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The title compound, deca­carbonyl-1κ2C,2κ2C,3κ3C,4κ3C-bis­[1,2(η5)-methyl­cyclo­pentadienyl]-tetrahedro-ditungsten­diirid­ium, [W2Ir2(C6H7)2(CO)10], is a mixed-metal cluster with tetrahedral metal-core geometry. The W atoms are each ligated by a η5-methyl­cyclo­penta­dienyl ligand and two carbonyl ligands, and the Ir atoms are each ligated by three carbonyl ligands.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801003750/bt6017sup1.cif
Contains datablocks ntl25, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801003750/bt6017Isup2.hkl
Contains datablock I

CCDC reference: 162793

Key indicators

  • Single-crystal X-ray study
  • T = 200 K
  • Mean [sigma](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




Comment top

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).

Experimental top

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.

Computing details top

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.

Figures top
[Figure 1] 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.
(I) top
Crystal data top
[W2Ir2(C6H7)2(CO)10]F(000) = 4224.00
Mr = 1190.49Dx = 3.236 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.7107 Å
a = 18.3035 (1) ÅCell parameters from 267775 reflections
b = 8.5629 (1) Åθ = 2.9–30.0°
c = 31.2876 (2) ŵ = 20.34 mm1
β = 94.7702 (4)°T = 200 K
V = 4886.75 (6) Å3Needle, red-brown
Z = 80.40 × 0.20 × 0.15 mm
Data collection top
Nonius KappaCCD
diffractometer
14253 independent reflections
Radiation source: fine-focus sealed tube12656 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.077
ϕ and ω scansθmax = 30.1°, θmin = 3.2°
Absorption correction: integration
Gaussian (Coppens, 1970) implemented in maXus (1999)
h = 2525
Tmin = 0.029, Tmax = 0.193k = 1210
129999 measured reflectionsl = 4444
Refinement top
Refinement on F0 restraints
Least-squares matrix: full0 constraints
R[F2 > 2σ(F2)] = 0.042H-atom parameters not refined
wR(F2) = 0.054Weighting scheme based on measured s.u.'s w = 1/[σ2(Fo) + 0.00040|Fo|2]
S = 2.40(Δ/σ)max = 0.032
12656 reflectionsΔρmax = 3.35 e Å3
649 parametersΔρmin = 2.86 e Å3
Crystal data top
[W2Ir2(C6H7)2(CO)10]V = 4886.75 (6) Å3
Mr = 1190.49Z = 8
Monoclinic, P21/nMo Kα radiation
a = 18.3035 (1) ŵ = 20.34 mm1
b = 8.5629 (1) ÅT = 200 K
c = 31.2876 (2) Å0.40 × 0.20 × 0.15 mm
β = 94.7702 (4)°
Data collection top
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 = 0.193Rint = 0.077
129999 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0420 restraints
wR(F2) = 0.054H-atom parameters not refined
S = 2.40Δρmax = 3.35 e Å3
12656 reflectionsΔρmin = 2.86 e Å3
649 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ir10.56524 (2)0.31024 (3)0.346149 (9)0.02105 (7)
Ir20.64578 (2)0.05483 (3)0.327935 (9)0.02159 (7)
Ir50.24298 (2)0.05311 (4)0.09590 (1)0.02709 (8)
Ir60.26744 (2)0.20304 (4)0.14688 (1)0.02679 (8)
W30.62643 (2)0.12848 (4)0.414546 (9)0.02057 (8)
W40.72109 (2)0.32363 (4)0.362323 (9)0.02030 (7)
