Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807036902/rk2027sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807036902/rk2027Isup2.hkl |
CCDC reference: 660055
The title compound was prepared by the interaction between Cp(CO)2Re?C?CHPh and Pt(PPh3)4 in benzene and at 298 K, 3 h. Suitable single crystals were obtained by recrystallization from ether at 298 K.
Seven phenyl cycles were idealized and refined as rigid groups with C—C bond lengths of 1.390 Å. All H atoms were positioned geometrically (C—H 0.93 Å) and refined using a riding model with Uiso(H) = 1.2Ueq(C).
There are the difference density maximum of 3.11 e/Å3 at a distance of 0.87Å from Re atom and the minimum of -1.48 e/Å3 at a distance of 0.68Å from the same atom.
The solvate diethyl ether molecule is situated close to the inversion center (the distance from the center to the oxygen atom about 0.5 Å) with the statistical occupancy of 0.5. A l l non-hydrogen atoms of the solvate molecule were refined isotropically and the C—O and C—C distances were restrained by SHELXL DFIX instructions to values of 1.43 and 1.50 Å respectively (Allen et al., 1987).
The molecule of the title compound, [η5-C5H5)(CO)2RePt (µ-C?CHPh)(PPh3)2] Et2O, is the dinuclear complex containing the Re and Pt atoms bridged by the µ-phenylvinylidene ligand. The phenyl ring and the C?C bond of vinylidene coupled with the Re—Pt-µ-C triangle form an almost planar system. Corresponding geometry was found for the analogous MnPt complex (Vasiliev et al., 2007). The structures of some µ-carbene (Casey et al., 1992; Bergamo et al., 2000) and µ-carbyne (Bergamo et al., 2000) complexes containing the Re—Pt-µ-C triangle system as the central fragment of molecule were reported.
The corresponding geometry in the analogous MnPt complex was reported by Vasiliev et al. (2007). For crystal structures of related µ-carbene complexes containing the Re–Pt–µ-C triangle system, see: Casey et al. (1992); Bergamo et al. (2000). For related literature, see: Allen et al. (1987).
Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXTL (Sheldrick, 2004); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Fig. 1. The molecular structure of title compound, with atom labels and 50% probability displacement ellipsoids for non-H atoms. H atoms, except for H2 atom, omitted for clarity. |
[PtRe(C5H5)(C8H6)(C18H15P)2(CO)2]·0.5C4H10O | F(000) = 2268 |
Mr = 1166.13 | Dx = 1.709 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 9791 reflections |
a = 22.529 (1) Å | θ = 2.4–27.4° |
b = 9.1786 (5) Å | µ = 5.86 mm−1 |
c = 21.941 (1) Å | T = 296 K |
β = 92.469 (1)° | Block, orange |
V = 4532.9 (4) Å3 | 0.36 × 0.21 × 0.18 mm |
Z = 4 |
Bruker SMART 4K CCD area-detector diffractometer | 10402 independent reflections |
Radiation source: fine-focus sealed tube | 7336 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.038 |
φ and ω scans | θmax = 27.5°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2004) | h = −29→29 |
Tmin = 0.278, Tmax = 0.418 | k = −11→11 |
38759 measured reflections | l = −28→28 |
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)] = 0.031 | Hydrogen site location: constr |
wR(F2) = 0.073 | H-atom parameters constrained |
