Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270102005644/ta1365sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270102005644/ta1365Isup2.hkl |
CCDC reference: 187913
Tetra-n-butylammonium octachlorodirhenate(III) (508 mg, 0.445 mmol) was combined with 1-butyl-3-methylimidazolium hexafluorophosphate (7 ml) and ethanol (7 ml) in a round-bottomed flask under a nitrogen atmosphere. Two drops of concentrated hydrochloric acid were added followed by diethylphenylphosphine (1.00 g, 6.02 mmol). The mixture was stirred for 30 min at 298 K. Tetrahydrofuran (15 ml) was added and the mixture was stirred for 1 h. Diethyl ether (60 ml) was added next and the mixture was stirred for 2 h, then allowed to sit for 14 h. This resulted in two distinct liquid layers, i.e. a larger brown–green top layer and a small dark-brown bottom layer. The layers were separated in air using a separatory funnel and the top layer was placed in a large Schlenk flask. Dark crystals of the title compound formed as this solution was allowed to slowly evaporate.
H atoms were placed in calculated positions and refined as rifing with C—H distances in the range 0.94–0.98 Å, and Uiso values of 1.2Ueq of the parent atom or 1.5Ueq of the parent atom for methyl groups. The highest peak in the final difference map is located 1.03 Å from atom Re2.
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1996); software used to prepare material for publication: SHELXL97.
Fig. 1. The molecular structure of the title compound drawn with 50% displacement ellipsoids. H atoms have been omitted for clarity. |
[Re2Cl5(C10H15P)3] | Dx = 1.927 Mg m−3 |
Mr = 1048.22 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, Pbca | Cell parameters from 4402 reflections |
a = 15.5374 (7) Å | θ = 2.4–27.4° |
b = 20.7751 (9) Å | µ = 7.22 mm−1 |
c = 22.3924 (10) Å | T = 213 K |
V = 7228.1 (6) Å3 | Plate, red |
Z = 8 | 0.12 × 0.11 × 0.08 mm |
F(000) = 4040 |
Bruker SMART diffractometer | 8235 independent reflections |
Radiation source: normal-focus sealed tube | 5875 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.053 |
ω scans | θmax = 27.6°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Blessing, 1995) | h = −20→18 |
Tmin = 0.410, Tmax = 0.561 | k = −21→27 |
34336 measured reflections | l = −24→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: inferred from neighbouring sites |
wR(F2) = 0.048 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.01P)2] where P = (Fo2 + 2Fc2)/3 |
8235 reflections | (Δ/σ)max = 0.009 |
367 parameters | Δρmax = 1.64 e Å−3 |
0 restraints | Δρmin = −1.11 e Å−3 |