W70.36056 (2)0.14311 (4)0.08069 (1)0.02391 (8)
W80.36385 (2)0.05680 (4)0.15998 (1)0.02461 (8)
O110.5062 (4)0.5362 (8)0.4090 (2)0.051 (2)
O120.4335 (4)0.0952 (8)0.3361 (2)0.044 (2)
O130.5345 (4)0.4946 (8)0.2618 (2)0.046 (2)
O210.7802 (4)0.1525 (8)0.3349 (2)0.049 (2)
O220.5335 (4)0.2103 (8)0.3251 (2)0.049 (2)
O230.6389 (4)0.1390 (8)0.2332 (2)0.051 (2)
O310.6904 (3)0.4130 (7)0.4662 (2)0.033 (2)
O320.7721 (4)0.0572 (7)0.4331 (2)0.042 (2)
O410.6635 (4)0.6530 (7)0.3854 (2)0.039 (2)
O420.7041 (4)0.4409 (8)0.2675 (2)0.046 (2)
O510.2962 (4)0.2713 (8)0.0280 (2)0.057 (2)
O520.1381 (4)0.1523 (7)0.0406 (2)0.048 (2)
O530.1250 (4)0.2390 (9)0.1376 (3)0.065 (3)
O610.3621 (4)0.4158 (8)0.2063 (2)0.052 (2)
O620.1878 (4)0.4614 (8)0.0953 (2)0.055 (2)
O630.1489 (4)0.1173 (9)0.2061 (2)0.057 (2)
O710.4749 (4)0.1224 (8)0.0748 (2)0.050 (2)
O720.4791 (4)0.3240 (7)0.1390 (2)0.039 (2)
O810.3560 (4)0.3847 (7)0.1187 (2)0.044 (2)
O820.2421 (4)0.1794 (9)0.2154 (2)0.052 (2)
C110.5299 (5)0.455 (1)0.3856 (3)0.031 (2)
C120.4839 (5)0.173 (1)0.3402 (3)0.029 (2)
C130.5474 (5)0.4262 (9)0.2926 (3)0.030 (2)
C210.7294 (5)0.073 (1)0.3334 (3)0.032 (2)
C220.5743 (5)0.111 (1)0.3279 (3)0.033 (2)
C230.6427 (5)0.109 (1)0.2690 (2)0.030 (2)
C310.6702 (4)0.3151 (9)0.4426 (2)0.022 (2)
C320.7209 (5)0.012 (1)0.4249 (3)0.033 (2)
C410.6794 (5)0.530 (1)0.3763 (3)0.030 (2)
C420.7055 (5)0.389 (1)0.3011 (3)0.032 (2)
C510.2748 (5)0.190 (1)0.0544 (3)0.033 (2)
C520.1775 (5)0.076 (1)0.0619 (3)0.036 (2)
C530.1712 (5)0.171 (1)0.1236 (3)0.038 (3)
C610.3264 (5)0.333 (1)0.1843 (3)0.034 (2)
C620.2202 (6)0.362 (1)0.1124 (3)0.036 (2)
C630.1951 (6)0.145 (1)0.1854 (3)0.041 (3)
C710.4292 (5)0.032 (1)0.0821 (3)0.037 (2)
C720.4322 (5)0.252 (1)0.1198 (3)0.030 (2)
C810.3552 (5)0.2605 (9)0.1309 (3)0.030 (2)
C820.2834 (5)0.130 (1)0.1936 (3)0.044 (3)
C3010.5522 (5)0.148 (1)0.4727 (3)0.030 (2)
C3020.5051 (5)0.104 (1)0.4378 (3)0.031 (2)
C3030.5272 (5)0.043 (1)0.4234 (3)0.035 (2)
C3040.5910 (6)0.090 (1)0.4499 (3)0.036 (2)
C3050.6057 (5)0.0290 (9)0.4805 (2)0.027 (2)
C3110.5461 (6)0.291 (1)0.5008 (3)0.041 (3)
C4010.8390 (4)0.296 (1)0.3409 (3)0.028 (2)
C4020.8354 (5)0.195 (1)0.3767 (3)0.034 (2)
C4030.8249 (5)0.285 (1)0.4129 (3)0.040 (3)
C4040.8209 (4)0.445 (1)0.4004 (3)0.033 (2)
C4050.8300 (4)0.449 (1)0.3554 (3)0.028 (2)
C4110.8602 (5)0.240 (1)0.2974 (3)0.043 (3)
C7010.4267 (5)0.257 (1)0.0267 (3)0.035 (2)
C7020.3764 (6)0.367 (1)0.0414 (3)0.037 (2)
C7030.3036 (6)0.317 (1)0.0289 (3)0.043 (3)
C7040.3081 (5)0.173 (1)0.0086 (3)0.035 (2)
C7050.3819 (6)0.137 (1)0.0079 (3)0.041 (3)
C7110.5064 (6)0.267 (1)0.0287 (3)0.051 (3)
C8010.4786 (5)0.172 (1)0.1819 (3)0.033 (2)
C8020.4302 (5)0.183 (1)0.2154 (3)0.037 (2)
C8030.4125 (5)0.031 (1)0.2308 (3)0.037 (2)
C8040.4515 (5)0.072 (1)0.2059 (3)0.039 (3)
C8050.4921 (5)0.013 (1)0.1766 (3)0.030 (2)
C8110.5166 (6)0.303 (1)0.1624 (3)0.044 (3)
H3020.46460.16300.42570.037*
H3030.50400.10130.40020.042*
H3040.61830.18300.44730.043*
H3050.64460.02930.50260.033*
H311b0.50680.35500.48920.050*
H311a0.53720.25970.52900.050*
