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A mixed tetranuclear cluster of ruthenium and cobalt, namely undeca­carbonyl-tri-μ-hydrido-(tri­cyclo­hexyl­phosphine)­tri­rutheniumcobalt, [CoRu3H3(CO)11(C18H33P)], has been synthesized by reaction between Co2(CO)8 and the electron-deficient cluster [Ru3H2(CO)6(PCy3)3]. The compound was characterized, both spectroscopically and crystallographically. The molecular structure of [CoRu3(μ-H)3(μ-CO)(CO)10(PCy3)] shows a tetrahedral metal core. The tris­(cyclo­hexyl)­phosphine ligand is attached in an axial position to one of the Ru atoms of the basal face.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802013387/dn6037sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802013387/dn6037Isup2.hkl
Contains datablock I

CCDC reference: 193721

Key indicators

  • Single-crystal X-ray study
  • T = 153 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.036
  • wR factor = 0.091
  • Data-to-parameter ratio = 15.0

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry








Computing details top

Data collection: EXPOSE in IPDS Software (Stoe & Cie, 2000); cell refinement: CELL in IPDS Software; data reduction: INTEGRATE in IPDS Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

undecacarbonyl-tri-µ-hydrido-(tricyclohexylphosphine)trirutheniumcobalt top
Crystal data top
[CoRu3H3(CO)11(C18H33P)]F(000) = 1888
Mr = 953.69Dx = 1.850 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 8000 reflections
a = 9.6492 (8) Åθ = 2.3–25.9°
b = 16.4487 (9) ŵ = 1.88 mm1
c = 21.6012 (17) ÅT = 153 K
β = 92.583 (10)°Plate, red
V = 3425.0 (4) Å30.75 × 0.45 × 0.10 mm
Z = 4
Data collection top
Stoe IPDS
diffractometer
6430 independent reflections
Radiation source: fine-focus sealed tube4807 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.034
Detector resolution: 0 pixels mm-1θmax = 25.9°, θmin = 2.3°
φ–oscillation scanh = 1111
Absorption correction: empirical (using intensity measurements)
(Walker & Stuart, 1983)
k = 1919
Tmin = 0.375, Tmax = 0.830l = 2626
23765 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.036Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.091H-atom parameters constrained
S = 0.92 w = 1/[σ2(Fo2) + (0.0661P)2]
where P = (Fo2 + 2Fc2)/3
6430 reflections(Δ/σ)max = 0.002
430 parametersΔρmax = 2.87 e Å3
0 restraintsΔρmin = 0.76 e Å3
Special details top

Experimental. A crystal was mounted at 153 K on a Stoe Image Plate Diffraction System (Stoe & Cie, 2000) using Mo Kα graphite monochromated radiation. Image plate distance 70 mm, φ oscillation scans 0 - 180°, step Δφ = 1°, 2 minutes per frame.