[Re2Cl5(C10H15P)3] | V = 7228.1 (6) Å3 |
Mr = 1048.22 | Z = 8 |
Orthorhombic, Pbca | Mo Kα radiation |
a = 15.5374 (7) Å | µ = 7.22 mm−1 |
b = 20.7751 (9) Å | T = 213 K |
c = 22.3924 (10) Å | 0.12 × 0.11 × 0.08 mm |
Bruker SMART diffractometer | 8235 independent reflections |
Absorption correction: multi-scan (SADABS; Blessing, 1995) | 5875 reflections with I > 2σ(I) |
Tmin = 0.410, Tmax = 0.561 | Rint = 0.053 |
34336 measured reflections |
R[F2 > 2σ(F2)] = 0.031 | 0 restraints |
wR(F2) = 0.048 | H-atom parameters constrained |
S = 1.01 | Δρmax = 1.64 e Å−3 |
8235 reflections | Δρmin = −1.11 e Å−3 |
367 parameters |
Experimental. Data were collected as 0.3deg omega-scans for three different positions of phi. The center of the detector was positioned 50 mm from the crystal at a 2-theta swing angle of -28deg, allowing the collection of a complete and highly redundant data set to at least 55deg 2-theta. Diffraction spots were integrated using an ellisoid-mask profile-fitting routine. |
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 | 0.060261 (12) | 0.164476 (10) | 0.309358 (8) | 0.02178 (5) | |
Re2 | 0.034854 (12) | 0.267171 (10) | 0.331621 (8) | 0.02161 (5) | |
Cl1 | 0.20442 (8) | 0.13431 (7) | 0.32603 (6) | 0.0332 (3) | |
Cl2 | −0.07278 (8) | 0.12664 (6) | 0.27447 (5) | 0.0314 (3) | |
Cl3 | −0.01176 (8) | 0.27246 (7) | 0.43046 (5) | 0.0332 (3) | |
Cl4 | −0.10976 (8) | 0.28271 (7) | 0.30502 (6) | 0.0378 (3) | |
Cl5 | 0.06926 (8) | 0.33197 (7) | 0.24935 (5) | 0.0322 (3) | |
P1 | 0.02328 (9) | 0.10440 (7) | 0.40104 (6) | 0.0274 (3) | |
P2 | 0.09768 (8) | 0.16714 (7) | 0.20299 (5) | 0.0255 (3) | |
P3 | 0.17498 (8) | 0.29998 (7) | 0.37212 (6) | 0.0259 (3) | |
C1 | 0.0810 (3) | 0.1164 (2) | 0.4717 (2) | 0.0269 (12) | |
C2 | 0.0414 (4) | 0.1425 (3) | 0.5208 (2) | 0.0368 (14) | |
H2A | −0.0161 | 0.1561 | 0.5180 | 0.044* | |
C3 | 0.0853 (4) | 0.1492 (3) | 0.5747 (2) | 0.0451 (16) | |
H3A | 0.0571 | 0.1665 | 0.6082 | 0.054* | |
C4 | 0.1698 (4) | 0.1305 (3) | 0.5786 (3) | 0.0471 (17) | |
H4A | 0.1999 | 0.1352 | 0.6148 | 0.056* | |
C5 | 0.2100 (4) | 0.1052 (3) | 0.5303 (2) | 0.0422 (15) | |
H5A | 0.2680 | 0.0927 | 0.5332 | 0.051* | |
C6 | 0.1669 (4) | 0.0974 (3) | 0.4770 (2) | 0.0369 (14) | |
H6A | 0.1954 | 0.0792 | 0.4440 | 0.044* | |
C7 | 0.0469 (4) | 0.0189 (2) | 0.3859 (2) | 0.0417 (15) | |
H7A | 0.1094 | 0.0145 | 0.3817 | 0.050* | |
H7B | 0.0300 | −0.0059 | 0.4212 | 0.050* | |
C8 | 0.0057 (4) | −0.0119 (3) | 0.3324 (3) | 0.0592 (19) | |
H8A | −0.0562 | −0.0064 | 0.3346 | 0.089* | |
H8B | 0.0195 | −0.0574 | 0.3318 | 0.089* | |
H8C | 0.0273 | 0.0083 | 0.2963 | 0.089* | |
