Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801003750/bt6017sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801003750/bt6017Isup2.hkl |
CCDC reference: 162793
Key indicators
- Single-crystal X-ray study
- T = 200 K
- Mean (C-C) = 0.013 Å
- R factor = 0.042
- wR factor = 0.054
- Data-to-parameter ratio = 19.5
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Na[W(CO)3(η5-C5H4Me)] was prepared from Na (46.8 mg, 2.03 mmol), methylcyclopentadiene (410 mg, 5.11 mmol) and W(CO)6 (543 mg, 5.10 mmol). IrCl(CO)2(p-toluidine) (598 mg, 1.53 mmol) was added to the crude solid Na[W(CO)3(η5-C5H4Me)] in CH2Cl2 (20 ml), and the mixture stirred at room temperature for 2 h. The solvent was removed in vacuo, and the resulting red–brown residue dissolved in CH2Cl2 (ca 3 ml) then applied to preparative thin-layer chromatography (TLC) plates. Elution with CH2Cl2/petroleum spirit (2/3) gave two bands. Crystallization of the contents of the second and major band (RF = 0.52) from CH2Cl2/methanol by liquid diffusion at 276 K over 24 h afforded a red–brown crystalline product identified as W2Ir2(CO)10(η5-C5H4Me)2 (733 mg, 81%). Analysis calculated for C22H14Ir2O10W2: C 22.20, H 1.19%; found: C 22.56 H 1.27%. MS (secondary ion, Cs+): [M - nCO]+, n = 2–10. IR (cyclohexane): ν(CO) 2063 (m), 2028 (s), 2006 (m), 1995 (m), 1982 (m), 1965 (w), 1948 (w), 1921 (w), 1890 (w), 1827 (w) cm-1. 1H NMR: δ 5.25 (t, JHH = 2 Hz, 4H, C5H4Me), 4.94 (t, JHH = 2 Hz, 4H, C5H4Me), 2.18 (s, 6H, Me) p.p.m.
Data collection: KappaCCD Software (Nonius, 1997); cell refinement: HKL SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO and Scalepak (Otwinowski & Minor, 1997); program(s) used to solve structure: PATTY in DIRDIF92 (Beurskens et al., 1992); program(s) used to refine structure: TEXSAN (Molecular Structure Corporation, 1997); software used to prepare material for publication: TEXSAN.
Fig. 1. A view of both molecules in the asymmetric unit of the title compound with the atom-numbering scheme. Displacement ellipsoids are shown at the 30% probability level. |
[W2Ir2(C6H7)2(CO)10] | F(000) = 4224.00 |
Mr = 1190.49 | Dx = 3.236 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.7107 Å |
a = 18.3035 (1) Å | Cell parameters from 267775 reflections |
b = 8.5629 (1) Å | θ = 2.9–30.0° |
c = 31.2876 (2) Å | µ = 20.34 mm−1 |
β = 94.7702 (4)° | T = 200 K |
V = 4886.75 (6) Å3 | Needle, red-brown |
Z = 8 | 0.40 × 0.20 × 0.15 mm |
Nonius KappaCCD diffractometer | 14253 independent reflections |
Radiation source: fine-focus sealed tube | 12656 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.077 |
ϕ and ω scans | θmax = 30.1°, θmin = 3.2° |
Absorption correction: integration Gaussian (Coppens, 1970) implemented in maXus (1999) | h = −25→25 |
Tmin = 0.029, Tmax = 0.193 | k = −12→10 |
129999 measured reflections | l = −44→44 |
Refinement on F | 0 restraints |
Least-squares matrix: full | 0 constraints |
R[F2 > 2σ(F2)] = 0.042 | H-atom parameters not refined |
wR(F2) = 0.054 | Weighting scheme based on measured s.u.'s w = 1/[σ2(Fo) + 0.00040|Fo|2] |
S = 2.40 | (Δ/σ)max = 0.032 |
12656 reflections | Δρmax = 3.35 e Å−3 |
649 parameters | Δρmin = −2.86 e Å−3 |
[W2Ir2(C6H7)2(CO)10] | V = 4886.75 (6) Å3 |
Mr = 1190.49 | Z = 8 |
Monoclinic, P21/n | Mo Kα radiation |
a = 18.3035 (1) Å | µ = 20.34 mm−1 |
b = 8.5629 (1) Å | T = 200 K |
c = 31.2876 (2) Å | 0.40 × 0.20 × 0.15 mm |
β = 94.7702 (4)° |
Nonius KappaCCD diffractometer | 14253 independent reflections |
Absorption correction: integration Gaussian (Coppens, 1970) implemented in maXus (1999) | 12656 reflections with I > 2σ(I) |
Tmin = 0.029, Tmax = 0.193 | Rint = 0.077 |
129999 measured reflections |
R[F2 > 2σ(F2)] = 0.042 | 0 restraints |
wR(F2) = 0.054 | H-atom parameters not refined |
S = 2.40 | Δρmax = 3.35 e Å−3 |
12656 reflections | Δρmin = −2.86 e Å−3 |
649 parameters |
Refinement. There are two independent C22 H14 Ir2 O10 W2 molecules in the crystallographic asymmetric unit. H atoms were included in the refinement at idealized positions which were frequently recalculated. |
x | y | z | Uiso*/Ueq | ||