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
xyzUiso*/UeqOcc. (<1)
C10.5322 (4)0.2021 (3)0.37067 (17)0.0193 (8)
H10.44230.19400.34860.023*
C20.5030 (4)0.1991 (3)0.43970 (19)0.0270 (10)
H2A0.58830.20880.46410.032*
H2B0.46870.14570.45020.032*
C30.3944 (5)0.2642 (3)0.4552 (2)0.0341 (11)
H3A0.30740.25210.43290.041*
H3B0.37850.26260.49920.041*
C40.4421 (5)0.3479 (3)0.4379 (2)0.0374 (11)
H4A0.52480.36190.46280.045*
H4B0.37050.38720.44660.045*
C50.4735 (5)0.3522 (3)0.3696 (2)0.0358 (11)
H5A0.50910.40570.36020.043*
H5B0.38850.34390.34460.043*
C60.5803 (4)0.2875 (3)0.3529 (2)0.0281 (10)
H6A0.59410.28940.30870.034*
H6B0.66840.29930.37450.034*
C70.5809 (4)0.0266 (3)0.37804 (18)0.0218 (9)
H70.59430.03320.42300.026*
C80.4261 (4)0.0119 (3)0.3649 (2)0.0329 (11)
H8A0.40770.00340.32090.040*
H8B0.37370.05900.37740.040*
C90.3808 (5)0.0640 (4)0.4014 (2)0.0455 (14)
H9A0.39050.05280.44540.055*
H9B0.28380.07520.39120.055*
C100.4671 (7)0.1386 (4)0.3866 (3)0.0518 (15)
H10A0.43990.18370.41240.062*
H10B0.44860.15390.34360.062*
C110.6185 (6)0.1230 (3)0.3973 (2)0.0416 (12)
H11A0.67040.17040.38520.050*
H11B0.63870.11340.44110.050*
C120.6639 (5)0.0497 (3)0.3605 (2)0.0310 (10)
H12A0.64930.06050.31650.037*
H12B0.76220.04000.36890.037*
C130.8216 (4)0.1389 (3)0.38563 (16)0.0193 (8)
H130.83080.19800.38930.023*
C140.9465 (4)0.1106 (3)0.35084 (18)0.0256 (9)
H14A0.94170.13320.30930.031*
H14B0.94490.05180.34730.031*
C151.0815 (4)0.1374 (3)0.3846 (2)0.0321 (11)
H15A1.15970.11700.36250.039*
H15B1.08640.19630.38490.039*
C161.0913 (4)0.1063 (3)0.4506 (2)0.0339 (11)
H16A1.09760.04740.45040.041*
H16B1.17480.12750.47160.041*
C170.9664 (4)0.1320 (3)0.48534 (19)0.0319 (11)
H17A0.96720.19060.49020.038*
H17B0.97180.10800.52640.038*
C180.8299 (4)0.1061 (3)0.45179 (18)0.0245 (9)
H18A0.82390.04730.45100.029*
H18B0.75220.12670.47410.029*
C190.6376 (5)0.0062 (3)0.1104 (2)0.0211 (10)0.85
C200.4468 (5)0.0832 (4)0.1717 (2)0.0360 (11)
C210.3252 (4)0.0302 (3)0.0860 (2)0.0271 (10)
C220.2658 (12)0.0395 (8)0.2104 (5)0.034 (2)0.85
C230.2692 (5)0.2094 (3)0.2160 (2)0.0408 (13)
C240.3197 (4)0.2094 (3)0.0900 (2)0.0279 (10)
C250.4648 (7)0.3199 (4)0.1706 (3)0.0308 (12)0.85
C260.8115 (5)0.1344 (3)0.10885 (19)0.0319 (11)
C270.5844 (4)0.1305 (3)0.0246 (2)0.0287 (10)
C280.7888 (4)0.0364 (3)0.23218 (17)0.0243 (9)
C290.7793 (4)0.2069 (3)0.23381 (18)0.0251 (10)
O190.6894 (4)0.0553 (2)0.10096 (16)0.0294 (8)0.85
O200.4532 (5)0.1524 (3)0.17556 (19)0.0627 (12)
O210.2633 (4)0.0281 (2)0.04067 (15)0.0410 (9)
O220.1675 (5)0.0376 (4)0.2371 (3)0.0502 (15)0.85
O230.1756 (4)0.2176 (3)0.2460 (2)0.0710 (14)
O240.2591 (4)0.2132 (2)0.04418 (15)0.0402 (8)
O250.4847 (5)0.3879 (3)0.1702 (2)0.0513 (12)0.85