C9 | −0.0907 (3) | 0.1078 (3) | 0.4198 (2) | 0.0347 (14) | |
H9A | −0.1026 | 0.1502 | 0.4370 | 0.042* | |
H9B | −0.1237 | 0.1045 | 0.3826 | 0.042* | |
C10 | −0.1245 (4) | 0.0569 (3) | 0.4629 (2) | 0.0534 (18) | |
H10A | −0.1101 | 0.0144 | 0.4480 | 0.080* | |
H10B | −0.1865 | 0.0609 | 0.4663 | 0.080* | |
H10C | −0.0983 | 0.0631 | 0.5018 | 0.080* | |
C11 | 0.1188 (3) | 0.0832 (3) | 0.1850 (2) | 0.0317 (13) | |
C12 | 0.0530 (4) | 0.0411 (3) | 0.1695 (2) | 0.0397 (14) | |
H12A | −0.0034 | 0.0570 | 0.1657 | 0.048* | |
C13 | 0.0680 (4) | −0.0226 (3) | 0.1596 (3) | 0.0570 (18) | |
H13A | 0.0223 | −0.0499 | 0.1491 | 0.068* | |
C14 | 0.1498 (4) | −0.0468 (3) | 0.1648 (3) | 0.0587 (19) | |
H14A | 0.1602 | −0.0908 | 0.1582 | 0.070* | |
C15 | 0.2165 (4) | −0.0062 (3) | 0.1799 (3) | 0.0555 (18) | |
H15A | 0.2727 | −0.0225 | 0.1834 | 0.067* | |
C16 | 0.2011 (4) | 0.0580 (3) | 0.1899 (2) | 0.0402 (14) | |
H16A | 0.2471 | 0.0853 | 0.2003 | 0.048* | |
C17 | 0.1949 (3) | 0.2098 (3) | 0.1818 (2) | 0.0305 (13) | |
H17A | 0.1862 | 0.2556 | 0.1901 | 0.037* | |
H17B | 0.2418 | 0.1949 | 0.2076 | 0.037* | |
C18 | 0.2241 (3) | 0.2030 (3) | 0.1167 (2) | 0.0387 (15) | |
H18A | 0.2240 | 0.1579 | 0.1055 | 0.058* | |
H18B | 0.2818 | 0.2203 | 0.1124 | 0.058* | |
H18C | 0.1850 | 0.2266 | 0.0910 | 0.058* | |
C19 | 0.0104 (3) | 0.1932 (3) | 0.1544 (2) | 0.0348 (14) | |
H19A | −0.0432 | 0.1754 | 0.1705 | 0.042* | |
H19B | 0.0062 | 0.2402 | 0.1577 | 0.042* | |
C20 | 0.0133 (4) | 0.1768 (3) | 0.0881 (2) | 0.0476 (17) | |
H20A | 0.0524 | 0.2060 | 0.0679 | 0.071* | |
H20B | −0.0438 | 0.1811 | 0.0712 | 0.071* | |
H20C | 0.0333 | 0.1330 | 0.0831 | 0.071* | |
C21 | 0.1606 (3) | 0.3832 (3) | 0.3959 (2) | 0.0289 (12) | |
C22 | 0.1721 (3) | 0.4331 (3) | 0.3562 (3) | 0.0401 (15) | |
H22A | 0.1880 | 0.4241 | 0.3166 | 0.048* | |
C23 | 0.1604 (4) | 0.4964 (3) | 0.3738 (3) | 0.0547 (18) | |
H23A | 0.1689 | 0.5298 | 0.3462 | 0.066* | |
C24 | 0.1368 (4) | 0.5104 (3) | 0.4307 (4) | 0.061 (2) | |
H24A | 0.1288 | 0.5534 | 0.4425 | 0.073* | |
C25 | 0.1247 (4) | 0.4617 (3) | 0.4707 (3) | 0.0566 (19) | |
H25A | 0.1082 | 0.4716 | 0.5100 | 0.068* | |
C26 | 0.1364 (3) | 0.3982 (3) | 0.4543 (3) | 0.0424 (15) | |
H26A | 0.1281 | 0.3651 | 0.4824 | 0.051* | |
C27 | 0.2658 (3) | 0.3022 (3) | 0.3203 (2) | 0.0336 (13) | |
H27A | 0.2857 | 0.2579 | 0.3143 | 0.040* | |
H27B | 0.2446 | 0.3179 | 0.2818 | 0.040* | |
C28 | 0.3437 (3) | 0.3430 (3) | 0.3379 (2) | 0.0512 (17) | |
H28A | 0.3257 | 0.3872 | 0.3440 | 0.077* | |
H28B | 0.3863 | 0.3414 | 0.3062 | 0.077* | |
H28C | 0.3686 | 0.3264 | 0.3745 | 0.077* | |