H311c0.59060.34900.50170.050*
H4020.83940.08460.37610.041*
H4030.82120.24630.44110.047*
H4040.81360.53200.41840.040*
H4050.83000.54030.33820.034*
H411a0.91120.21750.29930.051*
H411b0.84950.31950.27670.051*
H411c0.83330.14850.28930.051*
H7020.38930.45950.05720.044*
H7030.25980.37240.03350.052*
H7040.26800.11150.00270.042*
H7050.39990.04310.00370.049*
H711c0.52360.33360.05170.061*
H711a0.52080.30810.00250.061*
H711b0.52680.16580.03330.061*
H8020.41220.27840.22610.044*
H8030.38160.00560.25280.045*
H8040.45080.18240.20840.047*
H8050.52290.03120.15680.036*
H811c0.48260.38450.15530.052*
H811a0.55460.34070.18220.052*
H811b0.53700.26780.13720.052*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ir10.0205 (1)0.0206 (1)0.0218 (1)0.0012 (1)0.0001 (1)0.0003 (1)
Ir20.0245 (2)0.0195 (1)0.0209 (1)0.0001 (1)0.0025 (1)0.0025 (1)
Ir50.0261 (2)0.0230 (2)0.0308 (2)0.0010 (1)0.0059 (1)0.0018 (1)
Ir60.0285 (2)0.0236 (2)0.0281 (2)0.0032 (1)0.0010 (1)0.0033 (1)
W30.0230 (2)0.0203 (2)0.0185 (1)0.0009 (1)0.0025 (1)0.0013 (1)
W40.0203 (2)0.0214 (2)0.0192 (1)0.0022 (1)0.0011 (1)0.0005 (1)
W70.0255 (2)0.0221 (2)0.0234 (2)0.0015 (1)0.0021 (1)0.0015 (1)
W80.0256 (2)0.0223 (2)0.0250 (2)0.0010 (1)0.0034 (1)0.0002 (1)
O110.061 (5)0.043 (4)0.051 (4)0.012 (4)0.016 (4)0.017 (3)
O120.030 (3)0.038 (3)0.063 (5)0.008 (3)0.010 (3)0.007 (3)
O130.057 (4)0.051 (4)0.028 (3)0.002 (4)0.009 (3)0.012 (3)
O210.041 (4)0.040 (4)0.070 (5)0.020 (3)0.017 (4)0.008 (4)
O220.048 (4)0.032 (3)0.067 (5)0.019 (3)0.002 (4)0.010 (3)
O230.064 (5)0.054 (4)0.035 (4)0.000 (4)0.002 (3)0.001 (3)
O310.042 (4)0.037 (3)0.019 (3)0.018 (3)0.001 (2)0.001 (2)
O320.040 (4)0.047 (4)0.038 (4)0.018 (3)0.003 (3)0.025 (3)
O410.041 (4)0.019 (3)0.057 (4)0.002 (3)0.007 (3)0.001 (3)
O420.042 (4)0.074 (5)0.023 (3)0.007 (4)0.002 (3)0.018 (3)
O510.073 (6)0.045 (4)0.050 (4)0.017 (4)0.016 (4)0.002 (4)
O520.051 (4)0.036 (4)0.054 (4)0.003 (3)0.022 (4)0.000 (3)
O530.047 (5)0.054 (5)0.095 (7)0.017 (4)0.009 (4)0.019 (5)
O610.057 (5)0.047 (4)0.050 (4)0.004 (4)0.007 (4)0.022 (4)
O620.068 (5)0.035 (4)0.060 (5)0.019 (4)0.007 (4)0.009 (3)
O630.049 (5)0.064 (5)0.059 (5)0.007 (4)0.019 (4)0.013 (4)
O710.061 (5)0.049 (4)0.041 (4)0.016 (4)0.003 (3)0.006 (3)
O720.038 (4)0.033 (3)0.043 (4)0.011 (3)0.011 (3)0.006 (3)
O810.055 (5)0.026 (3)0.050 (4)0.004 (3)0.010 (3)0.002 (3)
O820.042 (4)0.072 (5)0.043 (4)0.006 (4)0.009 (3)0.018 (4)
C110.033 (5)0.035 (5)0.026 (4)0.000 (4)0.002 (3)0.000 (4)
C120.029 (4)0.032 (4)0.026 (4)0.001 (4)0.001 (3)0.003 (3)
C130.029 (4)0.024 (4)0.035 (5)0.003 (3)0.006 (4)0.005 (4)
C210.031 (5)0.027 (4)0.039 (5)0.004 (4)0.008 (4)0.001 (4)
C220.036 (5)0.033 (5)0.029 (4)0.007 (4)0.005 (4)0.009 (4)
C230.040 (5)0.029 (4)0.020 (4)0.007 (4)0.001 (3)0.005 (3)
C310.028 (4)0.021 (4)0.017 (3)0.001 (3)0.004 (3)0.001 (3)
C320.045 (5)0.023 (4)0.033 (5)0.001 (4)0.015 (4)0.007 (4)
C410.033 (5)0.029 (4)0.029 (4)0.005 (4)0.001 (3)0.004 (3)
C420.028 (4)0.033 (5)0.034 (5)0.009 (4)0.001 (4)0.009 (4)
C510.037 (5)0.030 (4)0.031 (4)0.003 (4)0.009 (4)0.001 (4)