O260.9293 (3)0.1415 (3)0.10848 (16)0.0496 (10)
O270.5637 (4)0.1401 (2)0.02685 (14)0.0417 (9)
O280.8663 (3)0.0157 (2)0.22985 (15)0.0399 (9)
O290.8496 (3)0.2627 (2)0.23342 (15)0.0391 (8)
P10.64760 (9)0.12019 (6)0.34253 (4)0.0149 (2)
Ru10.65296 (3)0.11906 (2)0.233179 (13)0.01605 (9)
Ru20.42985 (3)0.03243 (2)0.163341 (14)0.02085 (10)
Ru30.42638 (3)0.20460 (2)0.166509 (14)0.01777 (10)0.85
Co10.62732 (5)0.11866 (3)0.10736 (2)0.01966 (12)0.85
H1H0.52380.18630.22900.050*
H2H0.53760.05200.22800.050*
H3H0.53720.20800.12340.050*0.85
Ru3B0.62732 (5)0.11866 (3)0.10736 (2)0.01966 (12)0.15
Co1B0.42638 (3)0.20460 (2)0.166509 (14)0.01777 (10)0.15
C22B0.286 (7)0.020 (4)0.208 (3)0.020 (14)*0.15
O22B0.189 (4)0.002 (2)0.2377 (17)0.045 (10)*0.15
C25B0.408 (4)0.309 (3)0.1891 (19)0.043 (10)*0.15
O25B0.406 (3)0.3798 (19)0.2008 (14)0.058 (7)*0.15
C19B0.6119 (18)0.2422 (13)0.1155 (8)0.000 (4)*0.15
O19B0.6410 (19)0.3101 (13)0.1066 (8)0.025 (4)*0.15
H3HB0.55420.05620.11240.050*0.15
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0158 (18)0.019 (2)0.0228 (19)0.0028 (14)0.0001 (14)0.0005 (16)
C20.030 (2)0.025 (3)0.027 (2)0.0059 (17)0.0054 (17)0.0014 (17)
C30.040 (3)0.028 (3)0.035 (2)0.006 (2)0.0130 (19)0.003 (2)
C40.039 (3)0.028 (3)0.046 (3)0.006 (2)0.013 (2)0.005 (2)
C50.038 (3)0.018 (3)0.052 (3)0.0072 (19)0.010 (2)0.004 (2)
C60.032 (2)0.018 (3)0.035 (2)0.0021 (17)0.0086 (18)0.0045 (18)
C70.029 (2)0.015 (2)0.0215 (19)0.0044 (16)0.0012 (16)0.0032 (16)
C80.030 (2)0.038 (3)0.031 (2)0.016 (2)0.0029 (18)0.000 (2)
C90.049 (3)0.055 (4)0.033 (2)0.030 (3)0.005 (2)0.007 (2)
C100.084 (4)0.029 (4)0.043 (3)0.021 (3)0.006 (3)0.001 (2)
C110.072 (4)0.019 (3)0.034 (2)0.006 (2)0.007 (2)0.003 (2)
C120.050 (3)0.017 (3)0.027 (2)0.001 (2)0.0052 (19)0.0007 (18)
C130.0252 (19)0.016 (2)0.0165 (18)0.0029 (15)0.0047 (14)0.0042 (15)
C140.0189 (18)0.038 (3)0.0197 (18)0.0005 (17)0.0010 (15)0.0044 (18)
C150.0138 (18)0.050 (3)0.032 (2)0.0020 (18)0.0004 (16)0.010 (2)
C160.027 (2)0.039 (3)0.034 (2)0.0015 (19)0.0120 (18)0.007 (2)
C170.035 (2)0.039 (3)0.021 (2)0.007 (2)0.0089 (17)0.0018 (19)
C180.0225 (19)0.030 (3)0.0205 (19)0.0002 (17)0.0025 (15)0.0003 (17)
C190.029 (2)0.019 (3)0.016 (2)0.001 (2)0.0025 (17)0.0015 (19)
C200.052 (3)0.026 (3)0.029 (2)0.011 (2)0.006 (2)0.001 (2)
C210.033 (2)0.016 (3)0.032 (2)0.0070 (17)0.0043 (18)0.0003 (17)
C220.027 (5)0.044 (8)0.032 (4)0.007 (4)0.001 (3)0.004 (4)
C230.039 (3)0.049 (4)0.034 (2)0.017 (2)0.003 (2)0.005 (2)
C240.031 (2)0.018 (3)0.035 (2)0.0066 (17)0.0010 (18)0.0003 (18)
C250.037 (3)0.026 (4)0.029 (3)0.003 (3)0.007 (3)0.000 (2)
C260.034 (2)0.039 (3)0.023 (2)0.000 (2)0.0023 (17)0.0050 (19)
C270.027 (2)0.028 (3)0.031 (2)0.0013 (17)0.0070 (17)0.0018 (19)
