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The title compound, dicarbonyl-1κ
2C-di-μ-chloro-1:2κ
4Cl-[
cis,cis-2(η
4)-1,5-cyclooctadiene]dirhodium(I), [Rh
2Cl
2(C
8H
12)(CO)
2], consists of a dichloro-bridged dimer of rhodium, with a non-bonded Rh
Rh distance of 3.284 (2) Å. One Rh atom is coordinated to two carbonyl ligands, while the other Rh atom is coordinated to the cyclooctadiene moiety.
Supporting information
CCDC reference: 163878
Data collection: Kappa CCD Software (Enraf-Nonius, 1997); cell refinement: DENZO (Otwinowski & Minor, 1997); data reduction: DENZO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 1990); software used to prepare material for publication: SHELXCIF-97 (Sheldrick, 1997).
Di-µ-chloro-dicarbonyl-
cis,
cis-
η4-1,5-cyclooctadienedirhodium(I)
top
Crystal data top
[Rh2Cl2(CO)2(C8H12)] | F(000) = 848 |
Mr = 440.92 | Dx = 2.238 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71069 Å |
a = 6.6500 (12) Å | Cell parameters from 15389 reflections |
b = 12.261 (3) Å | θ = 2.1–30.0° |
c = 16.058 (3) Å | µ = 2.91 mm−1 |
β = 92.19 (3)° | T = 293 K |
V = 1308.3 (5) Å3 | Block, orange |
Z = 4 | 0.15 × 0.1 × 0.1 mm |
Data collection top
NONIUS KAPPA CCD diffractometer | 2261 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.000 |
Graphite monochromator | θmax = 30.0°, θmin = 2.1° |
area detector scans | h = 0→9 |
15389 measured reflections | k = 0→17 |
3699 independent reflections | l = −22→22 |
Refinement top
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)] = 0.067 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.196 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.12 | w = 1/[σ2(Fo2) + (0.1P)2] where P = (Fo2 + 2Fc2)/3 |
3699 reflections | (Δ/σ)max = 0.001 |
145 parameters | Δρmax = 1.01 e Å−3 |
0 restraints | Δρmin = −1.28 e Å−3 |
Special details top
Experimental. Diffractometer equiped with an area detector phi scans during 10 s with 1 °
steps Crystal to detector distance: 35 mm Total number of images collected:
251 Data are 96.8% complete to 2 theta = 60.04 degres |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Rh1 | 0.25775 (9) | 0.44712 (4) | 0.26378 (4) | 0.0429 (2) | |
Rh2 | −0.08231 (10) | 0.43789 (5) | 0.40667 (4) | 0.0510 (2) | |
Cl1 | 0.0824 (3) | 0.58375 (17) | 0.34039 (13) | 0.0588 (6) | |
Cl2 | 0.2106 (4) | 0.33330 (18) | 0.38400 (14) | 0.0682 (6) | |
O2 | −0.2848 (11) | 0.2460 (5) | 0.4799 (4) | 0.091 (2) | |
O1 | −0.4441 (10) | 0.5760 (5) | 0.4245 (5) | 0.085 (2) | |
C1 | 0.3903 (14) | 0.5657 (6) | 0.1892 (7) | 0.063 (2) | |
H1 | 0.3750 | 0.6158 | 0.2319 | 0.082* | |
C2 | 0.6035 (15) | 0.5334 (9) | 0.1698 (8) | 0.087 (3) | |
H2A | 0.6323 | 0.5601 | 0.1147 | 0.113* | |
H2B | 0.6953 | 0.5695 | 0.2093 | 0.113* | |
C3 | 0.6446 (14) | 0.4151 (8) | 0.1727 (7) | 0.072 (3) | |
H3A | 0.7766 | 0.4036 | 0.1990 | 0.093* | |
H3B | 0.6487 | 0.3879 | 0.1160 | 0.093* | |
C4 | 0.4924 (12) | 0.3492 (7) | 0.2188 (5) | 0.057 (2) | |
H4 | 0.5250 | 0.3315 | 0.2740 | 0.074* | |
C5 | 0.3113 (13) | 0.3133 (6) | 0.1866 (5) | 0.055 (2) | |
H5 | 0.2286 | 0.2745 | 0.2214 | 0.072* | |
C6 | 0.2382 (17) | 0.3329 (8) | 0.0988 (7) | 0.081 (3) | |
H6A | 0.3281 | 0.2966 | 0.0615 | 0.105* | |
H6B | 0.1060 | 0.3003 | 0.0906 | 0.105* | |
