Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270101007399/jz1465sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270101007399/jz1465Isup2.hkl |
CCDC reference: 169930
The salts Pt(COD)(CF3SO3)2 and NEt4[Re2(µ-PCy2)(CO)8] were reacted in dichloromethane solution in the presence of (CO)g (removal of the COD-ligand) at 258 K. The only separable product (thin-layer chromatography, eluant dichloromethane/n-hexane 1/5) was the title compound. Crystals were grown from chloroform/n-pentane, although very few were of acceptable quality and scattering power.
The U values of the carbon atoms were restrained such that anisotropic components along common bonds were approximately equal (command DELU $C). The largest peak of residual electron density is close to a heavy atoms, 0.9 Å from Re3.
Data collection: XSCANS (Siemens, 1995a); cell refinement: XSCANS; data reduction: SHELXTL (Siemens, 1995b); 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.
[PtRe4(CO)18(C12H22P)2] | F(000) = 3392 |
Mr = 1838.60 | Dx = 2.445 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 17.561 (2) Å | Cell parameters from 21 reflections |
b = 16.728 (3) Å | θ = 7.5–13.2° |
c = 17.408 (6) Å | µ = 12.58 mm−1 |
β = 102.42 (2)° | T = 203 K |
V = 4994 (2) Å3 | Needle, red |
Z = 4 | 0.40 × 0.05 × 0.04 mm |
Bruker P4 diffractometer | 4254 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.059 |
Graphite monochromator | θmax = 26.5°, θmin = 2.4° |
ω scans | h = −22→21 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→21 |
Tmin = 0.264, Tmax = 0.532 | l = 0→21 |
10719 measured reflections | 3 standard reflections every 397 reflections |
10342 independent reflections | intensity decay: 1% |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.059 | H-atom parameters constrained |
wR(F2) = 0.170 | w = 1/[σ2(Fo2) + (0.0419P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.97 | (Δ/σ)max = 0.001 |
10342 reflections | Δρmax = 1.33 e Å−3 |
605 parameters | Δρmin = −1.09 e Å−3 |
984 restraints | Extinction correction: SHELXL, none |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: none |
[PtRe4(CO)18(C12H22P)2] | V = 4994 (2) Å3 |
Mr = 1838.60 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 17.561 (2) Å | µ = 12.58 mm−1 |
b = 16.728 (3) Å | T = 203 K |
c = 17.408 (6) Å | 0.40 × 0.05 × 0.04 mm |
β = 102.42 (2)° |
Bruker P4 diffractometer | 4254 reflections with I > 2σ(I) |
Absorption correction: ψ scan (North et al., 1968) | Rint = 0.059 |
Tmin = 0.264, Tmax = 0.532 | 3 standard reflections every 397 reflections |
10719 measured reflections | intensity decay: 1% |
10342 independent reflections |
R[F2 > 2σ(F2)] = 0.059 | 984 restraints |
wR(F2) = 0.170 | H-atom parameters constrained |
S = 0.97 | Δρmax = 1.33 e Å−3 |
10342 reflections | Δρmin = −1.09 e Å−3 |
605 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. Max./min. residual electron density in the very close vicinity of heavy atoms. |
x | y | z | Uiso*/Ueq | ||