C520.029 (5)0.035 (5)0.044 (5)0.002 (4)0.011 (4)0.002 (4)
C530.033 (5)0.031 (5)0.051 (6)0.004 (4)0.004 (4)0.004 (4)
C610.037 (5)0.035 (5)0.032 (5)0.002 (4)0.007 (4)0.013 (4)
C620.053 (6)0.022 (4)0.034 (5)0.001 (4)0.002 (4)0.001 (4)
C630.041 (6)0.037 (5)0.046 (6)0.013 (4)0.009 (5)0.002 (4)
C710.028 (5)0.031 (5)0.050 (6)0.008 (4)0.012 (4)0.005 (4)
C720.030 (4)0.027 (4)0.031 (4)0.001 (4)0.005 (3)0.009 (4)
C810.040 (5)0.022 (4)0.026 (4)0.004 (4)0.009 (3)0.002 (3)
C820.030 (5)0.067 (7)0.033 (5)0.008 (5)0.004 (4)0.017 (5)
C3010.033 (5)0.032 (4)0.025 (4)0.009 (4)0.007 (3)0.002 (3)
C3020.028 (4)0.040 (5)0.028 (4)0.003 (4)0.013 (3)0.002 (4)
C3030.053 (6)0.031 (5)0.023 (4)0.010 (4)0.018 (4)0.008 (3)
C3040.061 (6)0.020 (4)0.029 (4)0.002 (4)0.011 (4)0.000 (3)
C3050.034 (4)0.029 (4)0.020 (4)0.001 (4)0.005 (3)0.006 (3)
C3110.046 (6)0.042 (5)0.039 (5)0.017 (5)0.018 (4)0.007 (4)
C4010.009 (3)0.039 (5)0.035 (4)0.004 (3)0.002 (3)0.005 (4)
C4020.016 (4)0.040 (5)0.046 (5)0.001 (4)0.003 (4)0.006 (4)
C4030.020 (4)0.065 (7)0.033 (5)0.005 (4)0.001 (3)0.003 (5)
C4040.020 (4)0.050 (6)0.029 (4)0.011 (4)0.001 (3)0.003 (4)
C4050.017 (4)0.037 (5)0.029 (4)0.012 (3)0.002 (3)0.007 (3)
C4110.040 (5)0.041 (5)0.050 (6)0.001 (5)0.016 (4)0.010 (5)
C7010.041 (5)0.026 (4)0.037 (5)0.001 (4)0.001 (4)0.011 (4)
C7020.050 (6)0.039 (5)0.022 (4)0.001 (4)0.005 (4)0.008 (4)
C7030.045 (6)0.049 (6)0.037 (5)0.014 (5)0.006 (4)0.006 (4)
C7040.044 (5)0.032 (4)0.028 (4)0.014 (4)0.005 (4)0.006 (4)
C7050.055 (6)0.039 (5)0.028 (4)0.016 (5)0.003 (4)0.005 (4)
C7110.044 (6)0.066 (7)0.044 (6)0.017 (6)0.007 (5)0.004 (5)
C8010.034 (5)0.026 (4)0.037 (5)0.003 (4)0.011 (4)0.008 (4)
C8020.035 (5)0.043 (5)0.032 (5)0.005 (4)0.011 (4)0.018 (4)
C8030.038 (5)0.044 (5)0.028 (4)0.005 (4)0.010 (4)0.006 (4)
C8040.043 (5)0.033 (5)0.038 (5)0.004 (4)0.022 (4)0.012 (4)
C8050.027 (4)0.033 (4)0.029 (4)0.000 (4)0.009 (3)0.007 (4)
C8110.043 (6)0.032 (5)0.055 (6)0.009 (4)0.000 (5)0.002 (4)
Geometric parameters (Å, º) top
Ir1—Ir22.7242 (4)O51—C511.17 (1)
Ir1—W32.8032 (4)O52—C521.14 (1)
Ir1—W42.8577 (4)O53—C531.14 (1)
Ir1—C111.898 (9)O61—C611.15 (1)
Ir1—C121.893 (9)O62—C621.15 (1)
Ir1—C131.952 (9)O63—C631.13 (1)
Ir2—W32.8330 (4)O71—C711.17 (1)
Ir2—W42.8476 (4)O72—C721.18 (1)
Ir2—C211.876 (9)O81—C811.131 (9)
Ir2—C221.929 (9)O82—C821.14 (1)
Ir2—C231.897 (8)C301—C3021.38 (1)
Ir5—Ir62.7271 (4)C301—C3051.42 (1)
Ir5—W72.8021 (5)C301—C3111.52 (1)
Ir5—W82.8596 (4)C302—C3031.41 (1)
Ir5—C511.875 (9)C302—H3020.95
Ir5—C521.893 (9)C303—C3041.43 (1)
Ir5—C531.918 (9)C303—H3030.95
Ir6—W72.8363 (5)C304—C3051.41 (1)
Ir6—W82.8482 (4)C304—H3040.95
Ir6—C611.888 (9)C305—H3050.95
Ir6—C621.898 (9)C311—H311b0.95
Ir6—C631.93 (1)C311—H311a0.95
W3—W42.9891 (4)C311—H311c0.95
W3—C311.962 (7)C401—C4021.42 (1)
W3—C322.001 (9)C401—C4051.40 (1)
W3—C3012.365 (8)C401—C4111.52 (1)
W3—C3022.403 (8)C402—C4031.40 (1)
W3—C3032.370 (9)C402—H4020.95
W3—C3042.291 (9)C403—C4041.42 (1)
W3—C3052.294 (7)C403—H4030.95
W4—C411.989 (9)C404—C4051.43 (1)
