −0.7 (12) |
C8—Re2—P2—C23 | 26.1 (3) | C12—C11—C16—C15 | 0.1 (11) |
P1—Re2—P2—C23 | 118.3 (3) | C8—C11—C16—C15 | −177.6 (6) |
C6—Re2—P2—C21 | 52.3 (4) | C14—C15—C16—C11 | 0.0 (12) |
C5—Re2—P2—C21 | −38.6 (4) | C19—P1—C17—C18 | 54.6 (7) |
C8—Re2—P2—C21 | 140.9 (3) | Re2—P1—C17—C18 | 178.5 (5) |
P1—Re2—P2—C21 | −126.9 (3) | Re1—P1—C17—C18 | −64.8 (6) |
C6—Re2—P2—Re1 | 174.2 (2) | C17—P1—C19—C20 | 55.9 (6) |
C5—Re2—P2—Re1 | 83.3 (2) | Re2—P1—C19—C20 | −63.7 (6) |
C8—Re2—P2—Re1 | −97.25 (19) | Re1—P1—C19—C20 | 177.1 (5) |
P1—Re2—P2—Re1 | −5.06 (6) | C23—P2—C21—C22 | −56.3 (7) |
C2—Re1—P2—C23 | 59.5 (3) | Re2—P2—C21—C22 | −180.0 (6) |
C4—Re1—P2—C23 | −30.1 (3) | Re1—P2—C21—C22 | 63.7 (7) |
C1—Re1—P2—C23 | 151.2 (3) | C21—P2—C23—C24 | −58.7 (7) |
P1—Re1—P2—C23 | −121.2 (3) | Re2—P2—C23—C24 | 60.7 (6) |
C2—Re1—P2—C21 | −54.6 (3) | Re1—P2—C23—C24 | −179.8 (5) |
C4—Re1—P2—C21 | −144.2 (3) |
Experimental details
Crystal data | |
Chemical formula | [Re2(C9H10O)(C4H10P)2(CO)7] |
Mr | 880.82 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 200 |
a, b, c (Å) | 8.425 (2), 10.504 (1), 17.674 (4) |
α, β, γ (°) | 73.04 (1), 78.82 (1), 88.59 (1) |
V (Å3) | 1466.8 (5) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 8.40 |
Crystal size (mm) | 0.38 × 0.15 × 0.06 |
Data collection | |
Diffractometer | Bruker P4 diffractometer |
Absorption correction | ψ scan (North et al., 1968) |
Tmin, Tmax | 0.083, 0.608 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 8026, 6665, 5086 |
Rint | 0.023 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.038, 0.096, 0.98 |
No. of reflections | 6665 |
No. of parameters | 330 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.94, −0.82 |
Computer programs: XSCANS (Bruker, 1996), XSCANS, SHELXTL (Bruker, 1998), SHELXTL.
Re1—P2 | 2.5122 (19) | Re2—P1 | 2.5024 (18) |
Re1—P1 | 2.5154 (17) | C8—O8 | 1.300 (8) |
Re2—C8 | 2.098 (7) | C8—C11 | 1.517 (9) |
Re2—P2 | 2.5023 (17) | O8—C9 | 1.495 (9) |
P2—Re1—P1 | 75.23 (5) | Re2—P2—Re1 | 104.40 (6) |
P2—Re2—P1 | 75.63 (6) | O8—C8—Re2 | 123.6 (5) |
Re2—P1—Re1 | 104.30 (6) |
The reaction of Re2(µ-PR2)2(CO)8 with nucleophilic lithium organyls LiR' leads to the salts Li(Re2(µ-PR2)2(CO)7{ax-C(R')O} which then can be converted to Fischer-type carbene complexes (Haupt et al., 1998a). The title compound, (I), with R = ethyl and E, R' = phenyl, is an axial monocarbene complex with a Re2P2 ring and slightly distorted octahedral coordination at both Re atoms. The C(Ph)OEt carbene group with a Z configuration is axially attached to Re2 with a Re═C double-bond length of 2.098 (7) Å. The orientation of the ReCOEt group is parallel to the Re···Re vector with a Re···Re—C8—O8 torsion angle of -3.2 (6)°. The Re1—P bonds of 2.5154 (17) and 2.5122 (19) Å for P1 and P2, respectively, are slightly longer than those for Re2–P of 2.5024 (18) and 2.5023 (17) Å, and reflect the unsymmetrical monosubstitution of this compound. These distances are, on average, slightly shorter than the Re—P bonds of the related mono- and dicarbene complexes which have µ-PPh2-bridging ligands instead (Haupt et al., 1998b). The average values for the enclosed ring angles are Re—P—Re = 104.35 (6)° and P–Re–P = 75.43 (6)°. The Re2P2 ring is folded, with an ReP2/P2Re dihedral angle of 6.2 (1)°. This is a well known effect due to an intramolecular balance of unsymmetrical or sterically unfavourable substituted carbonyl complexes of this type (Haupt et al., 1998a,b; Flörke & Petters, 2001). The C—Re—Re—C torsion angles range from 0.2 (4) to 8.8 (4)° (absolute values), in accordance with the ecliptic carbonyl-ligand arrangements.