Pt1 | −0.13666 (5) | 0.77198 (6) | 0.61435 (6) | 0.0344 (2) | |
Re1 | 0.02254 (5) | 0.73598 (6) | 0.60120 (5) | 0.0306 (2) | |
Re2 | −0.02303 (5) | 0.82922 (6) | 0.74965 (6) | 0.0302 (2) | |
Re3 | −0.28918 (5) | 0.73284 (6) | 0.52740 (6) | 0.0304 (2) | |
Re4 | −0.38559 (5) | 0.61900 (6) | 0.40553 (6) | 0.0322 (2) | |
P1 | 0.1020 (3) | 0.7773 (4) | 0.7288 (3) | 0.0301 (12) | |
P2 | −0.4254 (3) | 0.7394 (4) | 0.4603 (4) | 0.0331 (13) | |
O1 | 0.0310 (9) | 0.8999 (10) | 0.5165 (10) | 0.046 (4) | |
C1 | 0.0275 (12) | 0.8417 (13) | 0.5502 (13) | 0.031 (4) | |
O2 | 0.0119 (12) | 0.5667 (11) | 0.6715 (12) | 0.072 (6) | |
C2 | 0.0148 (15) | 0.6298 (14) | 0.6479 (15) | 0.042 (5) | |
O3 | −0.0892 (8) | 0.6832 (10) | 0.4455 (10) | 0.049 (5) | |
C3 | −0.0494 (13) | 0.7047 (14) | 0.5034 (15) | 0.042 (5) | |
O4 | 0.1674 (9) | 0.6786 (11) | 0.5457 (11) | 0.056 (5) | |
C4 | 0.1154 (13) | 0.6997 (13) | 0.5659 (14) | 0.037 (5) | |
O5 | −0.0407 (9) | 0.6729 (10) | 0.8449 (10) | 0.050 (5) | |
C5 | −0.0331 (13) | 0.7258 (13) | 0.8079 (11) | 0.028 (4) | |
O6 | −0.0033 (10) | 0.9914 (10) | 0.6649 (10) | 0.050 (5) | |
C6 | −0.0099 (11) | 0.9306 (14) | 0.6953 (13) | 0.030 (4) | |
O7 | 0.0502 (9) | 0.9086 (10) | 0.9083 (9) | 0.046 (4) | |
C7 | 0.0239 (12) | 0.8794 (12) | 0.8495 (13) | 0.028 (4) | |
O8 | −0.1857 (8) | 0.8813 (11) | 0.7792 (11) | 0.050 (5) | |
C8 | −0.1267 (12) | 0.8617 (13) | 0.7653 (13) | 0.032 (4) | |
O9 | −0.1457 (10) | 0.9309 (11) | 0.5287 (11) | 0.058 (5) | |
C9 | −0.1396 (12) | 0.8708 (14) | 0.5585 (14) | 0.035 (4) | |
O10 | −0.1499 (10) | 0.6152 (12) | 0.7002 (11) | 0.063 (6) | |
C10 | −0.1473 (14) | 0.6742 (16) | 0.6695 (13) | 0.041 (5) | |
O11 | −0.2405 (9) | 0.8193 (10) | 0.3846 (10) | 0.049 (5) | |
C11 | −0.2576 (12) | 0.7886 (16) | 0.4388 (14) | 0.041 (5) | |
O12 | −0.1938 (10) | 0.5779 (11) | 0.5093 (12) | 0.062 (5) | |
C12 | −0.2325 (11) | 0.6343 (14) | 0.5079 (16) | 0.042 (5) | |
O13 | −0.3084 (9) | 0.8931 (10) | 0.6154 (11) | 0.049 (5) | |
C13 | −0.2979 (13) | 0.8360 (13) | 0.5828 (14) | 0.035 (4) | |
O14 | −0.3374 (9) | 0.6491 (9) | 0.6697 (9) | 0.039 (4) | |
C14 | −0.3197 (12) | 0.6777 (12) | 0.6159 (13) | 0.030 (4) | |
O15 | −0.2839 (10) | 0.4811 (11) | 0.3645 (11) | 0.057 (5) | |
C15 | −0.3215 (13) | 0.5306 (13) | 0.3795 (15) | 0.037 (5) | |
O16 | −0.3517 (11) | 0.7080 (10) | 0.2587 (11) | 0.058 (5) | |
C16 | −0.3632 (12) | 0.6754 (13) | 0.3126 (13) | 0.030 (4) | |
O17 | −0.4220 (9) | 0.5205 (10) | 0.5451 (10) | 0.044 (4) | |
C17 | −0.4093 (12) | 0.5591 (14) | 0.4939 (13) | 0.033 (4) | |
O18 | −0.5402 (9) | 0.5650 (12) | 0.3008 (11) | 0.056 (5) | |
C18 | −0.4804 (14) | 0.5857 (15) | 0.3400 (14) | 0.042 (5) | |
C21 | 0.1876 (12) | 0.8453 (12) | 0.7341 (10) | 0.039 (5) | |
H21 | 0.2344 | 0.8112 | 0.7502 | 0.047* | |
C22 | 0.1948 (12) | 0.8842 (13) | 0.6568 (11) | 0.045 (5) | |
H22A | 0.1931 | 0.8429 | 0.6165 | 0.054* | |
H22B | 0.1507 | 0.9205 | 0.6389 | 0.054* | |
C23 | 0.2709 (12) | 0.9307 (13) | 0.6670 (13) | 0.053 (6) | |
H23A | 0.2743 | 0.9556 | 0.6169 | 0.064* | |