C29 | 0.2088 (3) | 0.2553 (3) | 0.4376 (2) | 0.0327 (13) | |
H29A | 0.1630 | 0.2588 | 0.4675 | 0.039* | |
H29B | 0.2127 | 0.2098 | 0.4263 | 0.039* | |
C30 | 0.2923 (3) | 0.2734 (3) | 0.4675 (2) | 0.0546 (19) | |
H30A | 0.3398 | 0.2655 | 0.4403 | 0.082* | |
H30B | 0.2999 | 0.2477 | 0.5033 | 0.082* | |
H30C | 0.2911 | 0.3187 | 0.4781 | 0.082* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Re1 | 0.02020 (10) | 0.02311 (10) | 0.02205 (9) | 0.00098 (9) | 0.00060 (8) | 0.00143 (9) |
Re2 | 0.01974 (10) | 0.02304 (10) | 0.02207 (9) | 0.00016 (9) | −0.00047 (8) | 0.00132 (9) |
Cl1 | 0.0243 (7) | 0.0403 (8) | 0.0349 (7) | 0.0084 (6) | −0.0016 (6) | 0.0014 (7) |
Cl2 | 0.0247 (7) | 0.0370 (8) | 0.0326 (7) | −0.0065 (6) | −0.0011 (6) | 0.0000 (6) |
Cl3 | 0.0328 (8) | 0.0388 (8) | 0.0278 (6) | −0.0001 (6) | 0.0079 (5) | −0.0010 (6) |
Cl4 | 0.0241 (8) | 0.0388 (8) | 0.0505 (8) | 0.0033 (6) | −0.0076 (6) | 0.0037 (7) |
Cl5 | 0.0368 (8) | 0.0313 (7) | 0.0284 (6) | −0.0018 (6) | −0.0017 (6) | 0.0055 (6) |
P1 | 0.0285 (8) | 0.0269 (7) | 0.0268 (7) | 0.0021 (6) | 0.0001 (6) | 0.0059 (6) |
P2 | 0.0250 (7) | 0.0281 (7) | 0.0233 (7) | −0.0013 (6) | 0.0021 (5) | −0.0014 (6) |
P3 | 0.0221 (8) | 0.0301 (8) | 0.0256 (7) | −0.0026 (6) | 0.0001 (6) | −0.0003 (6) |
C1 | 0.035 (3) | 0.021 (3) | 0.025 (3) | 0.003 (2) | −0.002 (2) | 0.008 (2) |
C2 | 0.036 (3) | 0.036 (3) | 0.038 (3) | 0.008 (3) | 0.001 (3) | 0.004 (3) |
C3 | 0.067 (5) | 0.034 (4) | 0.033 (3) | 0.013 (3) | −0.003 (3) | −0.002 (3) |
C4 | 0.065 (5) | 0.041 (4) | 0.035 (3) | 0.006 (3) | −0.021 (3) | −0.001 (3) |
C5 | 0.041 (4) | 0.045 (4) | 0.041 (3) | 0.007 (3) | −0.009 (3) | 0.002 (3) |
C6 | 0.042 (4) | 0.039 (3) | 0.030 (3) | 0.006 (3) | −0.001 (3) | 0.006 (3) |
C7 | 0.057 (4) | 0.026 (3) | 0.042 (3) | 0.003 (3) | −0.007 (3) | 0.008 (3) |
C8 | 0.093 (5) | 0.029 (3) | 0.055 (4) | 0.008 (3) | −0.010 (4) | −0.002 (3) |
C9 | 0.023 (3) | 0.048 (4) | 0.033 (3) | −0.006 (3) | 0.002 (2) | 0.014 (3) |
C10 | 0.046 (4) | 0.060 (5) | 0.054 (4) | −0.015 (3) | 0.008 (3) | 0.018 (4) |
C11 | 0.034 (3) | 0.034 (3) | 0.027 (3) | 0.001 (2) | 0.005 (2) | −0.006 (3) |
C12 | 0.035 (3) | 0.035 (3) | 0.049 (3) | 0.001 (3) | 0.001 (3) | −0.009 (3) |
C13 | 0.043 (4) | 0.040 (4) | 0.089 (5) | −0.009 (3) | 0.015 (4) | −0.017 (4) |
C14 | 0.063 (5) | 0.029 (4) | 0.084 (5) | −0.001 (3) | 0.029 (4) | −0.008 (4) |
C15 | 0.042 (4) | 0.041 (4) | 0.083 (5) | 0.011 (3) | 0.015 (4) | −0.006 (4) |
C16 | 0.037 (4) | 0.038 (4) | 0.046 (3) | 0.000 (3) | 0.007 (3) | −0.003 (3) |
C17 | 0.029 (3) | 0.033 (3) | 0.029 (3) | −0.004 (2) | 0.006 (2) | 0.000 (2) |