S = 1.00 | w = 1/[σ2(Fo2) + (0.0315P)2 + 4.6963P] where P = (Fo2 + 2Fc2)/3 |
10402 reflections | (Δ/σ)max = 0.002 |
453 parameters | Δρmax = 3.11 e Å−3 |
4 restraints | Δρmin = −1.48 e Å−3 |
[PtRe(C5H5)(C8H6)(C18H15P)2(CO)2]·0.5C4H10O | V = 4532.9 (4) Å3 |
Mr = 1166.13 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 22.529 (1) Å | µ = 5.86 mm−1 |
b = 9.1786 (5) Å | T = 296 K |
c = 21.941 (1) Å | 0.36 × 0.21 × 0.18 mm |
β = 92.469 (1)° |
Bruker SMART 4K CCD area-detector diffractometer | 10402 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2004) | 7336 reflections with I > 2σ(I) |
Tmin = 0.278, Tmax = 0.418 | Rint = 0.038 |
38759 measured reflections |
R[F2 > 2σ(F2)] = 0.031 | 4 restraints |
wR(F2) = 0.073 | H-atom parameters constrained |
S = 1.00 | Δρmax = 3.11 e Å−3 |
10402 reflections | Δρmin = −1.48 e Å−3 |
453 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 > 2σ(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 | Occ. (<1) | |
Pt | 0.248866 (8) | 0.446207 (18) | 0.314347 (8) | 0.03293 (5) | |
Re | 0.186644 (9) | 0.56086 (2) | 0.215806 (8) | 0.04006 (6) | |
C11 | 0.1165 (3) | 0.5152 (8) | 0.1403 (3) | 0.0688 (17) | |
H11 | 0.0868 | 0.5833 | 0.1314 | 0.083* | |
C12 | 0.1711 (3) | 0.5085 (8) | 0.1141 (2) | 0.0674 (17) | |
H12 | 0.1843 | 0.5712 | 0.0843 | 0.081* | |
C13 | 0.2037 (3) | 0.3910 (7) | 0.1401 (3) | 0.0668 (17) | |
H13 | 0.2421 | 0.3633 | 0.1311 | 0.080* | |
C14 | 0.1675 (3) | 0.3247 (7) | 0.1818 (3) | 0.0712 (18) | |
H14 | 0.1777 | 0.2430 | 0.2051 | 0.085* | |
C15 | 0.1135 (3) | 0.3995 (8) | 0.1833 (3) | 0.0707 (18) | |
H15 | 0.0819 | 0.3779 | 0.2077 | 0.085* | |
P1 | 0.34065 (5) | 0.38572 (13) | 0.35326 (6) | 0.0352 (3) | |
P2 | 0.18454 (5) | 0.31895 (13) | 0.37882 (5) | 0.0371 (3) | |
C1 | 0.2770 (2) | 0.5451 (5) | 0.2392 (2) | 0.0387 (10) | |
C2 | 0.3310 (2) | 0.5629 (5) | 0.2158 (2) | 0.0462 (12) | |
H2 | 0.3619 | 0.5207 | 0.2390 | 0.055* | |
C3 | 0.1518 (2) | 0.6161 (6) | 0.2899 (2) | 0.0512 (13) | |
O3 | 0.12681 (18) | 0.6630 (5) | 0.33088 (18) | 0.0728 (12) | |
C4 | 0.1973 (3) | 0.7638 (7) | 0.2106 (2) | 0.0580 (15) | |
O4 | 0.2019 (3) | 0.8908 (5) | 0.2078 (2) | 0.0956 (17) | |
C5 | 0.35039 (15) | 0.6378 (4) | 0.15943 (13) | 0.0445 (12) | |
C6 | 0.41017 (14) | 0.6250 (4) | 0.14714 (16) | 0.0579 (15) | |
H6 | 0.4351 | 0.5677 | 0.1721 | 0.069* | |
C7 | 0.43266 (13) | 0.6977 (4) | 0.09758 (18) | 0.0716 (18) | |
H7 | 0.4727 | 0.6891 | 0.0894 | 0.086* | |
C8 | 0.39537 (19) | 0.7832 (4) | 0.06030 (14) | 0.075 (2) | |
H8 | 0.4104 | 0.8318 | 0.0271 | 0.090* | |
C9 | 0.33558 (18) | 0.7960 (4) | 0.07259 (15) | 0.0668 (17) | |
H9 | 0.3106 | 0.8533 | 0.0476 | 0.080* | |
C10 | 0.31309 (12) | 0.7233 (4) | 0.12215 (16) | 0.0547 (14) | |
H10 | 0.2731 | 0.7319 | 0.1304 | 0.066* | |
C16 | 0.39374 (13) | 0.5381 (3) | 0.36984 (15) | 0.0417 (11) | |
C17 | 0.44538 (14) | 0.5143 (3) | 0.40541 (15) | 0.0501 (13) | |
H17 | 0.4541 | 0.4215 | 0.4203 | 0.060* | |
C18 | 0.48397 (12) | 0.6292 (4) | 0.41877 (16) | 0.0584 (15) | |
H18 | 0.5185 | 0.6133 | 0.4426 | 0.070* | |
C19 | 0.47092 (15) | 0.7679 (3) | 0.39656 (18) | 0.0671 (17) | |
H19 | 0.4967 | 0.8447 | 0.4055 | 0.081* | |
C20 | 0.41928 (17) | 0.7917 (3) | 0.36100 (17) | 0.0654 (17) | |