W4—C421.994 (9)C404—H4040.95
W4—C4012.326 (7)C405—H4050.95
W4—C4022.373 (9)C411—H411a0.95
W4—C4032.393 (9)C411—H411b0.95
W4—C4042.340 (8)C411—H411c0.95
W4—C4052.290 (7)C701—C7021.42 (1)
W7—W83.0108 (4)C701—C7051.42 (1)
W7—C711.955 (9)C701—C7111.46 (1)
W7—C721.955 (8)C702—C7031.42 (1)
W7—C7012.369 (9)C702—H7020.95
W7—C7022.309 (8)C703—C7041.39 (1)
W7—C7032.379 (9)C703—H7030.95
W7—C7042.391 (9)C704—C7051.39 (1)
W7—C7052.343 (9)C704—H7040.95
W8—C811.967 (8)C705—H7050.95
W8—C821.982 (9)C711—H711c0.95
W8—C8012.369 (9)C711—H711a0.95
W8—C8022.303 (8)C711—H711b0.95
W8—C8032.329 (8)C801—C8021.43 (1)
W8—C8042.338 (8)C801—C8051.40 (1)
W8—C8052.391 (8)C801—C8111.48 (1)
O11—C111.12 (1)C802—C8031.43 (1)
O12—C121.14 (1)C802—H8020.95
O13—C131.14 (1)C803—C8041.41 (1)
O21—C211.15 (1)C803—H8030.95
O22—C221.13 (1)C804—C8051.43 (1)
O23—C231.15 (1)C804—H8040.95
O31—C311.157 (9)C805—H8050.95
O32—C321.12 (1)C811—H811c0.95
O41—C411.13 (1)C811—H811a0.95
O42—C421.14 (1)C811—H811b0.95
O11···O53i3.21 (1)O41···C22iii3.08 (1)
O11···C311ii3.40 (1)O41···C21iii3.15 (1)
O11···O22iii3.47 (1)O41···C304iii3.34 (1)
O11···C53i3.52 (1)O41···C32iii3.44 (1)
O11···O52i3.57 (1)O42···C411v3.42 (1)
O12···O63i3.12 (1)O42···C23v3.43 (1)
O12···O62i3.25 (1)O42···C21v3.48 (1)
O12···C63i3.26 (1)O51···C702iii3.44 (1)
O12···C8033.33 (1)O51···C31x3.46 (1)
O12···O53iv3.36 (1)O51···C703iii3.52 (1)
O12···C62i3.38 (1)O52···C302iv3.46 (1)
O13···O22iii3.21 (1)O52···C311iv3.54 (1)
O13···C411v3.49 (1)O53···O62iii3.15 (1)
O13···C8113.51 (1)O61···O81vi3.22 (1)
O13···C8023.52 (1)O61···O63iv3.26 (1)
O13···O61iii3.56 (1)O61···O82iv3.33 (1)
O21···O41vi3.225 (9)O62···C53vi3.29 (1)
O21···O23vii3.23 (1)O62···O81vi3.37 (1)
O21···O42vii3.34 (1)O63···C12iv3.26 (1)
O21···C405vi3.58 (1)O63···C802iv3.41 (1)
O21···C41vi3.59 (1)O63···O82iv3.50 (1)
O22···O41vi3.14 (1)O71···C711xi3.51 (1)
O22···O53iv3.25 (1)O72···C811vi3.34 (1)
O22···C13vi3.29 (1)O72···O81vi3.385 (9)
O22···C11vi3.44 (1)O72···C411vii3.45 (1)
O23···C8013.24 (1)O72···C402vii3.47 (1)
O23···C8053.28 (1)O72···C401vii3.49 (1)
O23···C405vii3.30 (1)O81···C61iii3.25 (1)
O23···C8113.33 (1)O81···C702iii3.26 (1)
O23···O42vii3.34 (1)O81···C62iii3.29 (1)
O23···C411vii3.55 (1)O81···C72iii3.41 (1)
O31···O51viii3.060 (9)O82···C61i3.47 (1)
O31···C51viii3.17 (1)O82···C63i3.55 (1)
O31···C704viii3.30 (1)C302···C305xii3.58 (1)
O31···O52viii3.303 (9)C303···C311xii3.53 (1)
O31···C52viii3.33 (1)C304···C311xii3.51 (1)
O32···C703ix3.19 (1)C403···C711v3.48 (1)
O32···C704ix3.33 (1)C405···C805v3.53 (1)
O32···O41vi3.439 (9)
Ir2—Ir1—W361.65 (1)Ir5—W8—C804151.3 (2)
Ir2—Ir1—W461.29 (1)Ir5—W8—C805147.0 (2)
Ir2—Ir1—C11151.5 (3)Ir6—W8—W757.83 (1)
Ir2—Ir1—C1285.2 (3)Ir6—W8—C81127.0 (2)
Ir2—Ir1—C13106.5 (2)Ir6—W8—C8281.1 (3)
W3—Ir1—W463.74 (1)Ir6—W8—C801152.9 (2)
W3—Ir1—C1190.1 (3)Ir6—W8—C802139.2 (3)
W3—Ir1—C1289.5 (2)Ir6—W8—C803104.2 (2)
W3—Ir1—C13164.9 (3)Ir6—W8—C80496.1 (2)
W4—Ir1—C11104.4 (3)Ir6—W8—C805119.6 (2)
W4—Ir1—C12143.9 (3)W7—W8—C8197.4 (2)
W4—Ir1—C13103.0 (3)W7—W8—C82130.8 (3)