C18 | 0.034 (3) | 0.048 (4) | 0.034 (3) | −0.001 (3) | 0.011 (3) | 0.004 (3) |
C19 | 0.031 (3) | 0.045 (3) | 0.028 (3) | 0.002 (3) | −0.003 (2) | 0.001 (3) |
C20 | 0.054 (4) | 0.055 (4) | 0.034 (3) | 0.001 (3) | −0.011 (3) | −0.001 (3) |
C21 | 0.018 (3) | 0.031 (3) | 0.038 (3) | −0.004 (2) | −0.003 (2) | −0.002 (3) |
C22 | 0.033 (4) | 0.038 (4) | 0.049 (4) | −0.008 (3) | −0.003 (3) | 0.002 (3) |
C23 | 0.043 (4) | 0.040 (4) | 0.082 (5) | −0.008 (3) | −0.018 (4) | 0.015 (4) |
C24 | 0.040 (4) | 0.037 (4) | 0.105 (6) | 0.003 (3) | −0.019 (4) | −0.023 (5) |
C25 | 0.048 (4) | 0.055 (5) | 0.067 (5) | 0.005 (4) | −0.005 (4) | −0.027 (4) |
C26 | 0.041 (4) | 0.039 (4) | 0.047 (4) | −0.002 (3) | 0.000 (3) | −0.013 (3) |
C27 | 0.023 (3) | 0.042 (3) | 0.036 (3) | −0.001 (2) | 0.004 (2) | −0.006 (3) |
C28 | 0.031 (3) | 0.073 (5) | 0.049 (4) | −0.015 (3) | 0.005 (3) | −0.013 (4) |
C29 | 0.034 (3) | 0.033 (3) | 0.031 (3) | 0.000 (3) | −0.007 (2) | −0.001 (3) |
C30 | 0.037 (4) | 0.085 (6) | 0.041 (3) | 0.004 (4) | −0.012 (3) | 0.004 (4) |
Re1—Re2 | 2.2262 (3) | C12—H12A | 0.9400 |
Re1—Cl2 | 2.3453 (12) | C13—C14 | 1.372 (8) |
Re1—Cl1 | 2.3556 (12) | C13—H13A | 0.9400 |
Re1—P2 | 2.4525 (12) | C14—C15 | 1.378 (8) |
Re1—P1 | 2.4703 (13) | C14—H14A | 0.9400 |
Re2—Cl3 | 2.3314 (12) | C15—C16 | 1.375 (8) |
Re2—Cl5 | 2.3436 (12) | C15—H15A | 0.9400 |
Re2—Cl4 | 2.3469 (13) | C16—H16A | 0.9400 |
Re2—P3 | 2.4551 (13) | C17—C18 | 1.534 (6) |
P1—C9 | 1.821 (5) | C17—H17A | 0.9800 |
P1—C1 | 1.835 (5) | C17—H17B | 0.9800 |
P1—C7 | 1.845 (5) | C18—H18A | 0.9700 |
P2—C17 | 1.814 (5) | C18—H18B | 0.9700 |
P2—C11 | 1.819 (5) | C18—H18C | 0.9700 |
P2—C19 | 1.822 (5) | C19—C20 | 1.523 (6) |
P3—C29 | 1.813 (5) | C19—H19A | 0.9800 |
P3—C21 | 1.822 (5) | C19—H19B | 0.9800 |
P3—C27 | 1.827 (5) | C20—H20A | 0.9700 |
C1—C2 | 1.371 (6) | C20—H20B | 0.9700 |
C1—C6 | 1.397 (7) | C20—H20C | 0.9700 |
C2—C3 | 1.393 (7) | C21—C22 | 1.377 (7) |
C2—H2A | 0.9400 | C21—C26 | 1.396 (7) |
C3—C4 | 1.374 (7) | C22—C23 | 1.383 (8) |
C3—H3A | 0.9400 | C22—H22A | 0.9400 |
C4—C5 | 1.355 (7) | C23—C24 | 1.357 (8) |
C4—H4A | 0.9400 | C23—H23A | 0.9400 |
C5—C6 | 1.378 (7) | C24—C25 | 1.363 (8) |
C5—H5A | 0.9400 | C24—H24A | 0.9400 |
C6—H6A | 0.9400 | C25—C26 | 1.383 (8) |
C7—C8 | 1.502 (7) | C25—H25A | 0.9400 |
C7—H7A | 0.9800 | C26—H26A | 0.9400 |
C7—H7B | 0.9800 | C27—C28 | 1.530 (7) |
C8—H8A | 0.9700 | C27—H27A | 0.9800 |
C8—H8B | 0.9700 | C27—H27B | 0.9800 |
C8—H8C | 0.9700 | C28—H28A | 0.9700 |
C9—C10 | 1.524 (7) | C28—H28B | 0.9700 |
C9—H9A | 0.9800 | C28—H28C | 0.9700 |
C9—H9B | 0.9800 | C29—C30 | 1.508 (6) |