Ir1 | 0.56524 (2) | 0.31024 (3) | 0.346149 (9) | 0.02105 (7) | |
Ir2 | 0.64578 (2) | 0.05483 (3) | 0.327935 (9) | 0.02159 (7) | |
Ir5 | 0.24298 (2) | 0.05311 (4) | 0.09590 (1) | 0.02709 (8) | |
Ir6 | 0.26744 (2) | −0.20304 (4) | 0.14688 (1) | 0.02679 (8) | |
W3 | 0.62643 (2) | 0.12848 (4) | 0.414546 (9) | 0.02057 (8) | |
W4 | 0.72109 (2) | 0.32363 (4) | 0.362323 (9) | 0.02030 (7) | |
W7 | 0.36056 (2) | −0.14311 (4) | 0.08069 (1) | 0.02391 (8) | |
W8 | 0.36385 (2) | 0.05680 (4) | 0.15998 (1) | 0.02461 (8) | |
O11 | 0.5062 (4) | 0.5362 (8) | 0.4090 (2) | 0.051 (2) | |
O12 | 0.4335 (4) | 0.0952 (8) | 0.3361 (2) | 0.044 (2) | |
O13 | 0.5345 (4) | 0.4946 (8) | 0.2618 (2) | 0.046 (2) | |
O21 | 0.7802 (4) | −0.1525 (8) | 0.3349 (2) | 0.049 (2) | |
O22 | 0.5335 (4) | −0.2103 (8) | 0.3251 (2) | 0.049 (2) | |
O23 | 0.6389 (4) | 0.1390 (8) | 0.2332 (2) | 0.051 (2) | |
O31 | 0.6904 (3) | 0.4130 (7) | 0.4662 (2) | 0.033 (2) | |
O32 | 0.7721 (4) | −0.0572 (7) | 0.4331 (2) | 0.042 (2) | |
O41 | 0.6635 (4) | 0.6530 (7) | 0.3854 (2) | 0.039 (2) | |
O42 | 0.7041 (4) | 0.4409 (8) | 0.2675 (2) | 0.046 (2) | |
O51 | 0.2962 (4) | 0.2713 (8) | 0.0280 (2) | 0.057 (2) | |
O52 | 0.1381 (4) | −0.1523 (7) | 0.0406 (2) | 0.048 (2) | |
O53 | 0.1250 (4) | 0.2390 (9) | 0.1376 (3) | 0.065 (3) | |
O61 | 0.3621 (4) | −0.4158 (8) | 0.2063 (2) | 0.052 (2) | |
O62 | 0.1878 (4) | −0.4614 (8) | 0.0953 (2) | 0.055 (2) | |
O63 | 0.1489 (4) | −0.1173 (9) | 0.2061 (2) | 0.057 (2) | |
O71 | 0.4749 (4) | 0.1224 (8) | 0.0748 (2) | 0.050 (2) | |
O72 | 0.4791 (4) | −0.3240 (7) | 0.1390 (2) | 0.039 (2) | |
O81 | 0.3560 (4) | 0.3847 (7) | 0.1187 (2) | 0.044 (2) | |
O82 | 0.2421 (4) | 0.1794 (9) | 0.2154 (2) | 0.052 (2) | |
C11 | 0.5299 (5) | 0.455 (1) | 0.3856 (3) | 0.031 (2) | |
C12 | 0.4839 (5) | 0.173 (1) | 0.3402 (3) | 0.029 (2) | |
C13 | 0.5474 (5) | 0.4262 (9) | 0.2926 (3) | 0.030 (2) | |
C21 | 0.7294 (5) | −0.073 (1) | 0.3334 (3) | 0.032 (2) | |
C22 | 0.5743 (5) | −0.111 (1) | 0.3279 (3) | 0.033 (2) | |
C23 | 0.6427 (5) | 0.109 (1) | 0.2690 (2) | 0.030 (2) | |
C31 | 0.6702 (4) | 0.3151 (9) | 0.4426 (2) | 0.022 (2) | |
C32 | 0.7209 (5) | 0.012 (1) | 0.4249 (3) | 0.033 (2) | |
C41 | 0.6794 (5) | 0.530 (1) | 0.3763 (3) | 0.030 (2) | |
C42 | 0.7055 (5) | 0.389 (1) | 0.3011 (3) | 0.032 (2) | |
C51 | 0.2748 (5) | 0.190 (1) | 0.0544 (3) | 0.033 (2) | |
C52 | 0.1775 (5) | −0.076 (1) | 0.0619 (3) | 0.036 (2) | |
C53 | 0.1712 (5) | 0.171 (1) | 0.1236 (3) | 0.038 (3) | |
C61 | 0.3264 (5) | −0.333 (1) | 0.1843 (3) | 0.034 (2) | |
C62 | 0.2202 (6) | −0.362 (1) | 0.1124 (3) | 0.036 (2) | |
C63 | 0.1951 (6) | −0.145 (1) | 0.1854 (3) | 0.041 (3) | |
C71 | 0.4292 (5) | 0.032 (1) | 0.0821 (3) | 0.037 (2) | |
C72 | 0.4322 (5) | −0.252 (1) | 0.1198 (3) | 0.030 (2) | |
C81 | 0.3552 (5) | 0.2605 (9) | 0.1309 (3) | 0.030 (2) | |
C82 | 0.2834 (5) | 0.130 (1) | 0.1936 (3) | 0.044 (3) | |
C301 | 0.5522 (5) | 0.148 (1) | 0.4727 (3) | 0.030 (2) | |
C302 | 0.5051 (5) | 0.104 (1) | 0.4378 (3) | 0.031 (2) | |
C303 | 0.5272 (5) | −0.043 (1) | 0.4234 (3) | 0.035 (2) | |
C304 | 0.5910 (6) | −0.090 (1) | 0.4499 (3) | 0.036 (2) | |
C305 | 0.6057 (5) | 0.0290 (9) | 0.4805 (2) | 0.027 (2) | |
C311 | 0.5461 (6) | 0.291 (1) | 0.5008 (3) | 0.041 (3) | |
C401 | 0.8390 (4) | 0.296 (1) | 0.3409 (3) | 0.028 (2) | |
C402 | 0.8354 (5) | 0.195 (1) | 0.3767 (3) | 0.034 (2) | |
C403 | 0.8249 (5) | 0.285 (1) | 0.4129 (3) | 0.040 (3) | |
C404 | 0.8209 (4) | 0.445 (1) | 0.4004 (3) | 0.033 (2) | |
C405 | 0.8300 (4) | 0.449 (1) | 0.3554 (3) | 0.028 (2) | |
C411 | 0.8602 (5) | 0.240 (1) | 0.2974 (3) | 0.043 (3) | |
C701 | 0.4267 (5) | −0.257 (1) | 0.0267 (3) | 0.035 (2) | |
C702 | 0.3764 (6) | −0.367 (1) | 0.0414 (3) | 0.037 (2) | |
C703 | 0.3036 (6) | −0.317 (1) | 0.0289 (3) | 0.043 (3) | |
C704 | 0.3081 (5) | −0.173 (1) | 0.0086 (3) | 0.035 (2) | |
C705 | 0.3819 (6) | −0.137 (1) | 0.0079 (3) | 0.041 (3) | |
C711 | 0.5064 (6) | −0.267 (1) | 0.0287 (3) | 0.051 (3) | |
C801 | 0.4786 (5) | 0.172 (1) | 0.1819 (3) | 0.033 (2) | |
C802 | 0.4302 (5) | 0.183 (1) | 0.2154 (3) | 0.037 (2) | |
C803 | 0.4125 (5) | 0.031 (1) | 0.2308 (3) | 0.037 (2) | |