C11—Ir1—C1299.2 (4)W7—W8—C801115.5 (2)
C11—Ir1—C13100.7 (3)W7—W8—C802149.4 (2)
C12—Ir1—C1399.0 (3)W7—W8—C803135.2 (2)
Ir1—Ir2—W360.55 (1)W7—W8—C804101.8 (2)
Ir1—Ir2—W461.67 (1)W7—W8—C80592.4 (2)
Ir1—Ir2—C21154.1 (3)C81—W8—C8285.9 (4)
Ir1—Ir2—C22102.2 (2)C81—W8—C80178.5 (3)
Ir1—Ir2—C2392.1 (2)C81—W8—C80287.1 (3)
W3—Ir2—W463.50 (1)C81—W8—C803122.2 (3)
W3—Ir2—C21102.0 (3)C81—W8—C804136.6 (3)
W3—Ir2—C2291.5 (2)C81—W8—C805106.2 (3)
W3—Ir2—C23151.6 (2)C82—W8—C801113.2 (4)
W4—Ir2—C2194.0 (3)C82—W8—C80279.6 (4)
W4—Ir2—C22154.4 (2)C82—W8—C80376.5 (4)
W4—Ir2—C2398.4 (3)C82—W8—C804108.9 (4)
C21—Ir2—C2296.9 (4)C82—W8—C805133.9 (3)
C21—Ir2—C23100.8 (4)C801—W8—C80235.7 (3)
C22—Ir2—C23102.2 (4)C801—W8—C80360.3 (3)
Ir6—Ir5—W761.71 (1)C801—W8—C80458.1 (3)
Ir6—Ir5—W861.25 (1)C801—W8—C80534.1 (3)
Ir6—Ir5—C51149.4 (3)C802—W8—C80336.1 (3)
Ir6—Ir5—C5285.7 (3)C802—W8—C80457.7 (3)
Ir6—Ir5—C53104.1 (3)C802—W8—C80557.6 (3)
W7—Ir5—W864.24 (1)C803—W8—C80435.1 (3)
W7—Ir5—C5188.2 (3)C803—W8—C80559.2 (3)
W7—Ir5—C5290.8 (3)C804—W8—C80535.1 (3)
W7—Ir5—C53162.9 (3)Ir1—C11—O11176.9 (8)
W8—Ir5—C51102.3 (3)Ir1—C12—O12177.5 (8)
W8—Ir5—C52144.9 (3)Ir1—C13—O13177.6 (8)
W8—Ir5—C53101.3 (3)Ir2—C21—O21176.9 (8)
C51—Ir5—C52101.1 (4)Ir2—C22—O22175.4 (8)
C51—Ir5—C53104.5 (4)Ir2—C23—O23178.0 (8)
C52—Ir5—C5397.7 (4)W3—C31—O31166.5 (6)
Ir5—Ir6—W760.45 (1)W3—C32—O32175.6 (7)
Ir5—Ir6—W861.67 (1)W4—C41—O41172.3 (8)
Ir5—Ir6—C61153.4 (3)W4—C42—O42170.4 (8)
Ir5—Ir6—C62101.5 (3)Ir5—C51—O51177.9 (8)
Ir5—Ir6—C6394.1 (3)Ir5—C52—O52178.7 (9)
W7—Ir6—W863.96 (1)Ir5—C53—O53175.2 (9)
W7—Ir6—C61102.3 (3)Ir6—C61—O61177.9 (9)
W7—Ir6—C6289.3 (3)Ir6—C62—O62172.8 (9)
W7—Ir6—C63153.7 (3)Ir6—C63—O63175.0 (9)
W8—Ir6—C6193.2 (3)W7—C71—O71165.3 (9)
W8—Ir6—C62152.7 (3)W7—C72—O72171.8 (7)
W8—Ir6—C6399.2 (3)W8—C81—O81171.0 (7)
C61—Ir6—C6298.1 (4)W8—C82—O82173.6 (8)
C61—Ir6—C6398.6 (4)W3—C301—C30274.6 (5)
C62—Ir6—C63103.6 (4)W3—C301—C30569.5 (4)
Ir1—W3—Ir257.80 (1)W3—C301—C311125.2 (6)
Ir1—W3—W459.02 (1)C302—C301—C305108.3 (8)
Ir1—W3—C3190.7 (2)C302—C301—C311127.3 (9)
Ir1—W3—C32133.4 (2)C305—C301—C311124.2 (8)
Ir1—W3—C301109.2 (2)W3—C302—C30171.6 (5)
Ir1—W3—C30287.7 (2)W3—C302—C30371.6 (5)
Ir1—W3—C30399.9 (2)W3—C302—H302122.8
Ir1—W3—C304135.2 (3)C301—C302—C303108.7 (8)
Ir1—W3—C305143.9 (2)C301—C302—H302125.7
Ir2—W3—W458.49 (1)C303—C302—H302125.7
Ir2—W3—C31122.0 (2)W3—C303—C30274.1 (5)
Ir2—W3—C3282.5 (2)W3—C303—C30469.1 (5)
Ir2—W3—C301151.3 (2)W3—C303—H303122.3
Ir2—W3—C302117.6 (2)C302—C303—C304107.7 (8)
Ir2—W3—C30397.6 (2)C302—C303—H303126.1
Ir2—W3—C304110.1 (2)C304—C303—H303126.1
Ir2—W3—C305145.2 (2)W3—C304—C30375.2 (5)
W4—W3—C3163.6 (2)W3—C304—C30572.2 (5)
W4—W3—C3280.5 (2)W3—C304—H304118.2
W4—W3—C301141.0 (2)C303—C304—C305107.2 (7)
W4—W3—C302143.8 (2)C303—C304—H304126.4
W4—W3—C303153.5 (2)C305—C304—H304126.4
W4—W3—C304156.9 (2)W3—C305—C30175.0 (4)
W4—W3—C305147.8 (2)W3—C305—C30472.0 (5)
C31—W3—C3291.1 (3)W3—C305—H305118.9
C31—W3—C30180.6 (3)C301—C305—C304108.1 (7)
C31—W3—C302106.8 (3)C301—C305—H305126.0
C31—W3—C303137.8 (3)C304—C305—H305126.0