H23B | 0.3149 | 0.8938 | 0.6821 | 0.064* | |
C24 | 0.2760 (13) | 0.9953 (11) | 0.7300 (11) | 0.044 (5) | |
H24A | 0.3264 | 1.0226 | 0.7375 | 0.053* | |
H24B | 0.2348 | 1.0350 | 0.7131 | 0.053* | |
C25 | 0.2670 (12) | 0.9573 (13) | 0.8074 (11) | 0.047 (5) | |
H25A | 0.3120 | 0.9228 | 0.8273 | 0.056* | |
H25B | 0.2665 | 0.9995 | 0.8463 | 0.056* | |
C26 | 0.1931 (11) | 0.9083 (12) | 0.7981 (11) | 0.040 (5) | |
H26A | 0.1478 | 0.9439 | 0.7850 | 0.049* | |
H26B | 0.1918 | 0.8821 | 0.8481 | 0.049* | |
C31 | 0.1413 (12) | 0.6920 (12) | 0.7931 (10) | 0.041 (5) | |
H31 | 0.0967 | 0.6558 | 0.7928 | 0.050* | |
C32 | 0.1717 (12) | 0.7169 (10) | 0.8798 (10) | 0.035 (4) | |
H32A | 0.1314 | 0.7476 | 0.8979 | 0.042* | |
H32B | 0.2176 | 0.7512 | 0.8839 | 0.042* | |
C33 | 0.1935 (12) | 0.6424 (12) | 0.9329 (11) | 0.049 (6) | |
H33A | 0.2144 | 0.6594 | 0.9872 | 0.059* | |
H33B | 0.1468 | 0.6102 | 0.9322 | 0.059* | |
C34 | 0.2550 (11) | 0.5912 (12) | 0.9037 (11) | 0.044 (5) | |
H34A | 0.3035 | 0.6218 | 0.9088 | 0.053* | |
H34B | 0.2665 | 0.5431 | 0.9363 | 0.053* | |
C35 | 0.2250 (14) | 0.5669 (11) | 0.8170 (11) | 0.048 (6) | |
H35A | 0.1789 | 0.5328 | 0.8127 | 0.058* | |
H35B | 0.2653 | 0.5360 | 0.7991 | 0.058* | |
C36 | 0.2037 (14) | 0.6411 (12) | 0.7639 (12) | 0.049 (6) | |
H36A | 0.1833 | 0.6241 | 0.7095 | 0.059* | |
H36B | 0.2505 | 0.6734 | 0.7651 | 0.059* | |
C41 | −0.4939 (9) | 0.7258 (12) | 0.5247 (11) | 0.033 (4) | |
H41 | −0.4698 | 0.6854 | 0.5640 | 0.040* | |
C42 | −0.5750 (10) | 0.6907 (13) | 0.4839 (11) | 0.038 (5) | |
H42A | −0.6056 | 0.7315 | 0.4504 | 0.045* | |
H42B | −0.5677 | 0.6454 | 0.4505 | 0.045* | |
C43 | −0.6194 (12) | 0.6627 (13) | 0.5473 (13) | 0.050 (6) | |
H43A | −0.6701 | 0.6406 | 0.5216 | 0.060* | |
H43B | −0.5896 | 0.6204 | 0.5794 | 0.060* | |
C44 | −0.6316 (11) | 0.7336 (14) | 0.6009 (13) | 0.056 (6) | |
H44A | −0.6572 | 0.7144 | 0.6422 | 0.068* | |
H44B | −0.6654 | 0.7737 | 0.5697 | 0.068* | |
C45 | −0.5520 (11) | 0.7721 (15) | 0.6390 (12) | 0.053 (6) | |
H45A | −0.5194 | 0.7332 | 0.6733 | 0.063* | |
H45B | −0.5603 | 0.8182 | 0.6710 | 0.063* | |
C46 | −0.5104 (12) | 0.7994 (12) | 0.5730 (12) | 0.044 (5) | |
H46A | −0.5434 | 0.8376 | 0.5382 | 0.053* | |
H46B | −0.4612 | 0.8261 | 0.5964 | 0.053* | |
C51 | −0.4505 (9) | 0.8276 (10) | 0.3938 (13) | 0.036 (4) | |
H51 | −0.4180 | 0.8248 | 0.3539 | 0.043* | |
C52 | −0.4345 (12) | 0.9088 (9) | 0.4360 (12) | 0.043 (5) | |
H52A | −0.4635 | 0.9116 | 0.4782 | 0.051* | |
H52B | −0.3788 | 0.9129 | 0.4602 | 0.051* | |
C53 | −0.4582 (12) | 0.9797 (11) | 0.3796 (13) | 0.050 (6) | |
H53A | −0.4509 | 1.0297 | 0.4096 | 0.060* | |
H53B | −0.4243 | 0.9813 | 0.3416 | 0.060* | |
C54 | −0.5435 (11) | 0.9733 (11) | 0.3352 (14) | 0.050 (6) | |
H54A | −0.5559 | 1.0173 | 0.2974 | 0.060* | |
H54B | −0.5780 | 0.9773 | 0.3724 | 0.060* | |
C55 | −0.5565 (14) | 0.8926 (11) | 0.2914 (12) | 0.056 (6) | |
H55A | −0.6110 | 0.8884 | 0.2632 | 0.067* | |
H55B | −0.5235 | 0.8897 | 0.2528 | 0.067* | |