C10—H10A | 0.9700 | C29—H29A | 0.9800 |
C10—H10B | 0.9700 | C29—H29B | 0.9800 |
C10—H10C | 0.9700 | C30—H30A | 0.9700 |
C11—C16 | 1.386 (7) | C30—H30B | 0.9700 |
C11—C12 | 1.390 (7) | C30—H30C | 0.9700 |
C12—C13 | 1.362 (7) | ||
Re2—Re1—Cl2 | 103.86 (3) | C12—C11—P2 | 121.7 (4) |
Re2—Re1—Cl1 | 112.83 (3) | C13—C12—C11 | 121.7 (5) |
Cl2—Re1—Cl1 | 143.29 (5) | C13—C12—H12A | 119.1 |
Re2—Re1—P2 | 103.76 (4) | C11—C12—H12A | 119.1 |
Cl2—Re1—P2 | 83.86 (4) | C12—C13—C14 | 120.1 (6) |
Cl1—Re1—P2 | 86.25 (4) | C12—C13—H13A | 119.9 |
Re2—Re1—P1 | 104.88 (3) | C14—C13—H13A | 119.9 |
Cl2—Re1—P1 | 84.40 (4) | C13—C14—C15 | 119.5 (6) |
Cl1—Re1—P1 | 87.42 (4) | C13—C14—H14A | 120.3 |
P2—Re1—P1 | 150.89 (5) | C15—C14—H14A | 120.3 |
Re1—Re2—Cl3 | 108.23 (4) | C16—C15—C14 | 120.2 (6) |
Re1—Re2—Cl5 | 109.51 (3) | C16—C15—H15A | 119.9 |
Cl3—Re2—Cl5 | 142.19 (5) | C14—C15—H15A | 119.9 |
Re1—Re2—Cl4 | 104.17 (3) | C15—C16—C11 | 121.0 (6) |
Cl3—Re2—Cl4 | 86.39 (5) | C15—C16—H16A | 119.5 |
Cl5—Re2—Cl4 | 86.55 (5) | C11—C16—H16A | 119.5 |
Re1—Re2—P3 | 101.04 (3) | C18—C17—P2 | 116.8 (4) |
Cl3—Re2—P3 | 84.93 (4) | C18—C17—H17A | 108.1 |
Cl5—Re2—P3 | 85.91 (4) | P2—C17—H17A | 108.1 |
Cl4—Re2—P3 | 154.77 (5) | C18—C17—H17B | 108.1 |
C9—P1—C1 | 105.7 (2) | P2—C17—H17B | 108.1 |
C9—P1—C7 | 105.8 (3) | H17A—C17—H17B | 107.3 |
C1—P1—C7 | 101.0 (2) | C17—C18—H18A | 109.5 |
C9—P1—Re1 | 113.50 (17) | C17—C18—H18B | 109.5 |
C1—P1—Re1 | 122.29 (16) | H18A—C18—H18B | 109.5 |
C7—P1—Re1 | 106.70 (18) | C17—C18—H18C | 109.5 |
C17—P2—C11 | 105.1 (2) | H18A—C18—H18C | 109.5 |
C17—P2—C19 | 108.6 (2) | H18B—C18—H18C | 109.5 |
C11—P2—C19 | 106.7 (2) | C20—C19—P2 | 119.6 (4) |
C17—P2—Re1 | 117.53 (16) | C20—C19—H19A | 107.4 |
C11—P2—Re1 | 103.65 (17) | P2—C19—H19A | 107.4 |
C19—P2—Re1 | 114.24 (16) | C20—C19—H19B | 107.4 |
C29—P3—C21 | 106.6 (2) | P2—C19—H19B | 107.4 |
C29—P3—C27 | 107.5 (2) | H19A—C19—H19B | 107.0 |
C21—P3—C27 | 104.8 (2) | C19—C20—H20A | 109.5 |
C29—P3—Re2 | 114.44 (17) | C19—C20—H20B | 109.5 |
C21—P3—Re2 | 105.23 (16) | H20A—C20—H20B | 109.5 |
C27—P3—Re2 | 117.23 (16) | C19—C20—H20C | 109.5 |
C2—C1—C6 | 118.1 (5) | H20A—C20—H20C | 109.5 |
C2—C1—P1 | 121.7 (4) | H20B—C20—H20C | 109.5 |
C6—C1—P1 | 120.1 (4) | C22—C21—C26 | 118.1 (5) |
C1—C2—C3 | 121.0 (5) | C22—C21—P3 | 120.7 (4) |
C1—C2—H2A | 119.5 | C26—C21—P3 | 121.2 (4) |
C3—C2—H2A | 119.5 | C21—C22—C23 | 121.0 (6) |
C4—C3—C2 | 119.7 (5) | C21—C22—H22A | 119.5 |
C4—C3—H3A | 120.2 | C23—C22—H22A | 119.5 |
C2—C3—H3A | 120.2 | C24—C23—C22 | 120.4 (7) |
C5—C4—C3 | 120.0 (5) | C24—C23—H23A | 119.8 |