C804 | 0.4515 (5) | −0.072 (1) | 0.2059 (3) | 0.039 (3) | |
C805 | 0.4921 (5) | 0.013 (1) | 0.1766 (3) | 0.030 (2) | |
C811 | 0.5166 (6) | 0.303 (1) | 0.1624 (3) | 0.044 (3) | |
H302 | 0.4646 | 0.1630 | 0.4257 | 0.037* | |
H303 | 0.5040 | −0.1013 | 0.4002 | 0.042* | |
H304 | 0.6183 | −0.1830 | 0.4473 | 0.043* | |
H305 | 0.6446 | 0.0293 | 0.5026 | 0.033* | |
H311b | 0.5068 | 0.3550 | 0.4892 | 0.050* | |
H311a | 0.5372 | 0.2597 | 0.5290 | 0.050* | |
H311c | 0.5906 | 0.3490 | 0.5017 | 0.050* | |
H402 | 0.8394 | 0.0846 | 0.3761 | 0.041* | |
H403 | 0.8212 | 0.2463 | 0.4411 | 0.047* | |
H404 | 0.8136 | 0.5320 | 0.4184 | 0.040* | |
H405 | 0.8300 | 0.5403 | 0.3382 | 0.034* | |
H411a | 0.9112 | 0.2175 | 0.2993 | 0.051* | |
H411b | 0.8495 | 0.3195 | 0.2767 | 0.051* | |
H411c | 0.8333 | 0.1485 | 0.2893 | 0.051* | |
H702 | 0.3893 | −0.4595 | 0.0572 | 0.044* | |
H703 | 0.2598 | −0.3724 | 0.0335 | 0.052* | |
H704 | 0.2680 | −0.1115 | −0.0027 | 0.042* | |
H705 | 0.3999 | −0.0431 | −0.0037 | 0.049* | |
H711c | 0.5236 | −0.3336 | 0.0517 | 0.061* | |
H711a | 0.5208 | −0.3081 | 0.0025 | 0.061* | |
H711b | 0.5268 | −0.1658 | 0.0333 | 0.061* | |
H802 | 0.4122 | 0.2784 | 0.2261 | 0.044* | |
H803 | 0.3816 | 0.0056 | 0.2528 | 0.045* | |
H804 | 0.4508 | −0.1824 | 0.2084 | 0.047* | |
H805 | 0.5229 | −0.0312 | 0.1568 | 0.036* | |
H811c | 0.4826 | 0.3845 | 0.1553 | 0.052* | |
H811a | 0.5546 | 0.3407 | 0.1822 | 0.052* | |
H811b | 0.5370 | 0.2678 | 0.1372 | 0.052* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ir1 | 0.0205 (1) | 0.0206 (1) | 0.0218 (1) | 0.0012 (1) | 0.0001 (1) | 0.0003 (1) |
Ir2 | 0.0245 (2) | 0.0195 (1) | 0.0209 (1) | 0.0001 (1) | 0.0025 (1) | −0.0025 (1) |
Ir5 | 0.0261 (2) | 0.0230 (2) | 0.0308 (2) | 0.0010 (1) | −0.0059 (1) | 0.0018 (1) |
Ir6 | 0.0285 (2) | 0.0236 (2) | 0.0281 (2) | −0.0032 (1) | 0.0010 (1) | 0.0033 (1) |
W3 | 0.0230 (2) | 0.0203 (2) | 0.0185 (1) | −0.0009 (1) | 0.0025 (1) | 0.0013 (1) |
W4 | 0.0203 (2) | 0.0214 (2) | 0.0192 (1) | −0.0022 (1) | 0.0011 (1) | 0.0005 (1) |
W7 | 0.0255 (2) | 0.0221 (2) | 0.0234 (2) | −0.0015 (1) | −0.0021 (1) | 0.0015 (1) |
W8 | 0.0256 (2) | 0.0223 (2) | 0.0250 (2) | −0.0010 (1) | −0.0034 (1) | −0.0002 (1) |
O11 | 0.061 (5) | 0.043 (4) | 0.051 (4) | 0.012 (4) | 0.016 (4) | −0.017 (3) |
O12 | 0.030 (3) | 0.038 (3) | 0.063 (5) | −0.008 (3) | −0.010 (3) | −0.007 (3) |
O13 | 0.057 (4) | 0.051 (4) | 0.028 (3) | −0.002 (4) | −0.009 (3) | 0.012 (3) |
O21 | 0.041 (4) | 0.040 (4) | 0.070 (5) | 0.020 (3) | 0.017 (4) | 0.008 (4) |
O22 | 0.048 (4) | 0.032 (3) | 0.067 (5) | −0.019 (3) | −0.002 (4) | −0.010 (3) |
O23 | 0.064 (5) | 0.054 (4) | 0.035 (4) | 0.000 (4) | −0.002 (3) | 0.001 (3) |
O31 | 0.042 (4) | 0.037 (3) | 0.019 (3) | −0.018 (3) | 0.001 (2) | −0.001 (2) |
O32 | 0.040 (4) | 0.047 (4) | 0.038 (4) | 0.018 (3) | 0.003 (3) | 0.025 (3) |
O41 | 0.041 (4) | 0.019 (3) | 0.057 (4) | −0.002 (3) | 0.007 (3) | 0.001 (3) |
O42 | 0.042 (4) | 0.074 (5) | 0.023 (3) | −0.007 (4) | 0.002 (3) | 0.018 (3) |
O51 | 0.073 (6) | 0.045 (4) | 0.050 (4) | −0.017 (4) | −0.016 (4) | −0.002 (4) |
O52 | 0.051 (4) | 0.036 (4) | 0.054 (4) | −0.003 (3) | −0.022 (4) | 0.000 (3) |
O53 | 0.047 (5) | 0.054 (5) | 0.095 (7) | 0.017 (4) | 0.009 (4) | −0.019 (5) |
O61 | 0.057 (5) | 0.047 (4) | 0.050 (4) | 0.004 (4) | −0.007 (4) | 0.022 (4) |
O62 | 0.068 (5) | 0.035 (4) | 0.060 (5) | −0.019 (4) | −0.007 (4) | −0.009 (3) |
O63 | 0.049 (5) | 0.064 (5) | 0.059 (5) | −0.007 (4) | 0.019 (4) | −0.013 (4) |
O71 | 0.061 (5) | 0.049 (4) | 0.041 (4) | −0.016 (4) | 0.003 (3) | 0.006 (3) |
O72 | 0.038 (4) | 0.033 (3) | 0.043 (4) | 0.011 (3) | −0.011 (3) | 0.006 (3) |
O81 | 0.055 (5) | 0.026 (3) | 0.050 (4) | −0.004 (3) | −0.010 (3) | 0.002 (3) |
O82 | 0.042 (4) | 0.072 (5) | 0.043 (4) | −0.006 (4) | 0.009 (3) | −0.018 (4) |
C11 | 0.033 (5) | 0.035 (5) | 0.026 (4) | 0.000 (4) | 0.002 (3) | 0.000 (4) |
C12 | 0.029 (4) | 0.032 (4) | 0.026 (4) | −0.001 (4) | 0.001 (3) | 0.003 (3) |
C13 | 0.029 (4) | 0.024 (4) | 0.035 (5) | 0.003 (3) | −0.006 (4) | −0.005 (4) |
C21 | 0.031 (5) | 0.027 (4) | 0.039 (5) | −0.004 (4) | 0.008 (4) | −0.001 (4) |