H20 | 0.4105 | 0.8845 | 0.3461 | 0.078* | |
C21 | 0.38069 (13) | 0.6768 (3) | 0.34764 (15) | 0.0503 (13) | |
H21 | 0.3461 | 0.6927 | 0.3238 | 0.060* | |
C22 | 0.35058 (15) | 0.2911 (3) | 0.42695 (11) | 0.0381 (11) | |
C23 | 0.33064 (15) | 0.3641 (3) | 0.47767 (15) | 0.0492 (13) | |
H23 | 0.3110 | 0.4527 | 0.4729 | 0.059* | |
C24 | 0.34009 (17) | 0.3046 (4) | 0.53554 (12) | 0.0646 (16) | |
H24 | 0.3268 | 0.3535 | 0.5695 | 0.078* | |
C25 | 0.36947 (18) | 0.1722 (4) | 0.54270 (13) | 0.0702 (18) | |
H25 | 0.3758 | 0.1324 | 0.5814 | 0.084* | |
C26 | 0.38941 (16) | 0.0991 (3) | 0.49198 (18) | 0.0691 (18) | |
H26 | 0.4091 | 0.0105 | 0.4968 | 0.083* | |
C27 | 0.37996 (15) | 0.1586 (3) | 0.43411 (15) | 0.0518 (13) | |
H27 | 0.3933 | 0.1098 | 0.4002 | 0.062* | |
C28 | 0.37716 (14) | 0.2656 (3) | 0.29846 (14) | 0.0406 (11) | |
C29 | 0.43784 (14) | 0.2665 (4) | 0.28940 (17) | 0.0656 (16) | |
H29 | 0.4626 | 0.3297 | 0.3118 | 0.079* | |
C30 | 0.46151 (14) | 0.1729 (5) | 0.24695 (19) | 0.085 (2) | |
H30 | 0.5021 | 0.1736 | 0.2409 | 0.103* | |
C31 | 0.4245 (2) | 0.0784 (4) | 0.21355 (17) | 0.084 (2) | |
H31 | 0.4403 | 0.0158 | 0.1852 | 0.100* | |
C32 | 0.3638 (2) | 0.0775 (4) | 0.22261 (18) | 0.085 (2) | |
H32 | 0.3390 | 0.0143 | 0.2003 | 0.102* | |
C33 | 0.34014 (13) | 0.1711 (4) | 0.26506 (18) | 0.0662 (17) | |
H33 | 0.2995 | 0.1704 | 0.2711 | 0.079* | |
C34 | 0.10755 (13) | 0.2813 (4) | 0.34826 (16) | 0.0471 (12) | |
C35 | 0.06360 (18) | 0.3827 (4) | 0.35975 (18) | 0.0692 (17) | |
H35 | 0.0724 | 0.4630 | 0.3844 | 0.083* | |
C36 | 0.00648 (16) | 0.3642 (6) | 0.3344 (2) | 0.098 (3) | |
H36 | −0.0229 | 0.4321 | 0.3421 | 0.118* | |
C37 | −0.00669 (16) | 0.2442 (7) | 0.2976 (2) | 0.112 (3) | |
H37 | −0.0449 | 0.2318 | 0.2807 | 0.134* | |
C38 | 0.0373 (2) | 0.1428 (5) | 0.2861 (2) | 0.110 (3) | |
H38 | 0.0285 | 0.0625 | 0.2615 | 0.132* | |
C39 | 0.0944 (2) | 0.1614 (4) | 0.31145 (19) | 0.081 (2) | |
H39 | 0.1238 | 0.0935 | 0.3038 | 0.097* | |
C40 | 0.16695 (16) | 0.4012 (3) | 0.45167 (13) | 0.0417 (11) | |
C41 | 0.13200 (16) | 0.3307 (3) | 0.49323 (16) | 0.0573 (14) | |
H41 | 0.1171 | 0.2381 | 0.4846 | 0.069* | |
C42 | 0.11924 (18) | 0.3986 (5) | 0.54776 (15) | 0.0769 (19) | |
H42 | 0.0959 | 0.3514 | 0.5756 | 0.092* | |
C43 | 0.1414 (2) | 0.5370 (5) | 0.56073 (15) | 0.091 (2) | |
H43 | 0.1329 | 0.5824 | 0.5972 | 0.110* | |
C44 | 0.1764 (2) | 0.6075 (4) | 0.51916 (19) | 0.085 (2) | |
H44 | 0.1912 | 0.7001 | 0.5278 | 0.102* | |
C45 | 0.18914 (16) | 0.5396 (3) | 0.46463 (16) | 0.0554 (14) | |
H45 | 0.2125 | 0.5868 | 0.4368 | 0.066* | |
C46 | 0.21387 (15) | 0.1359 (3) | 0.39821 (14) | 0.0416 (11) | |
C47 | 0.22624 (17) | 0.0446 (4) | 0.34983 (12) | 0.0588 (15) | |
H47 | 0.2169 | 0.0738 | 0.3100 | 0.071* | |
C48 | 0.25250 (18) | −0.0904 (3) | 0.36103 (16) | 0.0685 (17) | |
H48 | 0.2608 | −0.1515 | 0.3287 | 0.082* | |
C49 | 0.26641 (16) | −0.1340 (3) | 0.4206 (2) | 0.0686 (18) | |
H49 | 0.2840 | −0.2243 | 0.4281 | 0.082* | |
C50 | 0.25405 (16) | −0.0427 (4) | 0.46898 (14) | 0.0599 (15) | |
H50 | 0.2633 | −0.0719 | 0.5088 | 0.072* | |
C51 | 0.22778 (16) | 0.0922 (3) | 0.45779 (13) | 0.0485 (13) | |
H51 | 0.2195 | 0.1533 | 0.4902 | 0.058* | |
O5 | 0.0180 (7) | 0.0325 (16) | 0.5073 (8) | 0.143 (5)* | 0.50 |