C31—W3—C304124.7 (3)C301—C311—H311b109.5
C31—W3—C30589.5 (3)C301—C311—H311a109.5
C32—W3—C301117.1 (3)C301—C311—H311c109.5
C32—W3—C302135.6 (3)H311b—C311—H311a109.5
C32—W3—C303109.3 (3)H311b—C311—H311c109.5
C32—W3—C30477.9 (3)H311a—C311—H311c109.5
C32—W3—C30582.7 (3)W4—C401—C40274.3 (5)
C301—W3—C30233.8 (3)W4—C401—C40570.9 (4)
C301—W3—C30357.3 (3)W4—C401—C411127.0 (6)
C301—W3—C30458.9 (3)C402—C401—C405107.3 (7)
C301—W3—C30535.5 (3)C402—C401—C411123.3 (8)
C302—W3—C30334.3 (3)C405—C401—C411128.9 (8)
C302—W3—C30458.4 (3)W4—C402—C40170.6 (5)
C302—W3—C30557.9 (3)W4—C402—C40373.7 (5)
C303—W3—C30435.7 (3)W4—C402—H402121.8
C303—W3—C30558.6 (3)C401—C402—C403109.0 (8)
C304—W3—C30535.7 (3)C401—C402—H402125.5
Ir1—W4—Ir257.04 (1)C403—C402—H402125.5
Ir1—W4—W357.24 (1)W4—C403—C40272.2 (5)
Ir1—W4—C4171.3 (2)W4—C403—C40470.5 (5)
Ir1—W4—C4277.3 (2)W4—C403—H403123.1
Ir1—W4—C401151.8 (2)C402—C403—C404108.3 (8)
Ir1—W4—C402150.0 (2)C402—C403—H403125.8
Ir1—W4—C403146.9 (2)C404—C403—H403125.8
Ir1—W4—C404146.5 (2)W4—C404—C40374.5 (5)
Ir1—W4—C405150.0 (2)W4—C404—C40570.1 (4)
Ir2—W4—W358.01 (1)W4—C404—H404120.5
Ir2—W4—C41128.3 (2)C403—C404—C405106.5 (8)
Ir2—W4—C4280.6 (2)C403—C404—H404126.7
Ir2—W4—C401103.8 (2)C405—C404—H404126.7
Ir2—W4—C40295.1 (2)W4—C405—C40173.7 (4)
Ir2—W4—C403118.1 (3)W4—C405—C40473.9 (5)
Ir2—W4—C404152.2 (2)W4—C405—H405118.7
Ir2—W4—C405137.8 (2)C401—C405—C404108.8 (8)
W3—W4—C4197.3 (2)C401—C405—H405125.6
W3—W4—C42129.7 (2)C404—C405—H405125.6
W3—W4—C401134.0 (2)C401—C411—H411a109.5
W3—W4—C402100.3 (2)C401—C411—H411b109.5
W3—W4—C40391.5 (2)C401—C411—H411c109.5
W3—W4—C404115.7 (2)H411a—C411—H411b109.5
W3—W4—C405149.6 (2)H411a—C411—H411c109.5
C41—W4—C4286.4 (3)H411b—C411—H411c109.5
C41—W4—C401122.5 (3)W7—C701—C70270.0 (5)
C41—W4—C402135.9 (3)W7—C701—C70571.5 (5)
C41—W4—C403106.0 (3)W7—C701—C711124.2 (6)
C41—W4—C40477.9 (3)C702—C701—C705104.4 (8)
C41—W4—C40587.5 (3)C702—C701—C711128.5 (9)
C42—W4—C40179.2 (3)C705—C701—C711127.1 (9)
C42—W4—C402111.4 (3)W7—C702—C70174.6 (5)
C42—W4—C403135.8 (3)W7—C702—C70375.0 (5)
C42—W4—C404114.1 (3)W7—C702—H702116.9
C42—W4—C40580.4 (3)C701—C702—C703109.3 (8)
C401—W4—C40235.1 (3)C701—C702—H702125.4
C401—W4—C40358.1 (3)C703—C702—H702125.4
C401—W4—C40459.2 (3)W7—C703—C70269.7 (5)
C401—W4—C40535.4 (3)W7—C703—C70473.5 (5)
C402—W4—C40334.1 (3)W7—C703—H703122.3
C402—W4—C40458.0 (3)C702—C703—C704107.5 (9)
C402—W4—C40558.3 (3)C702—C703—H703126.2
C403—W4—C40435.0 (3)C704—C703—H703126.3
C403—W4—C40558.5 (3)W7—C704—C70372.6 (5)
C404—W4—C40536.0 (3)W7—C704—C70571.1 (5)
Ir5—W7—Ir657.85 (1)W7—C704—H704121.9
Ir5—W7—W858.81 (1)C703—C704—C705107.6 (8)
Ir5—W7—C7192.1 (3)C703—C704—H704126.2
Ir5—W7—C72131.6 (2)C705—C704—H704126.2
Ir5—W7—C701144.5 (2)W7—C705—C70173.5 (5)
Ir5—W7—C702136.1 (3)W7—C705—C70474.8 (5)
Ir5—W7—C703101.1 (3)W7—C705—H705118.8
Ir5—W7—C70488.4 (2)C701—C705—C704111.0 (8)
Ir5—W7—C705110.1 (3)C701—C705—H705124.5
Ir6—W7—W858.21 (1)C704—C705—H705124.5
Ir6—W7—C71123.2 (3)C701—C711—H711c109.5
Ir6—W7—C7282.5 (3)C701—C711—H711a109.5