C5—C4—H4A | 120.0 | C22—C23—H23A | 119.8 |
C3—C4—H4A | 120.0 | C23—C24—C25 | 119.6 (6) |
C4—C5—C6 | 120.9 (6) | C23—C24—H24A | 120.2 |
C4—C5—H5A | 119.5 | C25—C24—H24A | 120.2 |
C6—C5—H5A | 119.5 | C24—C25—C26 | 121.0 (6) |
C5—C6—C1 | 120.3 (5) | C24—C25—H25A | 119.5 |
C5—C6—H6A | 119.9 | C26—C25—H25A | 119.5 |
C1—C6—H6A | 119.9 | C25—C26—C21 | 119.8 (6) |
C8—C7—P1 | 118.1 (4) | C25—C26—H26A | 120.1 |
C8—C7—H7A | 107.8 | C21—C26—H26A | 120.1 |
P1—C7—H7A | 107.8 | C28—C27—P3 | 117.5 (4) |
C8—C7—H7B | 107.8 | C28—C27—H27A | 107.9 |
P1—C7—H7B | 107.8 | P3—C27—H27A | 107.9 |
H7A—C7—H7B | 107.1 | C28—C27—H27B | 107.9 |
C7—C8—H8A | 109.5 | P3—C27—H27B | 107.9 |
C7—C8—H8B | 109.5 | H27A—C27—H27B | 107.2 |
H8A—C8—H8B | 109.5 | C27—C28—H28A | 109.5 |
C7—C8—H8C | 109.5 | C27—C28—H28B | 109.5 |
H8A—C8—H8C | 109.5 | H28A—C28—H28B | 109.5 |
H8B—C8—H8C | 109.5 | C27—C28—H28C | 109.5 |
C10—C9—P1 | 117.0 (4) | H28A—C28—H28C | 109.5 |
C10—C9—H9A | 108.0 | H28B—C28—H28C | 109.5 |
P1—C9—H9A | 108.0 | C30—C29—P3 | 118.7 (4) |
C10—C9—H9B | 108.0 | C30—C29—H29A | 107.6 |
P1—C9—H9B | 108.0 | P3—C29—H29A | 107.6 |
H9A—C9—H9B | 107.3 | C30—C29—H29B | 107.6 |
C9—C10—H10A | 109.5 | P3—C29—H29B | 107.6 |
C9—C10—H10B | 109.5 | H29A—C29—H29B | 107.1 |
H10A—C10—H10B | 109.5 | C29—C30—H30A | 109.5 |
C9—C10—H10C | 109.5 | C29—C30—H30B | 109.5 |
H10A—C10—H10C | 109.5 | H30A—C30—H30B | 109.5 |
H10B—C10—H10C | 109.5 | C29—C30—H30C | 109.5 |
C16—C11—C12 | 117.4 (5) | H30A—C30—H30C | 109.5 |
C16—C11—P2 | 120.7 (4) | H30B—C30—H30C | 109.5 |
Cl1—Re1—Re2—P3 | −4.10 (5) | Cl2—Re1—Re2—Cl4 | −1.88 (5) |
P2—Re1—Re2—Cl5 | −6.28 (5) | P1—Re1—Re2—Cl3 | 1.16 (5) |
Experimental details
Crystal data | |
Chemical formula | [Re2Cl5(C10H15P)3] |
Mr | 1048.22 |
Crystal system, space group | Orthorhombic, Pbca |
Temperature (K) | 213 |
a, b, c (Å) | 15.5374 (7), 20.7751 (9), 22.3924 (10) |
V (Å3) | 7228.1 (6) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 7.22 |
Crystal size (mm) | 0.12 × 0.11 × 0.08 |
Data collection | |
Diffractometer | Bruker SMART diffractometer |
Absorption correction | Multi-scan (SADABS; Blessing, 1995) |
Tmin, Tmax | 0.410, 0.561 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 34336, 8235, 5875 |
Rint | 0.053 |
(sin θ/λ)max (Å−1) | 0.651 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.031, 0.048, 1.01 |
No. of reflections | 8235 |
No. of parameters | 367 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.64, −1.11 |
Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2001), SAINT, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), SHELXTL (Siemens, 1996), SHELXL97.