C22 | 0.036 (5) | 0.033 (5) | 0.029 (4) | 0.007 (4) | 0.005 (4) | −0.009 (4) |
C23 | 0.040 (5) | 0.029 (4) | 0.020 (4) | 0.007 (4) | −0.001 (3) | −0.005 (3) |
C31 | 0.028 (4) | 0.021 (4) | 0.017 (3) | −0.001 (3) | 0.004 (3) | 0.001 (3) |
C32 | 0.045 (5) | 0.023 (4) | 0.033 (5) | 0.001 (4) | 0.015 (4) | 0.007 (4) |
C41 | 0.033 (5) | 0.029 (4) | 0.029 (4) | −0.005 (4) | 0.001 (3) | 0.004 (3) |
C42 | 0.028 (4) | 0.033 (5) | 0.034 (5) | −0.009 (4) | −0.001 (4) | 0.009 (4) |
C51 | 0.037 (5) | 0.030 (4) | 0.031 (4) | −0.003 (4) | −0.009 (4) | −0.001 (4) |
C52 | 0.029 (5) | 0.035 (5) | 0.044 (5) | 0.002 (4) | −0.011 (4) | 0.002 (4) |
C53 | 0.033 (5) | 0.031 (5) | 0.051 (6) | 0.004 (4) | 0.004 (4) | 0.004 (4) |
C61 | 0.037 (5) | 0.035 (5) | 0.032 (5) | 0.002 (4) | 0.007 (4) | 0.013 (4) |
C62 | 0.053 (6) | 0.022 (4) | 0.034 (5) | 0.001 (4) | 0.002 (4) | −0.001 (4) |
C63 | 0.041 (6) | 0.037 (5) | 0.046 (6) | −0.013 (4) | 0.009 (5) | −0.002 (4) |
C71 | 0.028 (5) | 0.031 (5) | 0.050 (6) | −0.008 (4) | −0.012 (4) | 0.005 (4) |
C72 | 0.030 (4) | 0.027 (4) | 0.031 (4) | 0.001 (4) | −0.005 (3) | −0.009 (4) |
C81 | 0.040 (5) | 0.022 (4) | 0.026 (4) | 0.004 (4) | −0.009 (3) | 0.002 (3) |
C82 | 0.030 (5) | 0.067 (7) | 0.033 (5) | −0.008 (5) | 0.004 (4) | −0.017 (5) |
C301 | 0.033 (5) | 0.032 (4) | 0.025 (4) | −0.009 (4) | 0.007 (3) | 0.002 (3) |
C302 | 0.028 (4) | 0.040 (5) | 0.028 (4) | −0.003 (4) | 0.013 (3) | −0.002 (4) |
C303 | 0.053 (6) | 0.031 (5) | 0.023 (4) | −0.010 (4) | 0.018 (4) | −0.008 (3) |
C304 | 0.061 (6) | 0.020 (4) | 0.029 (4) | 0.002 (4) | 0.011 (4) | 0.000 (3) |
C305 | 0.034 (4) | 0.029 (4) | 0.020 (4) | −0.001 (4) | 0.005 (3) | 0.006 (3) |
C311 | 0.046 (6) | 0.042 (5) | 0.039 (5) | −0.017 (5) | 0.018 (4) | −0.007 (4) |
C401 | 0.009 (3) | 0.039 (5) | 0.035 (4) | −0.004 (3) | 0.002 (3) | −0.005 (4) |
C402 | 0.016 (4) | 0.040 (5) | 0.046 (5) | −0.001 (4) | 0.003 (4) | −0.006 (4) |
C403 | 0.020 (4) | 0.065 (7) | 0.033 (5) | −0.005 (4) | 0.001 (3) | 0.003 (5) |
C404 | 0.020 (4) | 0.050 (6) | 0.029 (4) | −0.011 (4) | 0.001 (3) | −0.003 (4) |
C405 | 0.017 (4) | 0.037 (5) | 0.029 (4) | −0.012 (3) | −0.002 (3) | −0.007 (3) |
C411 | 0.040 (5) | 0.041 (5) | 0.050 (6) | 0.001 (5) | 0.016 (4) | −0.010 (5) |
C701 | 0.041 (5) | 0.026 (4) | 0.037 (5) | −0.001 (4) | −0.001 (4) | −0.011 (4) |
C702 | 0.050 (6) | 0.039 (5) | 0.022 (4) | −0.001 (4) | 0.005 (4) | −0.008 (4) |
C703 | 0.045 (6) | 0.049 (6) | 0.037 (5) | −0.014 (5) | 0.006 (4) | −0.006 (4) |
C704 | 0.044 (5) | 0.032 (4) | 0.028 (4) | 0.014 (4) | −0.005 (4) | −0.006 (4) |
C705 | 0.055 (6) | 0.039 (5) | 0.028 (4) | −0.016 (5) | −0.003 (4) | 0.005 (4) |
C711 | 0.044 (6) | 0.066 (7) | 0.044 (6) | 0.017 (6) | 0.007 (5) | 0.004 (5) |
C801 | 0.034 (5) | 0.026 (4) | 0.037 (5) | −0.003 (4) | −0.011 (4) | 0.008 (4) |
C802 | 0.035 (5) | 0.043 (5) | 0.032 (5) | 0.005 (4) | −0.011 (4) | −0.018 (4) |
C803 | 0.038 (5) | 0.044 (5) | 0.028 (4) | −0.005 (4) | −0.010 (4) | −0.006 (4) |
C804 | 0.043 (5) | 0.033 (5) | 0.038 (5) | −0.004 (4) | −0.022 (4) | 0.012 (4) |
C805 | 0.027 (4) | 0.033 (4) | 0.029 (4) | 0.000 (4) | −0.009 (3) | −0.007 (4) |
C811 | 0.043 (6) | 0.032 (5) | 0.055 (6) | −0.009 (4) | 0.000 (5) | 0.002 (4) |
Ir1—Ir2 | 2.7242 (4) | O51—C51 | 1.17 (1) |
Ir1—W3 | 2.8032 (4) | O52—C52 | 1.14 (1) |
Ir1—W4 | 2.8577 (4) | O53—C53 | 1.14 (1) |
Ir1—C11 | 1.898 (9) | O61—C61 | 1.15 (1) |
Ir1—C12 | 1.893 (9) | O62—C62 | 1.15 (1) |
Ir1—C13 | 1.952 (9) | O63—C63 | 1.13 (1) |
Ir2—W3 | 2.8330 (4) | O71—C71 | 1.17 (1) |
Ir2—W4 | 2.8476 (4) | O72—C72 | 1.18 (1) |
Ir2—C21 | 1.876 (9) | O81—C81 | 1.131 (9) |
Ir2—C22 | 1.929 (9) | O82—C82 | 1.14 (1) |
Ir2—C23 | 1.897 (8) | C301—C302 | 1.38 (1) |
Ir5—Ir6 | 2.7271 (4) | C301—C305 | 1.42 (1) |
Ir5—W7 | 2.8021 (5) | C301—C311 | 1.52 (1) |
Ir5—W8 | 2.8596 (4) | C302—C303 | 1.41 (1) |
Ir5—C51 | 1.875 (9) | C302—H302 | 0.95 |
Ir5—C52 | 1.893 (9) | C303—C304 | 1.43 (1) |
Ir5—C53 | 1.918 (9) | C303—H303 | 0.95 |
Ir6—W7 | 2.8363 (5) | C304—C305 | 1.41 (1) |
Ir6—W8 | 2.8482 (4) | C304—H304 | 0.95 |
Ir6—C61 | 1.888 (9) | C305—H305 | 0.95 |
Ir6—C62 | 1.898 (9) | C311—H311b | 0.95 |
Ir6—C63 | 1.93 (1) | C311—H311a | 0.95 |