C56 | −0.5368 (10) | 0.8230 (11) | 0.3498 (13) | 0.046 (6) | |
H56A | −0.5463 | 0.7721 | 0.3215 | 0.055* | |
H56B | −0.5706 | 0.8253 | 0.3879 | 0.055* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt1 | 0.0285 (4) | 0.0394 (5) | 0.0349 (5) | −0.0035 (4) | 0.0060 (4) | −0.0022 (5) |
Re1 | 0.0304 (4) | 0.0338 (5) | 0.0276 (5) | −0.0027 (4) | 0.0067 (4) | −0.0015 (4) |
Re2 | 0.0311 (5) | 0.0312 (5) | 0.0292 (5) | 0.0004 (4) | 0.0084 (4) | −0.0009 (4) |
Re3 | 0.0281 (4) | 0.0322 (5) | 0.0305 (5) | −0.0018 (4) | 0.0054 (4) | 0.0001 (4) |
Re4 | 0.0313 (5) | 0.0335 (5) | 0.0323 (5) | −0.0007 (4) | 0.0078 (4) | −0.0024 (4) |
P1 | 0.033 (3) | 0.030 (3) | 0.029 (3) | 0.002 (2) | 0.011 (2) | 0.002 (3) |
P2 | 0.031 (3) | 0.037 (3) | 0.032 (3) | −0.001 (2) | 0.008 (2) | −0.001 (3) |
O1 | 0.054 (10) | 0.037 (8) | 0.049 (12) | 0.000 (8) | 0.015 (9) | 0.002 (7) |
C1 | 0.031 (9) | 0.034 (7) | 0.027 (9) | 0.007 (7) | 0.006 (8) | −0.003 (7) |
O2 | 0.101 (15) | 0.039 (9) | 0.067 (15) | −0.018 (11) | −0.007 (12) | 0.010 (9) |
C2 | 0.060 (13) | 0.025 (7) | 0.043 (13) | 0.003 (7) | 0.014 (10) | −0.011 (7) |
O3 | 0.032 (9) | 0.055 (11) | 0.056 (10) | −0.011 (8) | −0.001 (7) | −0.017 (10) |
C3 | 0.041 (10) | 0.041 (12) | 0.042 (9) | −0.005 (9) | 0.007 (6) | −0.011 (9) |
O4 | 0.038 (9) | 0.059 (12) | 0.078 (14) | −0.009 (8) | 0.026 (9) | −0.013 (11) |
C4 | 0.041 (8) | 0.031 (11) | 0.036 (11) | 0.013 (8) | 0.002 (8) | 0.003 (9) |
O5 | 0.054 (10) | 0.041 (9) | 0.058 (12) | 0.017 (8) | 0.017 (9) | 0.027 (8) |
C5 | 0.050 (11) | 0.031 (7) | 0.019 (8) | 0.001 (8) | 0.019 (7) | −0.007 (6) |
O6 | 0.063 (11) | 0.047 (9) | 0.047 (12) | −0.015 (9) | 0.028 (10) | 0.003 (8) |
C6 | 0.023 (9) | 0.038 (8) | 0.028 (10) | 0.003 (6) | 0.001 (8) | 0.005 (7) |
O7 | 0.059 (11) | 0.053 (11) | 0.025 (8) | −0.008 (9) | 0.005 (8) | −0.009 (8) |
C7 | 0.039 (10) | 0.016 (9) | 0.031 (8) | 0.008 (8) | 0.008 (7) | −0.002 (7) |
O8 | 0.023 (7) | 0.070 (12) | 0.060 (12) | 0.004 (8) | 0.012 (8) | 0.010 (10) |
C8 | 0.030 (7) | 0.037 (12) | 0.028 (10) | 0.000 (7) | 0.008 (7) | 0.005 (8) |
O9 | 0.056 (11) | 0.054 (10) | 0.065 (14) | −0.002 (9) | 0.014 (10) | 0.025 (9) |
C9 | 0.031 (9) | 0.044 (10) | 0.033 (10) | 0.001 (6) | 0.012 (8) | 0.005 (9) |
O10 | 0.053 (11) | 0.074 (12) | 0.063 (13) | −0.016 (10) | 0.012 (10) | 0.034 (10) |
C10 | 0.050 (10) | 0.058 (11) | 0.015 (11) | −0.020 (10) | 0.008 (7) | 0.007 (8) |
O11 | 0.043 (9) | 0.059 (12) | 0.054 (11) | −0.015 (9) | 0.030 (9) | 0.002 (9) |
C11 | 0.029 (9) | 0.066 (12) | 0.030 (8) | −0.009 (9) | 0.007 (6) | 0.003 (8) |
O12 | 0.052 (11) | 0.049 (10) | 0.087 (15) | 0.012 (8) | 0.020 (11) | 0.001 (11) |
C12 | 0.016 (7) | 0.038 (8) | 0.076 (16) | −0.009 (6) | 0.021 (7) | −0.017 (9) |
O13 | 0.031 (8) | 0.043 (9) | 0.072 (13) | 0.001 (8) | 0.010 (9) | −0.014 (8) |
C13 | 0.040 (8) | 0.026 (7) | 0.040 (12) | −0.006 (7) | 0.012 (9) | 0.001 (7) |
O14 | 0.052 (10) | 0.047 (10) | 0.022 (8) | 0.015 (8) | 0.014 (7) | 0.012 (7) |