Re1—Re2 | 2.2262 (3) | Re2—Cl3 | 2.3314 (12) |
Re1—Cl2 | 2.3453 (12) | Re2—Cl5 | 2.3436 (12) |
Re1—Cl1 | 2.3556 (12) | Re2—Cl4 | 2.3469 (13) |
Re1—P2 | 2.4525 (12) | Re2—P3 | 2.4551 (13) |
Re1—P1 | 2.4703 (13) | ||
Re2—Re1—Cl2 | 103.86 (3) | Re1—Re2—Cl3 | 108.23 (4) |
Re2—Re1—Cl1 | 112.83 (3) | Re1—Re2—Cl5 | 109.51 (3) |
Cl2—Re1—Cl1 | 143.29 (5) | Cl3—Re2—Cl5 | 142.19 (5) |
Re2—Re1—P2 | 103.76 (4) | Re1—Re2—Cl4 | 104.17 (3) |
Cl2—Re1—P2 | 83.86 (4) | Cl3—Re2—Cl4 | 86.39 (5) |
Cl1—Re1—P2 | 86.25 (4) | Cl5—Re2—Cl4 | 86.55 (5) |
Re2—Re1—P1 | 104.88 (3) | Re1—Re2—P3 | 101.04 (3) |
Cl2—Re1—P1 | 84.40 (4) | Cl3—Re2—P3 | 84.93 (4) |
Cl1—Re1—P1 | 87.42 (4) | Cl5—Re2—P3 | 85.91 (4) |
P2—Re1—P1 | 150.89 (5) | Cl4—Re2—P3 | 154.77 (5) |
Cl1—Re1—Re2—P3 | −4.10 (5) | Cl2—Re1—Re2—Cl4 | −1.88 (5) |
P2—Re1—Re2—Cl5 | −6.28 (5) | P1—Re1—Re2—Cl3 | 1.16 (5) |
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Although many dirhenium compounds with multiple metal–metal bonds and tertiary phosphine ligands (PR3) of the type Re2Cl5(PR3)3 are known (Cotton & Walton, 1993), none containing diethylphenylphosphine ligands have been reported previously. Structures have been determined for 1,2,7- and 1,3,6-Re2Cl5(trimethylphosphine)3 and 1,3,6-Re2Cl5(triethylphosphine)3 (Cotton et al., 1990), 1,2,7- and 1,3,6-Re2Cl5(dimethylphenylphosphine)3 (Cotton et al., 1998), and 1,3,6-Re2Cl5(tri-n-propylphosphine)3 (Cotton et al., 1999) and 1,3,6-Re2Cl5(dicyclohexylphosphine)3 (Angaridis et al., 2002). The title compound, (I), was prepared from the quadruply bonded [Re2Cl8]2- ion in a solvent mixture containing a room-temperature ionic liquid.
As expected, the molecular structure of (I) is similar to that of the five previously characterized 1,3,6-Re2Cl5(PR3)3 compounds. In each molecule, one Re atom is bound to two trans-phosphine ligands, while the other Re atom is bound to one phosphine ligand. The two Re atoms are also bound to one another, with a metal–metal bond order of 3.5. The rotational conformation is essentially eclipsed, as opposed to the somewhat staggered conformations adopted by 1,3,6-Re2Cl5(dicyclohexylphosphine)3 and the two known 1,2,7-Re2Cl5(PR3)3 complexes. The Re—Re bond distance of 2.2262 (3) Å is slightly longer than those found in the other 1,3,6-Re2Cl5(PR3)3 compounds. This is presumably due to some additional steric crowding introduced by the larger PEt2Ph ligands. Average Re—P and Re—Cl bond lengths [2.459 (6) and 2.345 (4) Å, respectively] are well within the ranges [2.425 (4)–2.478 (5) Å for Re—P and 2.313 (4)–2.416 (8) Å for Re—Cl] observed before in these complexes. A threefold disordering of the dirhenium unit is a common feature of multiply-bonded dirhenium complexes of the types Re2Cl4(PR3)3 and Re2Cl5(PR3)3 (Cotton et al., 1999), but no such disorder exists in 1,3,6-Re2Cl5(PEt2Ph)3.