W3—W4 | 2.9891 (4) | C311—H311c | 0.95 |
W3—C31 | 1.962 (7) | C401—C402 | 1.42 (1) |
W3—C32 | 2.001 (9) | C401—C405 | 1.40 (1) |
W3—C301 | 2.365 (8) | C401—C411 | 1.52 (1) |
W3—C302 | 2.403 (8) | C402—C403 | 1.40 (1) |
W3—C303 | 2.370 (9) | C402—H402 | 0.95 |
W3—C304 | 2.291 (9) | C403—C404 | 1.42 (1) |
W3—C305 | 2.294 (7) | C403—H403 | 0.95 |
W4—C41 | 1.989 (9) | C404—C405 | 1.43 (1) |
W4—C42 | 1.994 (9) | C404—H404 | 0.95 |
W4—C401 | 2.326 (7) | C405—H405 | 0.95 |
W4—C402 | 2.373 (9) | C411—H411a | 0.95 |
W4—C403 | 2.393 (9) | C411—H411b | 0.95 |
W4—C404 | 2.340 (8) | C411—H411c | 0.95 |
W4—C405 | 2.290 (7) | C701—C702 | 1.42 (1) |
W7—W8 | 3.0108 (4) | C701—C705 | 1.42 (1) |
W7—C71 | 1.955 (9) | C701—C711 | 1.46 (1) |
W7—C72 | 1.955 (8) | C702—C703 | 1.42 (1) |
W7—C701 | 2.369 (9) | C702—H702 | 0.95 |
W7—C702 | 2.309 (8) | C703—C704 | 1.39 (1) |
W7—C703 | 2.379 (9) | C703—H703 | 0.95 |
W7—C704 | 2.391 (9) | C704—C705 | 1.39 (1) |
W7—C705 | 2.343 (9) | C704—H704 | 0.95 |
W8—C81 | 1.967 (8) | C705—H705 | 0.95 |
W8—C82 | 1.982 (9) | C711—H711c | 0.95 |
W8—C801 | 2.369 (9) | C711—H711a | 0.95 |
W8—C802 | 2.303 (8) | C711—H711b | 0.95 |
W8—C803 | 2.329 (8) | C801—C802 | 1.43 (1) |
W8—C804 | 2.338 (8) | C801—C805 | 1.40 (1) |
W8—C805 | 2.391 (8) | C801—C811 | 1.48 (1) |
O11—C11 | 1.12 (1) | C802—C803 | 1.43 (1) |
O12—C12 | 1.14 (1) | C802—H802 | 0.95 |
O13—C13 | 1.14 (1) | C803—C804 | 1.41 (1) |
O21—C21 | 1.15 (1) | C803—H803 | 0.95 |
O22—C22 | 1.13 (1) | C804—C805 | 1.43 (1) |
O23—C23 | 1.15 (1) | C804—H804 | 0.95 |
O31—C31 | 1.157 (9) | C805—H805 | 0.95 |
O32—C32 | 1.12 (1) | C811—H811c | 0.95 |
O41—C41 | 1.13 (1) | C811—H811a | 0.95 |
O42—C42 | 1.14 (1) | C811—H811b | 0.95 |
O11···O53i | 3.21 (1) | O41···C22iii | 3.08 (1) |
O11···C311ii | 3.40 (1) | O41···C21iii | 3.15 (1) |
O11···O22iii | 3.47 (1) | O41···C304iii | 3.34 (1) |
O11···C53i | 3.52 (1) | O41···C32iii | 3.44 (1) |
O11···O52i | 3.57 (1) | O42···C411v | 3.42 (1) |
O12···O63i | 3.12 (1) | O42···C23v | 3.43 (1) |
O12···O62i | 3.25 (1) | O42···C21v | 3.48 (1) |
O12···C63i | 3.26 (1) | O51···C702iii | 3.44 (1) |
O12···C803 | 3.33 (1) | O51···C31x | 3.46 (1) |
O12···O53iv | 3.36 (1) | O51···C703iii | 3.52 (1) |
O12···C62i | 3.38 (1) | O52···C302iv | 3.46 (1) |
O13···O22iii | 3.21 (1) | O52···C311iv | 3.54 (1) |
O13···C411v | 3.49 (1) | O53···O62iii | 3.15 (1) |
O13···C811 | 3.51 (1) | O61···O81vi | 3.22 (1) |
O13···C802 | 3.52 (1) | O61···O63iv | 3.26 (1) |
O13···O61iii | 3.56 (1) | O61···O82iv | 3.33 (1) |
O21···O41vi | 3.225 (9) | O62···C53vi | 3.29 (1) |
O21···O23vii | 3.23 (1) | O62···O81vi | 3.37 (1) |
O21···O42vii | 3.34 (1) | O63···C12iv | 3.26 (1) |
O21···C405vi | 3.58 (1) | O63···C802iv | 3.41 (1) |
O21···C41vi | 3.59 (1) | O63···O82iv | 3.50 (1) |
O22···O41vi | 3.14 (1) | O71···C711xi | 3.51 (1) |
O22···O53iv | 3.25 (1) | O72···C811vi | 3.34 (1) |
O22···C13vi | 3.29 (1) | O72···O81vi | 3.385 (9) |
O22···C11vi | 3.44 (1) | O72···C411vii | 3.45 (1) |
O23···C801 | 3.24 (1) | O72···C402vii | 3.47 (1) |
O23···C805 | 3.28 (1) | O72···C401vii | 3.49 (1) |
O23···C405vii | 3.30 (1) | O81···C61iii | 3.25 (1) |
O23···C811 | 3.33 (1) | O81···C702iii | 3.26 (1) |
O23···O42vii | 3.34 (1) | O81···C62iii | 3.29 (1) |
O23···C411vii | 3.55 (1) | O81···C72iii | 3.41 (1) |
O31···O51viii | 3.060 (9) | O82···C61i | 3.47 (1) |
O31···C51viii | 3.17 (1) | O82···C63i | 3.55 (1) |
O31···C704viii | 3.30 (1) | C302···C305xii | 3.58 (1) |
O31···O52viii | 3.303 (9) | C303···C311xii | 3.53 (1) |
O31···C52viii | 3.33 (1) | C304···C311xii | 3.51 (1) |
O32···C703ix | 3.19 (1) | C403···C711v | 3.48 (1) |
O32···C704ix | 3.33 (1) | C405···C805v | 3.53 (1) |
O32···O41vi | 3.439 (9) | ||
Ir2—Ir1—W3 | 61.65 (1) | Ir5—W8—C804 | 151.3 (2) |
Ir2—Ir1—W4 | 61.29 (1) | Ir5—W8—C805 | 147.0 (2) |
Ir2—Ir1—C11 | 151.5 (3) | Ir6—W8—W7 | 57.83 (1) |
Ir2—Ir1—C12 | 85.2 (3) | Ir6—W8—C81 | 127.0 (2) |
Ir2—Ir1—C13 | 106.5 (2) | Ir6—W8—C82 | 81.1 (3) |
W3—Ir1—W4 | 63.74 (1) | Ir6—W8—C801 | 152.9 (2) |
W3—Ir1—C11 | 90.1 (3) | Ir6—W8—C802 | 139.2 (3) |
W3—Ir1—C12 | 89.5 (2) | Ir6—W8—C803 | 104.2 (2) |
W3—Ir1—C13 | 164.9 (3) | Ir6—W8—C804 | 96.1 (2) |