Ir6—W7—C701145.0 (2)C701—C711—H711b109.5
Ir6—W7—C702110.3 (2)H711c—C711—H711a109.5
Ir6—W7—C70397.3 (2)H711c—C711—H711b109.5
Ir6—W7—C704116.8 (2)H711a—C711—H711b109.5
Ir6—W7—C705150.8 (2)W8—C801—C80269.6 (5)
W8—W7—C7165.0 (3)W8—C801—C80573.8 (5)
W8—W7—C7277.8 (2)W8—C801—C811129.2 (6)
W8—W7—C701147.7 (2)C802—C801—C805106.2 (8)
W8—W7—C702156.3 (2)C802—C801—C811126.3 (8)
W8—W7—C703153.6 (2)C805—C801—C811126.7 (9)
W8—W7—C704144.9 (2)W8—C802—C80174.7 (5)
W8—W7—C705142.6 (2)W8—C802—C80373.0 (5)
C71—W7—C7287.4 (3)W8—C802—H802119.4
C71—W7—C70188.1 (4)C801—C802—C803110.9 (8)
C71—W7—C702122.7 (4)C801—C802—H802124.6
C71—W7—C703137.8 (4)C803—C802—H802124.6
C71—W7—C704108.1 (4)W8—C803—C80271.0 (5)
C71—W7—C70581.1 (4)W8—C803—C80472.8 (5)
C72—W7—C70183.9 (3)W8—C803—H803120.4
C72—W7—C70280.2 (3)C802—C803—C804104.0 (8)
C72—W7—C703111.2 (4)C802—C803—H803128.0
C72—W7—C704137.3 (3)C804—C803—H803128.0
C72—W7—C705117.6 (4)W8—C804—C80372.1 (5)
C701—W7—C70235.3 (3)W8—C804—C80574.4 (5)
C701—W7—C70358.5 (3)W8—C804—H804120.4
C701—W7—C70458.1 (3)C803—C804—C805110.7 (8)
C701—W7—C70535.0 (3)C803—C804—H804124.7
C702—W7—C70335.3 (3)C805—C804—H804124.7
C702—W7—C70457.8 (3)W8—C805—C80172.1 (5)
C702—W7—C70557.6 (3)W8—C805—C80470.4 (5)
C703—W7—C70434.0 (3)W8—C805—H805123.2
C703—W7—C70556.8 (3)C801—C805—C804108.2 (8)
C704—W7—C70534.1 (3)C801—C805—H805125.9
Ir5—W8—Ir657.08 (1)C804—C805—H805125.9
Ir5—W8—W756.95 (1)C801—C811—H811c109.5
Ir5—W8—C8170.0 (2)C801—C811—H811a109.5
Ir5—W8—C8279.1 (3)C801—C811—H811b109.5
Ir5—W8—C801145.4 (2)H811c—C811—H811a109.5
Ir5—W8—C802149.6 (2)H811c—C811—H811b109.5
Ir5—W8—C803151.4 (2)H811a—C811—H811b109.5
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, y1/2, z+1/2; (v) x+3/2, y+1/2, z+1/2; (vi) x, y1, z; (vii) x+3/2, y1/2, z+1/2; (viii) x+1/2, y+1/2, z+1/2; (ix) x+1/2, y1/2, z+1/2; (x) x1/2, y+1/2, z1/2; (xi) x+1, y, z; (xii) x+1, y, z+1.

Experimental details

Crystal data
Chemical formula[W2Ir2(C6H7)2(CO)10]
Mr1190.49
Crystal system, space groupMonoclinic, P21/n
Temperature (K)200
a, b, c (Å)18.3035 (1), 8.5629 (1), 31.2876 (2)
β (°) 94.7702 (4)
V3)4886.75 (6)
Z8
Radiation typeMo Kα
µ (mm1)20.34
Crystal size (mm)0.40 × 0.20 × 0.15
Data collection
DiffractometerNonius KappaCCD
diffractometer
Absorption correctionIntegration
Gaussian (Coppens, 1970) implemented in maXus (1999)
Tmin, Tmax0.029, 0.193
No. of measured, independent and
observed [I > 2σ(I)] reflections
129999, 14253, 12656
Rint0.077
(sin θ/λ)max1)0.705
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.042, 0.054, 2.40
No. of reflections12656
No. of parameters649
H-atom treatmentH-atom parameters not refined
Δρmax, Δρmin (e Å3)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.

Selected bond lengths (Å) top
Ir1—Ir22.7242 (4)Ir5—W72.8021 (5)
Ir1—W32.8032 (4)Ir5—W82.8596 (4)
Ir1—W42.8577 (4)Ir6—W72.8363 (5)
Ir2—W32.8330 (4)Ir6—W82.8482 (4)
Ir2—W42.8476 (4)W3—W42.9891 (4)
Ir5—Ir62.7271 (4)W7—W83.0108 (4)
 

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