C14 | 0.036 (9) | 0.023 (9) | 0.033 (7) | −0.005 (8) | 0.009 (6) | −0.003 (7) |
O15 | 0.055 (11) | 0.054 (11) | 0.069 (13) | 0.005 (8) | 0.026 (10) | −0.025 (10) |
C15 | 0.041 (10) | 0.022 (8) | 0.054 (14) | −0.006 (7) | 0.020 (10) | −0.001 (7) |
O16 | 0.088 (13) | 0.039 (10) | 0.046 (11) | −0.005 (10) | 0.014 (10) | 0.015 (8) |
C16 | 0.030 (10) | 0.027 (10) | 0.030 (7) | 0.002 (8) | 0.001 (7) | −0.003 (6) |
O17 | 0.046 (9) | 0.050 (11) | 0.039 (10) | −0.008 (8) | 0.015 (8) | 0.007 (8) |
C17 | 0.030 (11) | 0.040 (8) | 0.027 (9) | −0.011 (8) | 0.003 (8) | −0.006 (8) |
O18 | 0.032 (8) | 0.083 (14) | 0.052 (12) | −0.009 (9) | 0.005 (7) | −0.001 (11) |
C18 | 0.045 (8) | 0.050 (13) | 0.026 (11) | −0.007 (8) | −0.001 (8) | −0.004 (9) |
C21 | 0.029 (8) | 0.060 (12) | 0.031 (10) | −0.015 (8) | 0.013 (8) | −0.016 (8) |
C22 | 0.044 (12) | 0.052 (13) | 0.047 (11) | −0.018 (9) | 0.028 (10) | −0.012 (9) |
C23 | 0.049 (12) | 0.050 (13) | 0.076 (14) | −0.020 (10) | 0.045 (12) | −0.020 (11) |
C24 | 0.039 (11) | 0.035 (12) | 0.060 (13) | −0.014 (9) | 0.013 (11) | −0.010 (9) |
C25 | 0.044 (12) | 0.044 (13) | 0.042 (11) | −0.004 (9) | −0.012 (11) | −0.003 (10) |
C26 | 0.042 (11) | 0.038 (11) | 0.040 (11) | 0.000 (8) | 0.006 (10) | −0.004 (9) |
C31 | 0.051 (12) | 0.037 (10) | 0.034 (8) | 0.013 (7) | 0.005 (8) | −0.001 (8) |
C32 | 0.042 (11) | 0.022 (10) | 0.038 (8) | 0.004 (8) | 0.004 (9) | −0.002 (7) |
C33 | 0.040 (12) | 0.062 (14) | 0.045 (10) | 0.017 (11) | 0.009 (10) | 0.022 (10) |
C34 | 0.034 (11) | 0.035 (11) | 0.060 (11) | 0.001 (8) | 0.002 (10) | 0.010 (10) |
C35 | 0.053 (13) | 0.037 (12) | 0.052 (12) | 0.010 (9) | 0.006 (11) | 0.014 (9) |
C36 | 0.069 (14) | 0.035 (12) | 0.046 (11) | 0.018 (9) | 0.021 (11) | 0.003 (9) |
C41 | 0.032 (7) | 0.035 (10) | 0.034 (11) | −0.008 (8) | 0.010 (7) | −0.007 (8) |
C42 | 0.041 (9) | 0.038 (12) | 0.036 (12) | −0.009 (9) | 0.015 (8) | −0.004 (9) |
C43 | 0.041 (11) | 0.056 (14) | 0.063 (15) | −0.003 (10) | 0.032 (10) | 0.005 (10) |
C44 | 0.044 (11) | 0.080 (16) | 0.057 (14) | 0.000 (11) | 0.038 (10) | −0.001 (12) |
C45 | 0.046 (11) | 0.066 (15) | 0.055 (14) | 0.005 (11) | 0.030 (10) | −0.005 (11) |
C46 | 0.036 (11) | 0.046 (12) | 0.054 (14) | −0.007 (9) | 0.017 (9) | −0.013 (9) |
C51 | 0.020 (8) | 0.031 (6) | 0.052 (12) | −0.017 (7) | −0.002 (8) | 0.005 (7) |
C52 | 0.050 (12) | 0.028 (7) | 0.052 (14) | −0.021 (9) | 0.017 (9) | 0.010 (8) |
C53 | 0.064 (12) | 0.033 (9) | 0.050 (15) | 0.000 (11) | 0.004 (11) | 0.006 (10) |
C54 | 0.049 (11) | 0.044 (10) | 0.059 (15) | −0.009 (11) | 0.014 (10) | 0.007 (10) |
C55 | 0.061 (14) | 0.057 (13) | 0.044 (14) | 0.006 (11) | −0.005 (10) | −0.004 (9) |
C56 | 0.046 (10) | 0.047 (10) | 0.033 (12) | 0.007 (9) | −0.015 (9) | −0.013 (9) |
Pt1—C9 | 1.91 (2) | O7—C7 | 1.14 (2) |
Pt1—C10 | 1.93 (2) | O8—C8 | 1.16 (2) |
Pt1—Re3 | 2.8548 (13) | O9—C9 | 1.12 (3) |
Pt1—Re2 | 2.9025 (15) | O10—C10 | 1.13 (3) |
Pt1—Re1 | 2.9165 (12) | O11—C11 | 1.17 (3) |
Re1—Re2 | 3.2620 (15) | O12—C12 | 1.16 (3) |