W4—Ir1—C11 | 104.4 (3) | Ir6—W8—C805 | 119.6 (2) |
W4—Ir1—C12 | 143.9 (3) | W7—W8—C81 | 97.4 (2) |
W4—Ir1—C13 | 103.0 (3) | W7—W8—C82 | 130.8 (3) |
C11—Ir1—C12 | 99.2 (4) | W7—W8—C801 | 115.5 (2) |
C11—Ir1—C13 | 100.7 (3) | W7—W8—C802 | 149.4 (2) |
C12—Ir1—C13 | 99.0 (3) | W7—W8—C803 | 135.2 (2) |
Ir1—Ir2—W3 | 60.55 (1) | W7—W8—C804 | 101.8 (2) |
Ir1—Ir2—W4 | 61.67 (1) | W7—W8—C805 | 92.4 (2) |
Ir1—Ir2—C21 | 154.1 (3) | C81—W8—C82 | 85.9 (4) |
Ir1—Ir2—C22 | 102.2 (2) | C81—W8—C801 | 78.5 (3) |
Ir1—Ir2—C23 | 92.1 (2) | C81—W8—C802 | 87.1 (3) |
W3—Ir2—W4 | 63.50 (1) | C81—W8—C803 | 122.2 (3) |
W3—Ir2—C21 | 102.0 (3) | C81—W8—C804 | 136.6 (3) |
W3—Ir2—C22 | 91.5 (2) | C81—W8—C805 | 106.2 (3) |
W3—Ir2—C23 | 151.6 (2) | C82—W8—C801 | 113.2 (4) |
W4—Ir2—C21 | 94.0 (3) | C82—W8—C802 | 79.6 (4) |
W4—Ir2—C22 | 154.4 (2) | C82—W8—C803 | 76.5 (4) |
W4—Ir2—C23 | 98.4 (3) | C82—W8—C804 | 108.9 (4) |
C21—Ir2—C22 | 96.9 (4) | C82—W8—C805 | 133.9 (3) |
C21—Ir2—C23 | 100.8 (4) | C801—W8—C802 | 35.7 (3) |
C22—Ir2—C23 | 102.2 (4) | C801—W8—C803 | 60.3 (3) |
Ir6—Ir5—W7 | 61.71 (1) | C801—W8—C804 | 58.1 (3) |
Ir6—Ir5—W8 | 61.25 (1) | C801—W8—C805 | 34.1 (3) |
Ir6—Ir5—C51 | 149.4 (3) | C802—W8—C803 | 36.1 (3) |
Ir6—Ir5—C52 | 85.7 (3) | C802—W8—C804 | 57.7 (3) |
Ir6—Ir5—C53 | 104.1 (3) | C802—W8—C805 | 57.6 (3) |
W7—Ir5—W8 | 64.24 (1) | C803—W8—C804 | 35.1 (3) |
W7—Ir5—C51 | 88.2 (3) | C803—W8—C805 | 59.2 (3) |
W7—Ir5—C52 | 90.8 (3) | C804—W8—C805 | 35.1 (3) |
W7—Ir5—C53 | 162.9 (3) | Ir1—C11—O11 | 176.9 (8) |
W8—Ir5—C51 | 102.3 (3) | Ir1—C12—O12 | 177.5 (8) |
W8—Ir5—C52 | 144.9 (3) | Ir1—C13—O13 | 177.6 (8) |
W8—Ir5—C53 | 101.3 (3) | Ir2—C21—O21 | 176.9 (8) |
C51—Ir5—C52 | 101.1 (4) | Ir2—C22—O22 | 175.4 (8) |
C51—Ir5—C53 | 104.5 (4) | Ir2—C23—O23 | 178.0 (8) |
C52—Ir5—C53 | 97.7 (4) | W3—C31—O31 | 166.5 (6) |
Ir5—Ir6—W7 | 60.45 (1) | W3—C32—O32 | 175.6 (7) |
Ir5—Ir6—W8 | 61.67 (1) | W4—C41—O41 | 172.3 (8) |
Ir5—Ir6—C61 | 153.4 (3) | W4—C42—O42 | 170.4 (8) |
Ir5—Ir6—C62 | 101.5 (3) | Ir5—C51—O51 | 177.9 (8) |
Ir5—Ir6—C63 | 94.1 (3) | Ir5—C52—O52 | 178.7 (9) |
W7—Ir6—W8 | 63.96 (1) | Ir5—C53—O53 | 175.2 (9) |
W7—Ir6—C61 | 102.3 (3) | Ir6—C61—O61 | 177.9 (9) |
W7—Ir6—C62 | 89.3 (3) | Ir6—C62—O62 | 172.8 (9) |
W7—Ir6—C63 | 153.7 (3) | Ir6—C63—O63 | 175.0 (9) |
W8—Ir6—C61 | 93.2 (3) | W7—C71—O71 | 165.3 (9) |
W8—Ir6—C62 | 152.7 (3) | W7—C72—O72 | 171.8 (7) |
W8—Ir6—C63 | 99.2 (3) | W8—C81—O81 | 171.0 (7) |
C61—Ir6—C62 | 98.1 (4) | W8—C82—O82 | 173.6 (8) |
C61—Ir6—C63 | 98.6 (4) | W3—C301—C302 | 74.6 (5) |
C62—Ir6—C63 | 103.6 (4) | W3—C301—C305 | 69.5 (4) |
Ir1—W3—Ir2 | 57.80 (1) | W3—C301—C311 | 125.2 (6) |
Ir1—W3—W4 | 59.02 (1) | C302—C301—C305 | 108.3 (8) |
Ir1—W3—C31 | 90.7 (2) | C302—C301—C311 | 127.3 (9) |
Ir1—W3—C32 | 133.4 (2) | C305—C301—C311 | 124.2 (8) |
Ir1—W3—C301 | 109.2 (2) | W3—C302—C301 | 71.6 (5) |
Ir1—W3—C302 | 87.7 (2) | W3—C302—C303 | 71.6 (5) |
Ir1—W3—C303 | 99.9 (2) | W3—C302—H302 | 122.8 |
Ir1—W3—C304 | 135.2 (3) | C301—C302—C303 | 108.7 (8) |
Ir1—W3—C305 | 143.9 (2) | C301—C302—H302 | 125.7 |
Ir2—W3—W4 | 58.49 (1) | C303—C302—H302 | 125.7 |
Ir2—W3—C31 | 122.0 (2) | W3—C303—C302 | 74.1 (5) |
Ir2—W3—C32 | 82.5 (2) | W3—C303—C304 | 69.1 (5) |
Ir2—W3—C301 | 151.3 (2) | W3—C303—H303 | 122.3 |
Ir2—W3—C302 | 117.6 (2) | C302—C303—C304 | 107.7 (8) |
Ir2—W3—C303 | 97.6 (2) | C302—C303—H303 | 126.1 |
Ir2—W3—C304 | 110.1 (2) | C304—C303—H303 | 126.1 |
Ir2—W3—C305 | 145.2 (2) | W3—C304—C303 | 75.2 (5) |
W4—W3—C31 | 63.6 (2) | W3—C304—C305 | 72.2 (5) |
W4—W3—C32 | 80.5 (2) | W3—C304—H304 | 118.2 |
W4—W3—C301 | 141.0 (2) | C303—C304—C305 | 107.2 (7) |
W4—W3—C302 | 143.8 (2) | C303—C304—H304 | 126.4 |
W4—W3—C303 | 153.5 (2) | C305—C304—H304 | 126.4 |
W4—W3—C304 | 156.9 (2) | W3—C305—C301 | 75.0 (4) |
W4—W3—C305 | 147.8 (2) | W3—C305—C304 | 72.0 (5) |
C31—W3—C32 | 91.1 (3) | W3—C305—H305 | 118.9 |
C31—W3—C301 | 80.6 (3) | C301—C305—C304 | 108.1 (7) |
C31—W3—C302 | 106.8 (3) | C301—C305—H305 | 126.0 |
C31—W3—C303 | 137.8 (3) | C304—C305—H305 | 126.0 |
C31—W3—C304 | 124.7 (3) | C301—C311—H311b | 109.5 |
C31—W3—C305 | 89.5 (3) | C301—C311—H311a | 109.5 |