C52 | −0.0330 (11) | 0.033 (3) | 0.5424 (10) | 0.165 (10)* | 0.50 |
H52A | −0.0289 | −0.0314 | 0.5773 | 0.198* | 0.50 |
H52B | −0.0686 | 0.0083 | 0.5181 | 0.198* | 0.50 |
C53 | −0.0324 (14) | 0.190 (3) | 0.5609 (13) | 0.186 (11)* | 0.50 |
H53A | −0.0655 | 0.2095 | 0.5859 | 0.224* | 0.50 |
H53B | −0.0353 | 0.2507 | 0.5252 | 0.224* | 0.50 |
H53C | 0.0040 | 0.2115 | 0.5836 | 0.224* | 0.50 |
C54 | 0.0247 (11) | −0.115 (2) | 0.4895 (11) | 0.154 (9)* | 0.50 |
H54A | −0.0133 | −0.1533 | 0.4742 | 0.185* | 0.50 |
H54B | 0.0381 | −0.1731 | 0.5244 | 0.185* | 0.50 |
C55 | 0.0689 (12) | −0.124 (3) | 0.4409 (12) | 0.174 (10)* | 0.50 |
H55A | 0.0735 | −0.2236 | 0.4288 | 0.209* | 0.50 |
H55B | 0.1064 | −0.0868 | 0.4564 | 0.209* | 0.50 |
H55C | 0.0552 | −0.0671 | 0.4064 | 0.209* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt | 0.03140 (10) | 0.03758 (9) | 0.02984 (10) | 0.00111 (8) | 0.00179 (7) | 0.00230 (8) |
Re | 0.04179 (12) | 0.04866 (12) | 0.02939 (10) | 0.00440 (9) | −0.00239 (8) | 0.00195 (8) |
C11 | 0.061 (4) | 0.092 (5) | 0.052 (4) | 0.001 (3) | −0.020 (3) | −0.013 (3) |
C12 | 0.079 (5) | 0.093 (4) | 0.030 (3) | −0.009 (4) | 0.001 (3) | −0.005 (3) |
C13 | 0.061 (4) | 0.085 (4) | 0.054 (4) | 0.005 (3) | −0.006 (3) | −0.027 (3) |
C14 | 0.101 (6) | 0.054 (3) | 0.057 (4) | −0.008 (4) | −0.015 (4) | −0.009 (3) |
C15 | 0.064 (4) | 0.097 (5) | 0.050 (4) | −0.020 (4) | −0.007 (3) | −0.004 (3) |
P1 | 0.0319 (6) | 0.0366 (6) | 0.0369 (7) | 0.0020 (5) | 0.0011 (5) | 0.0019 (5) |
P2 | 0.0382 (7) | 0.0398 (6) | 0.0333 (6) | −0.0039 (5) | 0.0024 (5) | 0.0007 (5) |
C1 | 0.039 (3) | 0.046 (3) | 0.031 (2) | 0.001 (2) | 0.003 (2) | 0.002 (2) |
C2 | 0.044 (3) | 0.050 (3) | 0.044 (3) | 0.000 (2) | 0.001 (2) | 0.009 (2) |
C3 | 0.042 (3) | 0.065 (3) | 0.046 (3) | 0.008 (3) | −0.003 (3) | 0.004 (3) |
O3 | 0.067 (3) | 0.097 (3) | 0.055 (3) | 0.024 (2) | 0.015 (2) | −0.004 (2) |
C4 | 0.081 (4) | 0.063 (4) | 0.031 (3) | 0.016 (3) | −0.002 (3) | 0.002 (3) |
O4 | 0.175 (5) | 0.048 (2) | 0.063 (3) | 0.010 (3) | 0.000 (3) | 0.005 (2) |
C5 | 0.049 (3) | 0.047 (3) | 0.038 (3) | −0.013 (2) | 0.005 (2) | −0.004 (2) |
C6 | 0.056 (4) | 0.071 (4) | 0.047 (3) | −0.018 (3) | 0.007 (3) | −0.005 (3) |
C7 | 0.065 (4) | 0.086 (5) | 0.066 (4) | −0.029 (4) | 0.026 (3) | −0.010 (4) |
C8 | 0.099 (6) | 0.074 (4) | 0.054 (4) | −0.039 (4) | 0.021 (4) | 0.001 (3) |
C9 | 0.082 (5) | 0.070 (4) | 0.048 (3) | −0.015 (3) | 0.004 (3) | 0.013 (3) |
C10 | 0.057 (4) | 0.061 (3) | 0.046 (3) | −0.007 (3) | 0.004 (3) | 0.010 (3) |
C16 | 0.040 (3) | 0.041 (3) | 0.044 (3) | −0.003 (2) | 0.004 (2) | −0.004 (2) |
C17 | 0.042 (3) | 0.055 (3) | 0.053 (3) | −0.005 (2) | −0.003 (3) | 0.003 (3) |
C18 | 0.043 (3) | 0.070 (4) | 0.061 (4) | −0.011 (3) | −0.002 (3) | −0.006 (3) |
C19 | 0.066 (4) | 0.062 (4) | 0.074 (4) | −0.022 (3) | 0.010 (3) | −0.019 (3) |
C20 | 0.080 (5) | 0.038 (3) | 0.078 (4) | −0.005 (3) | 0.000 (4) | −0.003 (3) |
C21 | 0.049 (3) | 0.041 (3) | 0.060 (3) | 0.005 (2) | 0.002 (3) | −0.004 (2) |
C22 | 0.037 (3) | 0.037 (2) | 0.040 (3) | −0.004 (2) | −0.004 (2) | 0.003 (2) |
C23 | 0.054 (3) | 0.047 (3) | 0.046 (3) | −0.004 (2) | −0.005 (3) | −0.002 (2) |