Re1—C4 | 1.96 (2) | O13—C13 | 1.15 (3) |
Re1—C3 | 1.96 (2) | O14—C14 | 1.15 (2) |
Re1—C2 | 1.97 (2) | O15—C15 | 1.12 (2) |
Re1—C1 | 1.99 (2) | O16—C16 | 1.14 (3) |
Re1—P1 | 2.454 (6) | O17—C17 | 1.16 (3) |
Re2—C7 | 1.95 (2) | O18—C18 | 1.18 (3) |
Re2—C8 | 1.97 (2) | C21—C26 | 1.523 (15) |
Re2—C6 | 1.98 (2) | C21—C22 | 1.525 (15) |
Re2—C5 | 2.03 (2) | C22—C23 | 1.523 (15) |
Re2—P1 | 2.459 (6) | C23—C24 | 1.528 (15) |
Re3—C14 | 1.97 (2) | C24—C25 | 1.528 (15) |
Re3—C11 | 1.98 (2) | C25—C26 | 1.514 (15) |
Re3—C12 | 1.99 (2) | C31—C32 | 1.546 (15) |
Re3—C13 | 2.00 (2) | C31—C36 | 1.557 (15) |
Re3—P2 | 2.429 (6) | C32—C33 | 1.550 (15) |
Re3—Re4 | 3.0739 (15) | C33—C34 | 1.547 (15) |
Re4—C18 | 1.89 (2) | C34—C35 | 1.542 (15) |
Re4—C17 | 1.95 (2) | C35—C36 | 1.545 (15) |
Re4—C15 | 1.97 (2) | C41—C46 | 1.553 (15) |
Re4—C16 | 1.98 (2) | C41—C42 | 1.563 (15) |
Re4—P2 | 2.396 (6) | C42—C43 | 1.555 (15) |
P1—C31 | 1.853 (19) | C43—C44 | 1.552 (15) |
P1—C21 | 1.872 (18) | C44—C45 | 1.552 (15) |
P2—C41 | 1.825 (18) | C45—C46 | 1.558 (16) |
P2—C51 | 1.870 (19) | C51—C52 | 1.542 (15) |
O1—C1 | 1.14 (2) | C51—C56 | 1.546 (15) |
O2—C2 | 1.14 (3) | C52—C53 | 1.539 (15) |
O3—C3 | 1.15 (3) | C53—C54 | 1.534 (15) |
O4—C4 | 1.10 (2) | C54—C55 | 1.543 (16) |
O5—C5 | 1.12 (2) | C55—C56 | 1.535 (16) |
O6—C6 | 1.16 (2) | ||
C9—Pt1—C10 | 172.9 (10) | C17—Re4—C15 | 91.4 (10) |
C9—Pt1—Re3 | 90.5 (7) | C18—Re4—C16 | 87.2 (9) |
C10—Pt1—Re3 | 83.6 (7) | C17—Re4—C16 | 177.3 (9) |
C9—Pt1—Re2 | 93.8 (7) | C15—Re4—C16 | 86.9 (9) |
C10—Pt1—Re2 | 89.9 (7) | C18—Re4—P2 | 101.1 (8) |
Re3—Pt1—Re2 | 155.33 (4) | C17—Re4—P2 | 89.3 (7) |
C9—Pt1—Re1 | 93.4 (6) | C15—Re4—P2 | 162.3 (7) |
C10—Pt1—Re1 | 93.5 (7) | C16—Re4—P2 | 92.9 (6) |
Re3—Pt1—Re1 | 135.80 (4) | C18—Re4—Re3 | 152.0 (8) |
Re2—Pt1—Re1 | 68.19 (4) | C17—Re4—Re3 | 87.4 (6) |
C4—Re1—Re2 | 139.4 (7) | C15—Re4—Re3 | 111.5 (7) |
C3—Re1—Re2 | 126.4 (7) | C16—Re4—Re3 | 95.3 (6) |
C2—Re1—Re2 | 93.1 (7) | P2—Re4—Re3 | 50.89 (14) |
C1—Re1—Re2 | 88.3 (6) | C31—P1—C21 | 104.3 (10) |
P1—Re1—Re2 | 48.47 (13) | C31—P1—Re1 | 113.3 (7) |
Pt1—Re1—Re2 | 55.70 (3) | C21—P1—Re1 | 120.7 (6) |
C4—Re1—C3 | 94.0 (10) | C31—P1—Re2 | 114.3 (7) |
C4—Re1—C2 | 89.2 (10) | C21—P1—Re2 | 120.8 (7) |
C3—Re1—C2 | 91.7 (10) | Re1—P1—Re2 | 83.19 (18) |
C4—Re1—C1 | 90.9 (9) | C41—P2—C51 | 112.3 (10) |
C3—Re1—C1 | 86.0 (10) | C41—P2—Re4 | 115.3 (7) |
C2—Re1—C1 | 177.7 (10) | C51—P2—Re4 | 117.8 (7) |
C4—Re1—P1 | 91.2 (7) | C41—P2—Re3 | 114.2 (7) |
C3—Re1—P1 | 174.7 (7) | C51—P2—Re3 | 114.2 (5) |
C2—Re1—P1 | 87.5 (7) | Re4—P2—Re3 | 79.15 (18) |
C1—Re1—P1 | 94.8 (6) | O1—C1—Re1 | 176 (2) |
C4—Re1—Pt1 | 164.9 (7) | O2—C2—Re1 | 176 (2) |
C3—Re1—Pt1 | 70.9 (7) | O3—C3—Re1 | 177 (2) |
C2—Re1—Pt1 | 90.1 (7) | O4—C4—Re1 | 179 (2) |
C1—Re1—Pt1 | 89.2 (6) | O5—C5—Re2 | 173.9 (18) |
P1—Re1—Pt1 | 103.81 (14) | O6—C6—Re2 | 178 (2) |
C7—Re2—Re1 | 141.7 (6) | O7—C7—Re2 | 179 (2) |
C8—Re2—Re1 | 129.2 (7) | O8—C8—Re2 | 176 (2) |
C6—Re2—Re1 | 87.5 (7) | O9—C9—Pt1 | 175 (2) |