C280.023 (2)0.033 (3)0.0167 (18)0.0017 (18)0.0008 (15)0.0019 (17)
C290.023 (2)0.035 (3)0.0171 (18)0.0020 (18)0.0009 (15)0.0051 (17)
O190.0340 (19)0.021 (2)0.0340 (19)0.0080 (16)0.0050 (15)0.0037 (16)
O200.102 (3)0.025 (3)0.059 (3)0.008 (2)0.018 (2)0.0067 (19)
O210.053 (2)0.035 (2)0.0337 (18)0.0079 (15)0.0145 (16)0.0002 (15)
O220.027 (3)0.067 (5)0.057 (3)0.006 (3)0.020 (2)0.005 (3)
O230.053 (2)0.095 (4)0.068 (3)0.034 (2)0.036 (2)0.015 (2)
O240.048 (2)0.036 (2)0.0345 (18)0.0077 (15)0.0155 (15)0.0005 (15)
O250.062 (3)0.023 (3)0.067 (3)0.009 (2)0.018 (2)0.001 (2)
O260.0282 (18)0.077 (3)0.044 (2)0.0052 (17)0.0063 (14)0.0071 (19)
O270.053 (2)0.048 (3)0.0244 (17)0.0070 (17)0.0002 (14)0.0015 (15)
O280.0419 (19)0.046 (2)0.0319 (17)0.0239 (17)0.0002 (14)0.0061 (15)
O290.0401 (18)0.037 (2)0.0397 (18)0.0215 (16)0.0017 (14)0.0079 (15)
P10.0145 (4)0.0138 (6)0.0164 (4)0.0010 (4)0.0014 (3)0.0008 (4)
Ru10.01498 (14)0.0178 (2)0.01538 (15)0.00075 (12)0.00039 (10)0.00176 (12)
Ru20.02312 (17)0.0193 (2)0.02001 (17)0.00484 (12)0.00010 (12)0.00004 (12)
Ru30.02062 (17)0.0153 (2)0.01712 (17)0.00574 (13)0.00194 (12)0.00007 (13)
Co10.0185 (2)0.0265 (3)0.0141 (2)0.00057 (19)0.00223 (17)0.00059 (19)
Ru3B0.0185 (2)0.0265 (3)0.0141 (2)0.00057 (19)0.00223 (17)0.00059 (19)
Co1B0.02062 (17)0.0153 (2)0.01712 (17)0.00574 (13)0.00194 (12)0.00007 (13)
Geometric parameters (Å, º) top
C1—C21.531 (5)C21—Ru21.912 (4)
C1—C61.534 (6)C22—O221.133 (13)
C1—P11.866 (4)C22—Ru21.922 (11)
C2—C31.545 (6)C23—O231.142 (6)
C3—C41.504 (7)C23—Ru31.897 (5)
C4—C51.521 (7)C24—O241.128 (5)
C5—C61.535 (6)C24—Ru31.909 (4)
C7—C81.527 (6)C25—O251.134 (7)
C7—C121.545 (6)C25—Ru31.934 (7)
C7—P11.849 (4)C26—O261.143 (5)
C8—C91.549 (7)C26—Co11.795 (5)
C9—C101.525 (9)C27—O271.133 (5)
C10—C111.491 (8)C27—Co11.826 (4)
C11—C121.520 (6)C28—O281.140 (5)
C13—C141.521 (5)C28—Ru11.889 (4)
C13—C181.526 (5)C29—O291.142 (5)
C13—P11.908 (4)C29—Ru11.890 (4)
C14—C151.530 (5)P1—Ru12.3651 (9)
C15—C161.514 (6)Ru1—Co12.7179 (6)
C16—C171.509 (7)Ru1—Ru32.9240 (5)
C17—C181.534 (5)Ru1—Ru22.9408 (5)
C19—O191.151 (6)Ru2—Co12.7041 (6)
C19—Co11.853 (5)Ru2—Ru32.8331 (5)
C19—Ru22.392 (5)Ru3—Co12.7592 (6)
C20—O201.144 (7)C22B—O22B1.20 (9)
C20—Ru21.917 (6)C25B—O25B1.19 (5)
C21—O211.125 (5)C19B—O19B1.17 (3)
C2—C1—C6110.1 (3)P1—Ru1—Ru2117.89 (3)
C2—C1—P1115.7 (3)Co1—Ru1—Ru256.929 (14)
C6—C1—P1112.8 (3)Ru3—Ru1—Ru257.772 (12)
C1—C2—C3110.2 (3)C21—Ru2—C2095.91 (19)
C4—C3—C2111.3 (4)C21—Ru2—C2292.7 (3)
C3—C4—C5111.0 (4)C20—Ru2—C2294.5 (4)
C4—C5—C6111.2 (4)C21—Ru2—C1989.98 (17)
C1—C6—C5111.3 (4)C20—Ru2—C1978.3 (2)
C8—C7—C12109.9 (4)C22—Ru2—C19172.5 (4)
C8—C7—P1114.2 (3)C21—Ru2—Co188.55 (13)
C12—C7—P1112.4 (3)C20—Ru2—Co1120.26 (15)