C24 | 0.074 (4) | 0.077 (4) | 0.042 (3) | −0.016 (3) | −0.004 (3) | 0.004 (3) |
C25 | 0.073 (4) | 0.077 (4) | 0.059 (4) | −0.013 (4) | −0.015 (3) | 0.032 (3) |
C26 | 0.064 (4) | 0.056 (3) | 0.086 (5) | 0.003 (3) | −0.009 (4) | 0.027 (3) |
C27 | 0.051 (3) | 0.047 (3) | 0.057 (3) | 0.003 (2) | 0.004 (3) | 0.011 (3) |
C28 | 0.040 (3) | 0.043 (3) | 0.039 (3) | 0.009 (2) | 0.003 (2) | 0.005 (2) |
C29 | 0.047 (3) | 0.097 (5) | 0.054 (4) | 0.010 (3) | 0.009 (3) | −0.006 (3) |
C30 | 0.062 (4) | 0.134 (6) | 0.062 (4) | 0.028 (4) | 0.017 (3) | −0.007 (4) |
C31 | 0.097 (6) | 0.096 (5) | 0.059 (4) | 0.035 (4) | 0.021 (4) | −0.010 (4) |
C32 | 0.095 (6) | 0.083 (5) | 0.078 (5) | −0.003 (4) | 0.009 (4) | −0.032 (4) |
C33 | 0.058 (4) | 0.066 (4) | 0.076 (4) | −0.002 (3) | 0.017 (3) | −0.029 (3) |
C34 | 0.046 (3) | 0.058 (3) | 0.037 (3) | −0.014 (3) | 0.002 (2) | 0.009 (2) |
C35 | 0.040 (3) | 0.098 (5) | 0.070 (4) | −0.004 (3) | −0.001 (3) | 0.007 (4) |
C36 | 0.046 (4) | 0.145 (8) | 0.102 (6) | −0.003 (4) | −0.007 (4) | 0.032 (6) |
C37 | 0.063 (5) | 0.171 (9) | 0.099 (6) | −0.053 (6) | −0.025 (5) | 0.040 (6) |
C38 | 0.095 (6) | 0.142 (8) | 0.091 (6) | −0.057 (6) | −0.022 (5) | −0.006 (5) |
C39 | 0.074 (5) | 0.092 (5) | 0.075 (5) | −0.031 (4) | −0.011 (4) | −0.010 (4) |
C40 | 0.042 (3) | 0.047 (3) | 0.036 (3) | −0.001 (2) | 0.004 (2) | −0.001 (2) |
C41 | 0.065 (4) | 0.060 (3) | 0.048 (3) | 0.001 (3) | 0.017 (3) | 0.005 (3) |
C42 | 0.077 (5) | 0.106 (5) | 0.050 (4) | 0.011 (4) | 0.023 (3) | 0.007 (4) |
C43 | 0.088 (6) | 0.124 (7) | 0.061 (4) | 0.000 (5) | 0.005 (4) | −0.042 (4) |
C44 | 0.081 (5) | 0.095 (5) | 0.080 (5) | −0.015 (4) | 0.017 (4) | −0.046 (4) |
C45 | 0.055 (3) | 0.057 (3) | 0.054 (3) | −0.004 (3) | 0.004 (3) | −0.013 (3) |
C46 | 0.044 (3) | 0.038 (3) | 0.043 (3) | −0.009 (2) | 0.001 (2) | 0.003 (2) |
C47 | 0.066 (4) | 0.054 (3) | 0.057 (4) | −0.002 (3) | 0.006 (3) | −0.006 (3) |
C48 | 0.076 (5) | 0.049 (3) | 0.081 (5) | 0.003 (3) | 0.007 (4) | −0.012 (3) |
C49 | 0.064 (4) | 0.043 (3) | 0.101 (5) | 0.003 (3) | 0.019 (4) | 0.014 (3) |
C50 | 0.055 (4) | 0.059 (3) | 0.067 (4) | 0.001 (3) | 0.014 (3) | 0.026 (3) |
C51 | 0.053 (3) | 0.047 (3) | 0.046 (3) | −0.004 (2) | 0.008 (3) | 0.010 (2) |
Pt—C1 | 2.008 (4) | C29—H29 | 0.9300 |
Pt—P1 | 2.2717 (12) | C30—C31 | 1.3900 |
Pt—P2 | 2.3753 (12) | C30—H30 | 0.9300 |
Pt—Re | 2.7360 (3) | C31—C32 | 1.3900 |
Re—C4 | 1.883 (6) | C31—H31 | 0.9300 |
Re—C3 | 1.905 (6) | C32—C33 | 1.3900 |
Re—C1 | 2.083 (5) | C32—H32 | 0.9300 |
Re—C11 | 2.278 (6) | C33—H33 | 0.9300 |
Re—C12 | 2.294 (5) | C34—C35 | 1.3900 |
Re—C15 | 2.305 (6) | C34—C39 | 1.3900 |
Re—C13 | 2.322 (6) | C35—C36 | 1.3900 |
Re—C14 | 2.327 (6) | C35—H35 | 0.9300 |
C11—C12 | 1.382 (8) | C36—C37 | 1.3900 |
C11—C15 | 1.424 (9) | C36—H36 | 0.9300 |
C11—H11 | 0.9300 | C37—C38 | 1.3900 |
C12—C13 | 1.411 (9) | C37—H37 | 0.9300 |
C12—H12 | 0.9300 | C38—C39 | 1.3900 |
C13—C14 | 1.391 (9) | C38—H38 | 0.9300 |
C13—H13 | 0.9300 | C39—H39 | 0.9300 |
C14—C15 | 1.398 (9) | C40—C41 | 1.3900 |
C14—H14 | 0.9300 | C40—C45 | 1.3900 |
C15—H15 | 0.9300 | C41—C42 | 1.3900 |
P1—C22 | 1.841 (3) | C41—H41 | 0.9300 |
P1—C28 | 1.850 (3) | C42—C43 | 1.3900 |
P1—C16 | 1.866 (3) | C42—H42 | 0.9300 |
P2—C40 | 1.827 (3) | C43—C44 | 1.3900 |