C5—Re2—Re1 | 92.9 (5) | O10—C10—Pt1 | 176 (2) |
P1—Re2—Re1 | 48.34 (14) | O11—C11—Re3 | 177 (2) |
Pt1—Re2—Re1 | 56.11 (3) | O12—C12—Re3 | 169 (2) |
C7—Re2—C8 | 89.1 (9) | O13—C13—Re3 | 175 (2) |
C7—Re2—C6 | 89.3 (9) | O14—C14—Re3 | 176.5 (19) |
C8—Re2—C6 | 92.1 (9) | O15—C15—Re4 | 179 (2) |
C7—Re2—C5 | 89.2 (8) | O16—C16—Re4 | 179 (2) |
C8—Re2—C5 | 89.0 (9) | O17—C17—Re4 | 177 (2) |
C6—Re2—C5 | 178.1 (9) | O18—C18—Re4 | 178 (2) |
C7—Re2—P1 | 93.7 (6) | C26—C21—C22 | 110.2 (14) |
C8—Re2—P1 | 175.2 (7) | C26—C21—P1 | 112.4 (12) |
C6—Re2—P1 | 91.8 (6) | C22—C21—P1 | 115.7 (12) |
C5—Re2—P1 | 87.1 (6) | C23—C22—C21 | 110.6 (14) |
C7—Re2—Pt1 | 162.2 (6) | C22—C23—C24 | 111.1 (14) |
C8—Re2—Pt1 | 73.1 (7) | C25—C24—C23 | 109.7 (14) |
C6—Re2—Pt1 | 91.4 (6) | C26—C25—C24 | 112.3 (13) |
C5—Re2—Pt1 | 90.3 (6) | C25—C26—C21 | 111.7 (13) |
P1—Re2—Pt1 | 104.08 (15) | C32—C31—C36 | 110.3 (14) |
C14—Re3—C11 | 179.5 (9) | C32—C31—P1 | 112.9 (12) |
C14—Re3—C12 | 88.6 (10) | C36—C31—P1 | 114.9 (13) |
C11—Re3—C12 | 91.3 (11) | C31—C32—C33 | 110.8 (13) |
C14—Re3—C13 | 88.0 (9) | C34—C33—C32 | 110.5 (13) |
C11—Re3—C13 | 91.8 (10) | C35—C34—C33 | 110.6 (13) |
C12—Re3—C13 | 152.9 (9) | C34—C35—C36 | 111.2 (14) |
C14—Re3—P2 | 89.5 (6) | C35—C36—C31 | 109.9 (14) |
C11—Re3—P2 | 91.0 (6) | C46—C41—C42 | 106.6 (13) |
C12—Re3—P2 | 115.6 (7) | C46—C41—P2 | 117.2 (12) |
C13—Re3—P2 | 91.3 (7) | C42—C41—P2 | 115.1 (12) |
C14—Re3—Pt1 | 94.3 (6) | C43—C42—C41 | 109.7 (13) |
C11—Re3—Pt1 | 85.2 (6) | C44—C43—C42 | 110.6 (14) |
C12—Re3—Pt1 | 80.5 (6) | C43—C44—C45 | 110.3 (14) |
C13—Re3—Pt1 | 73.0 (6) | C44—C45—C46 | 109.2 (14) |
P2—Re3—Pt1 | 163.66 (16) | C41—C46—C45 | 109.8 (14) |
C14—Re3—Re4 | 92.7 (6) | C52—C51—C56 | 109.8 (13) |
C11—Re3—Re4 | 87.7 (7) | C52—C51—P2 | 113.9 (13) |
C12—Re3—Re4 | 65.8 (7) | C56—C51—P2 | 110.0 (12) |
C13—Re3—Re4 | 141.2 (6) | C53—C52—C51 | 112.2 (14) |
P2—Re3—Re4 | 49.95 (15) | C54—C53—C52 | 111.6 (14) |
Pt1—Re3—Re4 | 145.35 (4) | C53—C54—C55 | 109.6 (14) |
C18—Re4—C17 | 90.8 (10) | C56—C55—C54 | 110.4 (14) |
C18—Re4—C15 | 96.5 (10) | C55—C56—C51 | 110.3 (14) |
Experimental details
Crystal data | |
Chemical formula | [PtRe4(CO)18(C12H22P)2] |
Mr | 1838.60 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 203 |
a, b, c (Å) | 17.561 (2), 16.728 (3), 17.408 (6) |
β (°) | 102.42 (2) |
V (Å3) | 4994 (2) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 12.58 |
Crystal size (mm) | 0.40 × 0.05 × 0.04 |
Data collection | |
Diffractometer | Bruker P4 diffractometer |
Absorption correction | ψ scan (North et al., 1968) |
Tmin, Tmax | 0.264, 0.532 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10719, 10342, 4254 |
Rint | 0.059 |
(sin θ/λ)max (Å−1) | 0.628 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.059, 0.170, 0.97 |
No. of reflections | 10342 |
No. of parameters | 605 |
No. of restraints | 984 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.33, −1.09 |
Computer programs: XSCANS (Siemens, 1995a), XSCANS, SHELXTL (Siemens, 1995b), SHELXTL.