C32—W3—C301 | 117.1 (3) | C301—C311—H311c | 109.5 |
C32—W3—C302 | 135.6 (3) | H311b—C311—H311a | 109.5 |
C32—W3—C303 | 109.3 (3) | H311b—C311—H311c | 109.5 |
C32—W3—C304 | 77.9 (3) | H311a—C311—H311c | 109.5 |
C32—W3—C305 | 82.7 (3) | W4—C401—C402 | 74.3 (5) |
C301—W3—C302 | 33.8 (3) | W4—C401—C405 | 70.9 (4) |
C301—W3—C303 | 57.3 (3) | W4—C401—C411 | 127.0 (6) |
C301—W3—C304 | 58.9 (3) | C402—C401—C405 | 107.3 (7) |
C301—W3—C305 | 35.5 (3) | C402—C401—C411 | 123.3 (8) |
C302—W3—C303 | 34.3 (3) | C405—C401—C411 | 128.9 (8) |
C302—W3—C304 | 58.4 (3) | W4—C402—C401 | 70.6 (5) |
C302—W3—C305 | 57.9 (3) | W4—C402—C403 | 73.7 (5) |
C303—W3—C304 | 35.7 (3) | W4—C402—H402 | 121.8 |
C303—W3—C305 | 58.6 (3) | C401—C402—C403 | 109.0 (8) |
C304—W3—C305 | 35.7 (3) | C401—C402—H402 | 125.5 |
Ir1—W4—Ir2 | 57.04 (1) | C403—C402—H402 | 125.5 |
Ir1—W4—W3 | 57.24 (1) | W4—C403—C402 | 72.2 (5) |
Ir1—W4—C41 | 71.3 (2) | W4—C403—C404 | 70.5 (5) |
Ir1—W4—C42 | 77.3 (2) | W4—C403—H403 | 123.1 |
Ir1—W4—C401 | 151.8 (2) | C402—C403—C404 | 108.3 (8) |
Ir1—W4—C402 | 150.0 (2) | C402—C403—H403 | 125.8 |
Ir1—W4—C403 | 146.9 (2) | C404—C403—H403 | 125.8 |
Ir1—W4—C404 | 146.5 (2) | W4—C404—C403 | 74.5 (5) |
Ir1—W4—C405 | 150.0 (2) | W4—C404—C405 | 70.1 (4) |
Ir2—W4—W3 | 58.01 (1) | W4—C404—H404 | 120.5 |
Ir2—W4—C41 | 128.3 (2) | C403—C404—C405 | 106.5 (8) |
Ir2—W4—C42 | 80.6 (2) | C403—C404—H404 | 126.7 |
Ir2—W4—C401 | 103.8 (2) | C405—C404—H404 | 126.7 |
Ir2—W4—C402 | 95.1 (2) | W4—C405—C401 | 73.7 (4) |
Ir2—W4—C403 | 118.1 (3) | W4—C405—C404 | 73.9 (5) |
Ir2—W4—C404 | 152.2 (2) | W4—C405—H405 | 118.7 |
Ir2—W4—C405 | 137.8 (2) | C401—C405—C404 | 108.8 (8) |
W3—W4—C41 | 97.3 (2) | C401—C405—H405 | 125.6 |
W3—W4—C42 | 129.7 (2) | C404—C405—H405 | 125.6 |
W3—W4—C401 | 134.0 (2) | C401—C411—H411a | 109.5 |
W3—W4—C402 | 100.3 (2) | C401—C411—H411b | 109.5 |
W3—W4—C403 | 91.5 (2) | C401—C411—H411c | 109.5 |
W3—W4—C404 | 115.7 (2) | H411a—C411—H411b | 109.5 |
W3—W4—C405 | 149.6 (2) | H411a—C411—H411c | 109.5 |
C41—W4—C42 | 86.4 (3) | H411b—C411—H411c | 109.5 |
C41—W4—C401 | 122.5 (3) | W7—C701—C702 | 70.0 (5) |
C41—W4—C402 | 135.9 (3) | W7—C701—C705 | 71.5 (5) |
C41—W4—C403 | 106.0 (3) | W7—C701—C711 | 124.2 (6) |
C41—W4—C404 | 77.9 (3) | C702—C701—C705 | 104.4 (8) |
C41—W4—C405 | 87.5 (3) | C702—C701—C711 | 128.5 (9) |
C42—W4—C401 | 79.2 (3) | C705—C701—C711 | 127.1 (9) |
C42—W4—C402 | 111.4 (3) | W7—C702—C701 | 74.6 (5) |
C42—W4—C403 | 135.8 (3) | W7—C702—C703 | 75.0 (5) |
C42—W4—C404 | 114.1 (3) | W7—C702—H702 | 116.9 |
C42—W4—C405 | 80.4 (3) | C701—C702—C703 | 109.3 (8) |
C401—W4—C402 | 35.1 (3) | C701—C702—H702 | 125.4 |
C401—W4—C403 | 58.1 (3) | C703—C702—H702 | 125.4 |
C401—W4—C404 | 59.2 (3) | W7—C703—C702 | 69.7 (5) |
C401—W4—C405 | 35.4 (3) | W7—C703—C704 | 73.5 (5) |
C402—W4—C403 | 34.1 (3) | W7—C703—H703 | 122.3 |
C402—W4—C404 | 58.0 (3) | C702—C703—C704 | 107.5 (9) |
C402—W4—C405 | 58.3 (3) | C702—C703—H703 | 126.2 |
C403—W4—C404 | 35.0 (3) | C704—C703—H703 | 126.3 |
C403—W4—C405 | 58.5 (3) | W7—C704—C703 | 72.6 (5) |
C404—W4—C405 | 36.0 (3) | W7—C704—C705 | 71.1 (5) |
Ir5—W7—Ir6 | 57.85 (1) | W7—C704—H704 | 121.9 |
Ir5—W7—W8 | 58.81 (1) | C703—C704—C705 | 107.6 (8) |
Ir5—W7—C71 | 92.1 (3) | C703—C704—H704 | 126.2 |
Ir5—W7—C72 | 131.6 (2) | C705—C704—H704 | 126.2 |
Ir5—W7—C701 | 144.5 (2) | W7—C705—C701 | 73.5 (5) |
Ir5—W7—C702 | 136.1 (3) | W7—C705—C704 | 74.8 (5) |
Ir5—W7—C703 | 101.1 (3) | W7—C705—H705 | 118.8 |
Ir5—W7—C704 | 88.4 (2) | C701—C705—C704 | 111.0 (8) |
Ir5—W7—C705 | 110.1 (3) | C701—C705—H705 | 124.5 |
Ir6—W7—W8 | 58.21 (1) | C704—C705—H705 | 124.5 |
Ir6—W7—C71 | 123.2 (3) | C701—C711—H711c | 109.5 |
Ir6—W7—C72 | 82.5 (3) | C701—C711—H711a | 109.5 |
Ir6—W7—C701 | 145.0 (2) | C701—C711—H711b | 109.5 |
Ir6—W7—C702 | 110.3 (2) | H711c—C711—H711a | 109.5 |
Ir6—W7—C703 | 97.3 (2) | H711c—C711—H711b | 109.5 |
Ir6—W7—C704 | 116.8 (2) | H711a—C711—H711b | 109.5 |
Ir6—W7—C705 | 150.8 (2) | W8—C801—C802 | 69.6 (5) |
W8—W7—C71 | 65.0 (3) | W8—C801—C805 | 73.8 (5) |
W8—W7—C72 | 77.8 (2) | W8—C801—C811 | 129.2 (6) |
W8—W7—C701 | 147.7 (2) | C802—C801—C805 | 106.2 (8) |