P2—C46 | 1.849 (3) | C43—H43 | 0.9300 |
P2—C34 | 1.865 (3) | C44—C45 | 1.3900 |
C1—C2 | 1.351 (6) | C44—H44 | 0.9300 |
C2—C5 | 1.497 (5) | C45—H45 | 0.9300 |
C2—H2 | 0.9300 | C46—C47 | 1.3900 |
C3—O3 | 1.163 (6) | C46—C51 | 1.3900 |
C4—O4 | 1.171 (6) | C47—C48 | 1.3900 |
C5—C6 | 1.3900 | C47—H47 | 0.9300 |
C5—C10 | 1.3900 | C48—C49 | 1.3900 |
C6—C7 | 1.3900 | C48—H48 | 0.9300 |
C6—H6 | 0.9300 | C49—C50 | 1.3900 |
C7—C8 | 1.3900 | C49—H49 | 0.9300 |
C7—H7 | 0.9300 | C50—C51 | 1.3900 |
C8—C9 | 1.3900 | C50—H50 | 0.9300 |
C8—H8 | 0.9300 | C51—H51 | 0.9300 |
C9—C10 | 1.3900 | O5—O5i | 1.05 (3) |
C9—H9 | 0.9300 | O5—C54i | 1.23 (3) |
C10—H10 | 0.9300 | O5—C52i | 1.30 (3) |
C16—C17 | 1.3900 | O5—C52 | 1.409 (10) |
C16—C21 | 1.3900 | O5—C54 | 1.420 (10) |
C17—C18 | 1.3900 | C52—C54i | 1.05 (3) |
C17—H17 | 0.9300 | C52—C55i | 1.23 (3) |
C18—C19 | 1.3900 | C52—O5i | 1.30 (3) |
C18—H18 | 0.9300 | C52—C53 | 1.498 (10) |
C19—C20 | 1.3900 | C52—H52A | 0.97 (3) |
C19—H19 | 0.9300 | C52—H52B | 0.97 (3) |
C20—C21 | 1.3900 | C53—C55i | 1.02 (3) |
C20—H20 | 0.9300 | C53—C54i | 1.32 (3) |
C21—H21 | 0.9300 | C53—H53A | 0.96 (3) |
C22—C23 | 1.3900 | C53—H53B | 0.96 (3) |
C22—C27 | 1.3900 | C53—H53C | 0.96 (3) |
C23—C24 | 1.3900 | C54—C52i | 1.05 (3) |
C23—H23 | 0.9300 | C54—O5i | 1.23 (3) |
C24—C25 | 1.3900 | C54—C53i | 1.32 (3) |
C24—H24 | 0.9300 | C54—C55 | 1.491 (10) |
C25—C26 | 1.3900 | C54—H54A | 0.97 (3) |
C25—H25 | 0.9300 | C54—H54B | 0.97 (2) |
C26—C27 | 1.3900 | C55—C53i | 1.02 (3) |
C26—H26 | 0.9300 | C55—C52i | 1.23 (3) |
C27—H27 | 0.9300 | C55—H55A | 0.96 (3) |
C28—C29 | 1.3900 | C55—H55B | 0.96 (3) |
C28—C33 | 1.3900 | C55—H55C | 0.96 (3) |
C29—C30 | 1.3900 | ||
C1—Pt—P1 | 95.99 (14) | C26—C25—C24 | 120.0 |
C1—Pt—P2 | 158.97 (14) | C26—C25—H25 | 120.0 |
P1—Pt—P2 | 102.99 (4) | C24—C25—H25 | 120.0 |
C1—Pt—Re | 49.21 (14) | C25—C26—C27 | 120.0 |
P1—Pt—Re | 144.89 (3) | C25—C26—H26 | 120.0 |
P2—Pt—Re | 110.78 (3) | C27—C26—H26 | 120.0 |
C4—Re—C3 | 81.2 (2) | C26—C27—C22 | 120.0 |
C4—Re—C1 | 87.6 (2) | C26—C27—H27 | 120.0 |
C3—Re—C1 | 104.0 (2) | C22—C27—H27 | 120.0 |
C4—Re—C11 | 103.0 (2) | C29—C28—C33 | 120.0 |
C3—Re—C11 | 111.8 (2) | C29—C28—P1 | 123.8 (2) |
C1—Re—C11 | 143.8 (2) | C33—C28—P1 | 116.2 (2) |
C4—Re—C12 | 99.4 (2) | C30—C29—C28 | 120.0 |
C3—Re—C12 | 146.6 (2) | C30—C29—H29 | 120.0 |
C1—Re—C12 | 109.4 (2) | C28—C29—H29 | 120.0 |
C11—Re—C12 | 35.2 (2) | C29—C30—C31 | 120.0 |
C4—Re—C15 | 135.1 (3) | C29—C30—H30 | 120.0 |
C3—Re—C15 | 96.8 (2) | C31—C30—H30 | 120.0 |
C1—Re—C15 | 135.2 (2) | C32—C31—C30 | 120.0 |
C11—Re—C15 | 36.2 (2) | C32—C31—H31 | 120.0 |
C12—Re—C15 | 59.2 (2) | C30—C31—H31 | 120.0 |
C4—Re—C13 | 126.6 (2) | C31—C32—C33 | 120.0 |
C3—Re—C13 | 151.2 (2) | C31—C32—H32 | 120.0 |
C1—Re—C13 | 86.5 (2) | C33—C32—H32 | 120.0 |
C11—Re—C13 | 59.2 (2) | C32—C33—C28 | 120.0 |
C12—Re—C13 | 35.6 (2) | C32—C33—H33 | 120.0 |
C15—Re—C13 | 59.1 (2) | C28—C33—H33 | 120.0 |
C4—Re—C14 | 157.6 (2) | C35—C34—C39 | 120.0 |
C3—Re—C14 | 116.4 (2) | C35—C34—P2 | 118.0 (2) |
C1—Re—C14 | 100.4 (2) | C39—C34—P2 | 121.8 (2) |
C11—Re—C14 | 58.8 (2) | C34—C35—C36 | 120.0 |
C12—Re—C14 | 58.3 (2) | C34—C35—H35 | 120.0 |
C15—Re—C14 | 35.1 (2) | C36—C35—H35 | 120.0 |