Pt1—Re3 | 2.8548 (13) | Re2—P1 | 2.459 (6) |
Pt1—Re2 | 2.9025 (15) | Re3—P2 | 2.429 (6) |
Pt1—Re1 | 2.9165 (12) | Re3—Re4 | 3.0739 (15) |
Re1—Re2 | 3.2620 (15) | Re4—P2 | 2.396 (6) |
Re1—P1 | 2.454 (6) | ||
C9—Pt1—C10 | 172.9 (10) | Pt1—Re2—Re1 | 56.11 (3) |
Re3—Pt1—Re2 | 155.33 (4) | P1—Re2—Pt1 | 104.08 (15) |
Re3—Pt1—Re1 | 135.80 (4) | P2—Re3—Pt1 | 163.66 (16) |
Re2—Pt1—Re1 | 68.19 (4) | C12—Re3—Re4 | 65.8 (7) |
C3—Re1—Re2 | 126.4 (7) | P2—Re3—Re4 | 49.95 (15) |
P1—Re1—Re2 | 48.47 (13) | Pt1—Re3—Re4 | 145.35 (4) |
Pt1—Re1—Re2 | 55.70 (3) | C15—Re4—Re3 | 111.5 (7) |
P1—Re1—Pt1 | 103.81 (14) | P2—Re4—Re3 | 50.89 (14) |
C8—Re2—Re1 | 129.2 (7) | Re1—P1—Re2 | 83.19 (18) |
P1—Re2—Re1 | 48.34 (14) | Re4—P2—Re3 | 79.15 (18) |
As a continuation of our investigations into triangular cluster complexes M2Rh(µ-PR2)(µ-CO)2(CO)8 (M = Mn, Re; R = organic residue) as hydroformylation catalysts (Beckers et al., 1998; Haupt et al., 2001), we wished for selectivity reasons to exchange the rhodium(I) atom for a more nucleophilic platinum(II) atom as reaction centre. Platinum(II) carbonyl cluster complexes of this type are very rare (Braunstein et al., 1999).
The molecule [(µ-PCy2)(CO)8Re2]2Pt(CO)2, (I) (Fig. 1), consists of two phosphido-bridged dirhenium carbonyl moieties that are linked via the central platinum atom. The Pt(CO)2 constituent extends the original (µ-P1)Re2 core to a four-membered, nearly planar µ-PRe2Pt ring. The maximum deviation of an atom from this best plane is 0.082 (6) Å for P1; the PRe2/Re2Pt dihedral angle is 8.1°. Both Re atoms have a slightly distorted octahedral coordination from four terminal CO groups, the bridging P and the Pt atom. The CO ligands at both rhenium show an ecliptic arrangement with C—Re1—Re2—C torsion angles (here and in the following text as absolute values) from 0.4 to 3.7°. The CO groups attached to Pt are also in ecliptic position relative to those at Re1 and Re2, with torsion angles from 0.5 to 6.1°. The Re1—Re2 bond measures 3.2620 (15) Å and the µ-P1 bridge is symmetric with respect to the equal P—Re bond lengths of 2.454 (6) and 2.459 (6) Å. The two Pt—Re bonds differ slightly in length with 2.9165 (12) and 2.9025 (15) Å for Re1 and Re2, respectively, but they are longer than other unsupported Pt—Re bonds known from the literature. For these, the values reported range from 2.706 (1) to 2.899 (1) Å (Casey et al., 1987, 1992; Urbancic et al., 1984; Beringhelli et al., 1990, 1993; Mague & Lin, 1994). A µ-H bridged Pt—Re edge has been reported with 2.906 (1) Å (Beringhelli et al., 1990). \sch
A third but shorter Pt—Re3 bond of 2.8548 (13) Å connects the second (µ-P2)Re2(CO)8 unit to platinum. Again, the Re3—Re4 bond of 3.0739 (15) Å is bridged by a PCy2 ligand and both rhenium atoms are attached to four terminal CO groups. These groups show also an ecliptic arrangement along the Re—Re vector, with torsion angles in the range 3.7 to 7.7°. Neglecting the Re—Re bond, Re4 is coordinated by five non-metal atoms, thus realising a distorted square pyramidal coordination, whereas Re3 reaches a strongly distorted octahedral coordination with the additional Re—Pt interaction. The CO ligands at Re3 and those attached to Pt show staggered conformation along the Re3—Pt vector with torsion angles of C9—Pt—Re3—C13 58.8 (10)° and C10—Pt—Re3—C12 57.2 (10)°, realising a sterically favourable arrangement. In contrast to the symmetric µ-P1 bridge, the µ-P2 atom shows two different P—Re bond lengths of 2.429 (6) (Re3) and 2.396 (6) Å (Re4), the longer one being trans to the Re3–Pt bond. With respect to the different Re—Pt—Re angles in the basal Re3Pt plane of 68.19 (4), 135.80 (4) and 155.33 (4)° for Re1/2, Re1/3 and Re2/3, respectively, the fivefold coordination geometry around Pt can be described as pseudo-trigonal bipyramidal with the CO groups 9 and 10 at the apices. The Re3Pt plane is almost planar with a maximum deviation of 0.082 (2) Å for Pt from the best plane. A similar Y-shaped planar coordination pattern for the central metal atom with Y-angles in the range of 64, 138 and 158° is known from the coordination of e.g. Ir or Rh in (µ-PR2)(CO)8Re2[µ-M(CO)2PPh3] (M = Ir, Rh) (Haupt et al., 1994). The uncommon coordination geometry observed here for platinum, with the different bonding patterns of one bridging and one end-on linked (µ-PCy2)(CO)8Re2 unit, must be due to stereochemical reasons. Neither an alternative planar quadratic nor spirocyclic Re4Pt arrangement, both then with two bridging Re2 units, would be possible because of the steric repulsion of the CO groups 3, 8 and 12,15 or 9, 10 and 12,15.