C7—C8—C9109.2 (4)C22—Ru2—Co1144.9 (4)
C10—C9—C8111.9 (4)C19—Ru2—Co142.10 (13)
C11—C10—C9111.6 (4)C21—Ru2—Ru391.95 (13)
C10—C11—C12111.1 (5)C20—Ru2—Ru3172.13 (13)
C11—C12—C7110.5 (4)C22—Ru2—Ru385.2 (4)
C14—C13—C18110.2 (3)C19—Ru2—Ru3101.70 (13)
C14—C13—P1114.1 (3)Co1—Ru2—Ru359.720 (15)
C18—C13—P1114.1 (3)C21—Ru2—Ru1143.40 (13)
C13—C14—C15110.7 (3)C20—Ru2—Ru1112.01 (14)
C16—C15—C14111.6 (4)C22—Ru2—Ru1107.5 (3)
C17—C16—C15110.9 (4)C19—Ru2—Ru173.91 (11)
C16—C17—C18112.1 (4)Co1—Ru2—Ru157.380 (13)
C13—C18—C17110.6 (3)Ru3—Ru2—Ru160.817 (11)
O19—C19—Co1153.4 (4)C23—Ru3—C2494.2 (2)
O19—C19—Ru2128.5 (4)C23—Ru3—C2595.1 (3)
Co1—C19—Ru278.00 (18)C24—Ru3—C2595.4 (2)
O20—C20—Ru2177.8 (4)C23—Ru3—Co1151.54 (17)
O21—C21—Ru2179.3 (4)C24—Ru3—Co189.02 (13)
O22—C22—Ru2174.8 (12)C25—Ru3—Co1112.8 (2)
O23—C23—Ru3175.7 (5)C23—Ru3—Ru293.79 (17)
O24—C24—Ru3178.4 (4)C24—Ru3—Ru291.52 (14)
O25—C25—Ru3176.7 (5)C25—Ru3—Ru2168.26 (18)
O26—C26—Co1177.2 (5)Co1—Ru3—Ru257.817 (14)
O27—C27—Co1176.5 (4)C23—Ru3—Ru1109.98 (14)
O28—C28—Ru1176.7 (4)C24—Ru3—Ru1143.92 (13)
O29—C29—Ru1176.3 (4)C25—Ru3—Ru1108.16 (16)
C7—P1—C1103.99 (19)Co1—Ru3—Ru157.052 (13)
C7—P1—C13104.30 (18)Ru2—Ru3—Ru161.412 (12)
C1—P1—C13104.45 (18)C26—Co1—C27100.53 (19)
C7—P1—Ru1115.56 (13)C26—Co1—C1995.3 (2)
C1—P1—Ru1111.79 (12)C27—Co1—C1998.6 (2)
C13—P1—Ru1115.48 (11)C26—Co1—Ru2141.68 (14)
C28—Ru1—C2995.89 (19)C27—Co1—Ru2111.12 (14)
C28—Ru1—P193.64 (12)C19—Co1—Ru259.91 (14)
C29—Ru1—P191.71 (12)C26—Co1—Ru186.35 (13)
C28—Ru1—Co191.08 (11)C27—Co1—Ru1169.91 (14)
C29—Ru1—Co192.22 (12)C19—Co1—Ru188.00 (13)
P1—Ru1—Co1173.52 (3)Ru2—Co1—Ru165.690 (15)
C28—Ru1—Ru3147.60 (12)C26—Co1—Ru3129.34 (16)
C29—Ru1—Ru395.94 (12)C27—Co1—Ru3105.40 (13)
P1—Ru1—Ru3116.02 (3)C19—Co1—Ru3122.19 (15)
Co1—Ru1—Ru358.420 (14)Ru2—Co1—Ru362.463 (15)
C28—Ru1—Ru297.90 (13)Ru1—Co1—Ru364.528 (15)
C29—Ru1—Ru2146.22 (12)
C6—C1—C2—C356.7 (5)C13—C14—C15—C1656.9 (5)
P1—C1—C2—C3173.9 (3)C14—C15—C16—C1755.2 (6)
C1—C2—C3—C457.7 (5)C15—C16—C17—C1854.6 (5)
C2—C3—C4—C556.9 (5)C14—C13—C18—C1756.4 (5)
C3—C4—C5—C655.7 (5)P1—C13—C18—C17173.6 (3)
C2—C1—C6—C556.3 (5)C16—C17—C18—C1355.6 (5)
P1—C1—C6—C5172.8 (3)C8—C7—P1—C154.2 (3)
C4—C5—C6—C155.6 (5)C12—C7—P1—C1179.8 (3)
C12—C7—C8—C957.3 (5)C8—C7—P1—C13163.4 (3)
P1—C7—C8—C9175.4 (3)C12—C7—P1—C1370.6 (3)
C7—C8—C9—C1055.6 (5)C2—C1—P1—C745.0 (3)
C8—C9—C10—C1155.1 (6)C6—C1—P1—C7173.1 (3)
C9—C10—C11—C1255.8 (6)C2—C1—P1—C1364.1 (3)
C10—C11—C12—C758.1 (5)C6—C1—P1—C1364.0 (3)
C8—C7—C12—C1159.3 (5)C14—C13—P1—C799.6 (3)
P1—C7—C12—C11172.4 (3)C18—C13—P1—C728.3 (3)
C18—C13—C14—C1557.3 (5)C14—C13—P1—C1151.5 (3)
P1—C13—C14—C15172.8 (3)C18—C13—P1—C180.5 (3)
 

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