C13—Re—C14 | 34.8 (2) | C37—C36—C35 | 120.0 |
C4—Re—Pt | 111.49 (16) | C37—C36—H36 | 120.0 |
C3—Re—Pt | 69.14 (15) | C35—C36—H36 | 120.0 |
C1—Re—Pt | 46.87 (12) | C36—C37—C38 | 120.0 |
C11—Re—Pt | 145.02 (18) | C36—C37—H37 | 120.0 |
C12—Re—Pt | 137.67 (18) | C38—C37—H37 | 120.0 |
C15—Re—Pt | 109.39 (17) | C39—C38—C37 | 120.0 |
C13—Re—Pt | 102.23 (17) | C39—C38—H38 | 120.0 |
C14—Re—Pt | 88.66 (16) | C37—C38—H38 | 120.0 |
C12—C11—C15 | 108.1 (6) | C38—C39—C34 | 120.0 |
C12—C11—Re | 73.0 (3) | C38—C39—H39 | 120.0 |
C15—C11—Re | 72.9 (3) | C34—C39—H39 | 120.0 |
C12—C11—H11 | 126.0 | C41—C40—C45 | 120.0 |
C15—C11—H11 | 126.0 | C41—C40—P2 | 122.15 (19) |
Re—C11—H11 | 119.9 | C45—C40—P2 | 117.85 (19) |
C11—C12—C13 | 108.8 (6) | C42—C41—C40 | 120.0 |
C11—C12—Re | 71.8 (3) | C42—C41—H41 | 120.0 |
C13—C12—Re | 73.3 (3) | C40—C41—H41 | 120.0 |
C11—C12—H12 | 125.6 | C41—C42—C43 | 120.0 |
C13—C12—H12 | 125.6 | C41—C42—H42 | 120.0 |
Re—C12—H12 | 121.1 | C43—C42—H42 | 120.0 |
C14—C13—C12 | 106.9 (6) | C44—C43—C42 | 120.0 |
C14—C13—Re | 72.8 (3) | C44—C43—H43 | 120.0 |
C12—C13—Re | 71.1 (3) | C42—C43—H43 | 120.0 |
C14—C13—H13 | 126.6 | C43—C44—C45 | 120.0 |
C12—C13—H13 | 126.6 | C43—C44—H44 | 120.0 |
Re—C13—H13 | 121.3 | C45—C44—H44 | 120.0 |
C13—C14—C15 | 109.6 (6) | C44—C45—C40 | 120.0 |
C13—C14—Re | 72.4 (3) | C44—C45—H45 | 120.0 |
C15—C14—Re | 71.6 (4) | C40—C45—H45 | 120.0 |
C13—C14—H14 | 125.2 | C47—C46—C51 | 120.0 |
C15—C14—H14 | 125.2 | C47—C46—P2 | 116.98 (19) |
Re—C14—H14 | 122.5 | C51—C46—P2 | 122.84 (19) |
C14—C15—C11 | 106.5 (6) | C46—C47—C48 | 120.0 |
C14—C15—Re | 73.3 (4) | C46—C47—H47 | 120.0 |
C11—C15—Re | 70.9 (3) | C48—C47—H47 | 120.0 |
C14—C15—H15 | 126.7 | C49—C48—C47 | 120.0 |
C11—C15—H15 | 126.7 | C49—C48—H48 | 120.0 |
Re—C15—H15 | 120.9 | C47—C48—H48 | 120.0 |
C22—P1—C28 | 104.41 (16) | C50—C49—C48 | 120.0 |
C22—P1—C16 | 97.46 (15) | C50—C49—H49 | 120.0 |
C28—P1—C16 | 105.92 (16) | C48—C49—H49 | 120.0 |
C22—P1—Pt | 121.31 (12) | C49—C50—C51 | 120.0 |
C28—P1—Pt | 108.92 (12) | C49—C50—H50 | 120.0 |
C16—P1—Pt | 117.11 (11) | C51—C50—H50 | 120.0 |
C40—P2—C46 | 105.26 (16) | C50—C51—C46 | 120.0 |
C40—P2—C34 | 99.07 (17) | C50—C51—H51 | 120.0 |
C46—P2—C34 | 103.43 (17) | C46—C51—H51 | 120.0 |
C40—P2—Pt | 118.61 (11) | O5i—O5—C54i | 76.8 (16) |
C46—P2—Pt | 111.27 (12) | O5i—O5—C52i | 72.8 (14) |
C34—P2—Pt | 117.32 (13) | C54i—O5—C52i | 124 (2) |
C2—C1—Pt | 133.5 (4) | O5i—O5—C52 | 62.1 (16) |
C2—C1—Re | 141.6 (4) | C54i—O5—C52 | 46.2 (14) |
Pt—C1—Re | 83.92 (17) | C52i—O5—C52 | 134.8 (13) |
C1—C2—C5 | 132.0 (4) | O5i—O5—C54 | 57.4 (15) |
C1—C2—H2 | 114.0 | C54i—O5—C54 | 134.2 (13) |
C5—C2—H2 | 114.0 | C52i—O5—C54 | 45.0 (13) |
O3—C3—Re | 171.5 (5) | C52—O5—C54 | 104.7 (15) |
O4—C4—Re | 177.6 (6) | C54i—C52—O5i | 73.4 (16) |
C6—C5—C10 | 120.0 | C55i—C52—O5i | 140 (3) |
C6—C5—C2 | 116.2 (3) | C55i—C52—O5 | 137 (3) |
C10—C5—C2 | 123.7 (3) | O5i—C52—C53 | 132 (2) |
C5—C6—C7 | 120.0 | O5—C52—C53 | 99 (2) |
C5—C6—H6 | 120.0 | C54i—C52—H52A | 162 (3) |
C7—C6—H6 | 120.0 | C55i—C52—H52A | 103 (2) |
C8—C7—C6 | 120.0 | O5i—C52—H52A | 111 (2) |
C8—C7—H7 | 120.0 | O5—C52—H52A | 112 (2) |
C6—C7—H7 | 120.0 | C53—C52—H52A | 112 (2) |
C9—C8—C7 | 120.0 | C54i—C52—H52B | 88 (3) |