C7 | 0.226 (2) | 0.4504 (10) | 0.0761 (7) | 0.104 (4) | |
H7A | 0.1073 | 0.4613 | 0.0398 | 0.135* | |
H7B | 0.3424 | 0.4691 | 0.0447 | 0.135* | |
C8 | 0.2148 (15) | 0.5272 (7) | 0.1488 (6) | 0.063 (2) | |
H8 | 0.0901 | 0.5493 | 0.1670 | 0.082* | |
C9 | −0.3070 (14) | 0.5237 (8) | 0.4192 (6) | 0.060 (2) | |
C10 | −0.2082 (14) | 0.3191 (8) | 0.4530 (5) | 0.062 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rh1 | 0.0454 (4) | 0.0412 (3) | 0.0426 (4) | 0.0020 (2) | 0.0078 (3) | 0.0023 (2) |
Rh2 | 0.0527 (4) | 0.0623 (4) | 0.0384 (4) | 0.0012 (3) | 0.0078 (3) | 0.0015 (3) |
Cl1 | 0.0612 (13) | 0.0526 (11) | 0.0640 (14) | 0.0080 (9) | 0.0200 (11) | −0.0011 (9) |
Cl2 | 0.0786 (15) | 0.0684 (13) | 0.0590 (13) | 0.0218 (11) | 0.0204 (11) | 0.0205 (10) |
O2 | 0.113 (6) | 0.073 (4) | 0.091 (5) | −0.021 (4) | 0.034 (5) | 0.010 (4) |
O1 | 0.053 (4) | 0.099 (5) | 0.103 (6) | 0.010 (4) | 0.012 (4) | 0.000 (4) |
C1 | 0.072 (6) | 0.054 (5) | 0.065 (6) | −0.013 (4) | 0.016 (5) | 0.011 (4) |
C2 | 0.061 (6) | 0.100 (8) | 0.100 (9) | −0.013 (6) | 0.025 (6) | 0.008 (7) |
C3 | 0.046 (5) | 0.086 (7) | 0.083 (7) | 0.001 (5) | 0.006 (5) | −0.025 (6) |
C4 | 0.054 (5) | 0.072 (5) | 0.046 (5) | 0.018 (4) | 0.004 (4) | −0.015 (4) |
C5 | 0.065 (5) | 0.047 (4) | 0.055 (5) | −0.006 (4) | 0.011 (4) | −0.010 (4) |
C6 | 0.082 (7) | 0.087 (7) | 0.073 (7) | −0.007 (6) | −0.007 (5) | −0.019 (6) |
C7 | 0.122 (11) | 0.135 (11) | 0.053 (7) | 0.000 (8) | −0.010 (7) | 0.013 (6) |
C8 | 0.072 (6) | 0.066 (5) | 0.054 (5) | 0.010 (5) | 0.019 (5) | 0.022 (4) |
C9 | 0.053 (5) | 0.074 (5) | 0.054 (5) | −0.004 (5) | 0.006 (4) | 0.000 (4) |
C10 | 0.069 (6) | 0.069 (6) | 0.049 (5) | 0.002 (5) | 0.009 (4) | −0.003 (4) |
Geometric parameters (Å, º) top
Rh1—C5 | 2.094 (7) | O2—C10 | 1.125 (10) |
Rh1—C1 | 2.099 (8) | O1—C9 | 1.121 (10) |
Rh1—C8 | 2.101 (8) | C1—C8 | 1.395 (14) |
Rh1—C4 | 2.118 (7) | C1—C2 | 1.516 (12) |
Rh1—Cl1 | 2.406 (2) | C2—C3 | 1.476 (12) |
Rh1—Cl2 | 2.412 (2) | C3—C4 | 1.512 (12) |
Rh2—C9 | 1.844 (9) | C4—C5 | 1.365 (11) |
Rh2—C10 | 1.850 (9) | C5—C6 | 1.493 (13) |
Rh2—Cl1 | 2.371 (2) | C6—C7 | 1.487 (13) |
Rh2—Cl2 | 2.372 (2) | C7—C8 | 1.504 (14) |
| | | |
C5—Rh1—C1 | 96.9 (4) | Rh2—Cl1—Rh1 | 86.88 (8) |
C5—Rh1—C8 | 82.3 (4) | Rh2—Cl2—Rh1 | 86.71 (7) |
C1—Rh1—C8 | 38.8 (4) | C8—C1—C2 | 126.1 (10) |
C5—Rh1—C4 | 37.8 (3) | C8—C1—Rh1 | 70.7 (5) |
C1—Rh1—C4 | 82.4 (4) | C2—C1—Rh1 | 110.6 (6) |
C8—Rh1—C4 | 92.5 (4) | C3—C2—C1 | 115.1 (8) |
C5—Rh1—Cl1 | 160.8 (2) | C2—C3—C4 | 114.4 (8) |
C1—Rh1—Cl1 | 91.8 (3) | C5—C4—C3 | 125.7 (8) |
C8—Rh1—Cl1 | 94.1 (3) | C5—C4—Rh1 | 70.2 (5) |
C4—Rh1—Cl1 | 161.3 (2) | C3—C4—Rh1 | 112.3 (6) |
C5—Rh1—Cl2 | 92.9 (2) | C4—C5—C6 | 123.8 (8) |
C1—Rh1—Cl2 | 158.1 (3) | C4—C5—Rh1 | 72.0 (4) |
C8—Rh1—Cl2 | 163.0 (3) | C6—C5—Rh1 | 112.1 (6) |
C4—Rh1—Cl2 | 93.7 (3) | C7—C6—C5 | 113.6 (8) |
Cl1—Rh1—Cl2 | 85.03 (8) | C6—C7—C8 | 114.9 (9) |
C9—Rh2—C10 | 91.4 (4) | C1—C8—C7 | 120.6 (10) |
C9—Rh2—Cl1 | 90.5 (3) | C1—C8—Rh1 | 70.5 (5) |
C10—Rh2—Cl1 | 176.7 (3) | C7—C8—Rh1 | 112.3 (6) |
C9—Rh2—Cl2 | 176.8 (3) | O1—C9—Rh2 | 178.2 (9) |
C10—Rh2—Cl2 | 91.3 (3) | O2—C10—Rh2 | 178.8 (8) |
Cl1—Rh2—Cl2 | 86.71 (8) | | |
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