W8—W7—C702 | 156.3 (2) | C802—C801—C811 | 126.3 (8) |
W8—W7—C703 | 153.6 (2) | C805—C801—C811 | 126.7 (9) |
W8—W7—C704 | 144.9 (2) | W8—C802—C801 | 74.7 (5) |
W8—W7—C705 | 142.6 (2) | W8—C802—C803 | 73.0 (5) |
C71—W7—C72 | 87.4 (3) | W8—C802—H802 | 119.4 |
C71—W7—C701 | 88.1 (4) | C801—C802—C803 | 110.9 (8) |
C71—W7—C702 | 122.7 (4) | C801—C802—H802 | 124.6 |
C71—W7—C703 | 137.8 (4) | C803—C802—H802 | 124.6 |
C71—W7—C704 | 108.1 (4) | W8—C803—C802 | 71.0 (5) |
C71—W7—C705 | 81.1 (4) | W8—C803—C804 | 72.8 (5) |
C72—W7—C701 | 83.9 (3) | W8—C803—H803 | 120.4 |
C72—W7—C702 | 80.2 (3) | C802—C803—C804 | 104.0 (8) |
C72—W7—C703 | 111.2 (4) | C802—C803—H803 | 128.0 |
C72—W7—C704 | 137.3 (3) | C804—C803—H803 | 128.0 |
C72—W7—C705 | 117.6 (4) | W8—C804—C803 | 72.1 (5) |
C701—W7—C702 | 35.3 (3) | W8—C804—C805 | 74.4 (5) |
C701—W7—C703 | 58.5 (3) | W8—C804—H804 | 120.4 |
C701—W7—C704 | 58.1 (3) | C803—C804—C805 | 110.7 (8) |
C701—W7—C705 | 35.0 (3) | C803—C804—H804 | 124.7 |
C702—W7—C703 | 35.3 (3) | C805—C804—H804 | 124.7 |
C702—W7—C704 | 57.8 (3) | W8—C805—C801 | 72.1 (5) |
C702—W7—C705 | 57.6 (3) | W8—C805—C804 | 70.4 (5) |
C703—W7—C704 | 34.0 (3) | W8—C805—H805 | 123.2 |
C703—W7—C705 | 56.8 (3) | C801—C805—C804 | 108.2 (8) |
C704—W7—C705 | 34.1 (3) | C801—C805—H805 | 125.9 |
Ir5—W8—Ir6 | 57.08 (1) | C804—C805—H805 | 125.9 |
Ir5—W8—W7 | 56.95 (1) | C801—C811—H811c | 109.5 |
Ir5—W8—C81 | 70.0 (2) | C801—C811—H811a | 109.5 |
Ir5—W8—C82 | 79.1 (3) | C801—C811—H811b | 109.5 |
Ir5—W8—C801 | 145.4 (2) | H811c—C811—H811a | 109.5 |
Ir5—W8—C802 | 149.6 (2) | H811c—C811—H811b | 109.5 |
Ir5—W8—C803 | 151.4 (2) | H811a—C811—H811b | 109.5 |
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) −x+1, −y+1, −z+1; (iii) x, y+1, z; (iv) −x+1/2, y−1/2, −z+1/2; (v) −x+3/2, y+1/2, −z+1/2; (vi) x, y−1, z; (vii) −x+3/2, y−1/2, −z+1/2; (viii) x+1/2, −y+1/2, z+1/2; (ix) x+1/2, −y−1/2, z+1/2; (x) x−1/2, −y+1/2, z−1/2; (xi) −x+1, −y, −z; (xii) −x+1, −y, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [W2Ir2(C6H7)2(CO)10] |
Mr | 1190.49 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 200 |
a, b, c (Å) | 18.3035 (1), 8.5629 (1), 31.2876 (2) |
β (°) | 94.7702 (4) |
V (Å3) | 4886.75 (6) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 20.34 |
Crystal size (mm) | 0.40 × 0.20 × 0.15 |
Data collection | |
Diffractometer | Nonius KappaCCD diffractometer |
Absorption correction | Integration Gaussian (Coppens, 1970) implemented in maXus (1999) |
Tmin, Tmax | 0.029, 0.193 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 129999, 14253, 12656 |
Rint | 0.077 |
(sin θ/λ)max (Å−1) | 0.705 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.042, 0.054, 2.40 |
No. of reflections | 12656 |
No. of parameters | 649 |
H-atom treatment | H-atom parameters not refined |
Δρmax, Δρmin (e Å−3) | 3.35, −2.86 |
Computer programs: KappaCCD Software (Nonius, 1997), HKL SCALEPACK (Otwinowski & Minor, 1997), DENZO and Scalepak (Otwinowski & Minor, 1997), PATTY in DIRDIF92 (Beurskens et al., 1992), TEXSAN (Molecular Structure Corporation, 1997), TEXSAN.
Ir1—Ir2 | 2.7242 (4) | Ir5—W7 | 2.8021 (5) |
Ir1—W3 | 2.8032 (4) | Ir5—W8 | 2.8596 (4) |
Ir1—W4 | 2.8577 (4) | Ir6—W7 | 2.8363 (5) |
Ir2—W3 | 2.8330 (4) | Ir6—W8 | 2.8482 (4) |
Ir2—W4 | 2.8476 (4) | W3—W4 | 2.9891 (4) |
Ir5—Ir6 | 2.7271 (4) | W7—W8 | 3.0108 (4) |
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Mixed-metal clusters containing very different metals have attracted significant recent interest, with tungsten–iridium clusters the focus of a considerable number of studies (Waterman et al., 2000). A precursor to much of the existing tungsten–iridium cluster chemistry is the cyclopentadienyl-containing cluster W2Ir2(CO)10(η5-C5H5)2 (Shapley et al., 1981). The methylcyclopentadienyl-containing clusters can be prepared analogously, as detailed below. This structural study, which reveals two independent molecules in the asymmetric unit, shows that the metal–metal core bond distances in the title complex are essentially identical to those of the cyclopentadienyl-containing analogue (Churchill et al., 1982).