C9—C8—H8 | 120.0 | C55i—C52—H52B | 78 (2) |
C7—C8—H8 | 120.0 | O5i—C52—H52B | 70.8 (15) |
C8—C9—C10 | 120.0 | O5—C52—H52B | 112.0 (19) |
C8—C9—H9 | 120.0 | C53—C52—H52B | 112 (2) |
C10—C9—H9 | 120.0 | H52A—C52—H52B | 110 (2) |
C9—C10—C5 | 120.0 | C54i—C53—H53A | 135 (3) |
C9—C10—H10 | 120.0 | C52—C53—H53A | 109 (2) |
C5—C10—H10 | 120.0 | C55i—C53—H53B | 107 (3) |
C17—C16—C21 | 120.0 | C52—C53—H53B | 109 (2) |
C17—C16—P1 | 120.38 (18) | H53A—C53—H53B | 109 (3) |
C21—C16—P1 | 119.60 (18) | C55i—C53—H53C | 144 (4) |
C16—C17—C18 | 120.0 | C54i—C53—H53C | 114 (3) |
C16—C17—H17 | 120.0 | C52—C53—H53C | 109 (3) |
C18—C17—H17 | 120.0 | H53A—C53—H53C | 109 (3) |
C17—C18—C19 | 120.0 | H53B—C53—H53C | 109 (3) |
C17—C18—H18 | 120.0 | O5i—C54—C53i | 120 (3) |
C19—C18—H18 | 120.0 | C53i—C54—O5 | 138 (2) |
C20—C19—C18 | 120.0 | O5i—C54—C55 | 129 (2) |
C20—C19—H19 | 120.0 | O5—C54—C55 | 109 (2) |
C18—C19—H19 | 120.0 | C52i—C54—H54A | 102 (3) |
C19—C20—C21 | 120.0 | O5—C54—H54A | 109.8 (17) |
C19—C20—H20 | 120.0 | C55—C54—H54A | 110 (2) |
C21—C20—H20 | 120.0 | O5i—C54—H54B | 121 (2) |
C20—C21—C16 | 120.0 | C53i—C54—H54B | 109.0 (18) |
C20—C21—H21 | 120.0 | O5—C54—H54B | 109.8 (19) |
C16—C21—H21 | 120.0 | C55—C54—H54B | 110 (2) |
C23—C22—C27 | 120.0 | H54A—C54—H54B | 108 (2) |
C23—C22—P1 | 116.39 (19) | C54—C55—H55A | 109 (2) |
C27—C22—P1 | 123.46 (19) | C52i—C55—H55B | 104 (3) |
C24—C23—C22 | 120.0 | C54—C55—H55B | 109 (3) |
C24—C23—H23 | 120.0 | H55A—C55—H55B | 109 (3) |
C22—C23—H23 | 120.0 | C54—C55—H55C | 109 (2) |
C25—C24—C23 | 120.0 | H55A—C55—H55C | 109 (3) |
C25—C24—H24 | 120.0 | H55B—C55—H55C | 109 (3) |
C23—C24—H24 | 120.0 |
Symmetry code: (i) −x, −y, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [PtRe(C5H5)(C8H6)(C18H15P)2(CO)2]·0.5C4H10O |
Mr | 1166.13 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 296 |
a, b, c (Å) | 22.529 (1), 9.1786 (5), 21.941 (1) |
β (°) | 92.469 (1) |
V (Å3) | 4532.9 (4) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 5.86 |
Crystal size (mm) | 0.36 × 0.21 × 0.18 |
Data collection | |
Diffractometer | Bruker SMART 4K CCD area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2004) |
Tmin, Tmax | 0.278, 0.418 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 38759, 10402, 7336 |
Rint | 0.038 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.031, 0.073, 1.00 |
No. of reflections | 10402 |
No. of parameters | 453 |
No. of restraints | 4 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 3.11, −1.48 |
Computer programs: SMART (Bruker, 2001), SMART, SAINT (Bruker, 2001), SHELXTL (Sheldrick, 2004), SHELXTL.
The molecule of the title compound, [η5-C5H5)(CO)2RePt (µ-C?CHPh)(PPh3)2] Et2O, is the dinuclear complex containing the Re and Pt atoms bridged by the µ-phenylvinylidene ligand. The phenyl ring and the C?C bond of vinylidene coupled with the Re—Pt-µ-C triangle form an almost planar system. Corresponding geometry was found for the analogous MnPt complex (Vasiliev et al., 2007). The structures of some µ-carbene (Casey et al., 1992; Bergamo et al., 2000) and µ-carbyne (Bergamo et al., 2000) complexes containing the Re—Pt-µ-C triangle system as the central fragment of molecule were reported.