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The structure of the title compound, [Co2(C8H18Sn2)(CO)6], a distannyl-substituted dicobaltatetrahedrane, shows geo­metrical parameters noticeably different from those observed in the only monostannyl-substituted dicobaltatetrahedrane structurally studied so far. Thus, the complexed acetyl­enic bond in the title compound is shorter, and the cobalt–cobalt and cobalt–carbon bonds are longer, while the Sn—C—C angles are much smaller than in the complex with monostannyl-substituted ligand.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801016154/ya6054sup1.cif
Contains datablocks I, c624

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801016154/ya6054Isup2.hkl
Contains datablock I

CCDC reference: 175981

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.034
  • wR factor = 0.091
  • Data-to-parameter ratio = 21.0

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
ABSTM_02 Alert C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.620 0.997 Tmin and Tmax expected: 0.490 0.906 RR = 1.149 Please check that your absorption correction is appropriate. PLAT_320 Alert C Check Hybridisation of C(7) in main residue ? PLAT_320 Alert C Check Hybridisation of C(8) in main residue ? General Notes
ABSTM_02 When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.908 Tmax scaled 0.906 Tmin scaled 0.563
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
3 Alert Level C = Please check

Comment top

The title compound (I) was prepared thirty years ago, but the nature of the bonding in the crystal remained unknown until now. The tin–carbon bond in stannyl alkynes is relatively labile, though these can be used in Stille-type palladium-catalysed cross-coupling reactions with organyl halides (Mitchell, 1998). However, the reactivity of the carbon–carbon triple bond is such that oligomeric and polymeric side-products are obtained in large amounts. Complexation of the carbon–carbon triple bond by the dicobalt hexacarbonyl moiety to give a dicobaltatetrahedrane structure does not hinder cross-coupling with activated organyl halides (Zavgorodnii et al., 2000). The title compound is air- and moisture-insensitive, whereas the uncomplexed bis(trimethylstannyl)acetylene is easily hydrolysed by atmospheric moisture.

Only one dicobaltatetrahedrane derived from a stannyl alkyne has so far been studied by X-ray crystallography (Wrackmeyer et al., 1997) but this compound (A) could be atypical for steric reasons, as it is prepared by reacting diphenyldiethynyltin Ph2Sn(CCH)2 with dicobalt octacarbonyl, both acetylenic bonds being converted to dicobaltatetrahedrane moieties.

The structure of (I) is shown in Fig. 1. The length of the complexed acetylenic triple bond in this structure is 1.309 (5) Å, as compared with 1.238 Å in the uncomplexed stannyl acetylene and 1.212 (1) Å in acetylene itself (Khaikin et al., 2000); it is markedly shorter than in (A) [1.322 (9) and 1.335 (9) Å]. The cobalt–cobalt distance (2.5043 (9) Å) is considerably longer than in (A) [2.4788 (2) and 2.487 (2) Å]. While in (A) the cobalt–carbon bond lengths in the dicobaltatetrahedrane moiety lie between 1.944 and 1.990 Å (the authors describe these as "normal" values), all four Co—C bonds in the title compound are equal or longer than 2.000 Å (up to 2.007 Å). The originally linear Sn—C—C—Sn arrangement is naturally considerably bent, the angles Sn—C—C being 144.7 (3)° and 145.7 (3)°; in (A), however, the bond angles are much larger at 150.5 (5) and 151.5 (5)°.

Experimental top

The compound was prepared in 66% yield as a dark red solid, decomposing at 373 K, according to the procedure described previously (Seyferth & White, 1971).

Refinement top

Hydrogen atoms were placed in calculated positions and included in the refinement in the riding motion approximation with Uiso constrained to be 1.5 times Ueq of the carrier atom for the methyl-H and 1.2 times Ueq for the remaining H atoms. The highest peak in the final difference map is at a distance of 0.84 Å from Sn2.

Structure description top

The title compound (I) was prepared thirty years ago, but the nature of the bonding in the crystal remained unknown until now. The tin–carbon bond in stannyl alkynes is relatively labile, though these can be used in Stille-type palladium-catalysed cross-coupling reactions with organyl halides (Mitchell, 1998). However, the reactivity of the carbon–carbon triple bond is such that oligomeric and polymeric side-products are obtained in large amounts. Complexation of the carbon–carbon triple bond by the dicobalt hexacarbonyl moiety to give a dicobaltatetrahedrane structure does not hinder cross-coupling with activated organyl halides (Zavgorodnii et al., 2000). The title compound is air- and moisture-insensitive, whereas the uncomplexed bis(trimethylstannyl)acetylene is easily hydrolysed by atmospheric moisture.

Only one dicobaltatetrahedrane derived from a stannyl alkyne has so far been studied by X-ray crystallography (Wrackmeyer et al., 1997) but this compound (A) could be atypical for steric reasons, as it is prepared by reacting diphenyldiethynyltin Ph2Sn(CCH)2 with dicobalt octacarbonyl, both acetylenic bonds being converted to dicobaltatetrahedrane moieties.

The structure of (I) is shown in Fig. 1. The length of the complexed acetylenic triple bond in this structure is 1.309 (5) Å, as compared with 1.238 Å in the uncomplexed stannyl acetylene and 1.212 (1) Å in acetylene itself (Khaikin et al., 2000); it is markedly shorter than in (A) [1.322 (9) and 1.335 (9) Å]. The cobalt–cobalt distance (2.5043 (9) Å) is considerably longer than in (A) [2.4788 (2) and 2.487 (2) Å]. While in (A) the cobalt–carbon bond lengths in the dicobaltatetrahedrane moiety lie between 1.944 and 1.990 Å (the authors describe these as "normal" values), all four Co—C bonds in the title compound are equal or longer than 2.000 Å (up to 2.007 Å). The originally linear Sn—C—C—Sn arrangement is naturally considerably bent, the angles Sn—C—C being 144.7 (3)° and 145.7 (3)°; in (A), however, the bond angles are much larger at 150.5 (5) and 151.5 (5)°.

Computing details top

Data collection: CAD4 Version 5.0 (Nonius, 1989); cell refinement: CAD4 Version 5.0 (Nonius, 1989); data reduction: XCAD4 (Harms, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997), PARST95 (Nardelli, 1995).

Figures top
[Figure 1] Fig. 1. : View of the title compound showing the labelling of all non-H atoms. Displacement ellipsoids are shown at the 30% probability level. H atoms are omitted for clarity.
(I) top
Crystal data top
[Co2(C8H18Sn2)(CO)6]Z = 2
Mr = 637.52F(000) = 608
Triclinic, P1Dx = 1.942 Mg m3
a = 8.659 (4) ÅAg Kα radiation, λ = 0.56083 Å
b = 10.0360 (17) ÅCell parameters from 25 reflections
c = 13.292 (3) Åθ = 12.1–15.4°
α = 91.731 (16)°µ = 1.98 mm1
β = 91.17 (3)°T = 293 K
γ = 109.09 (2)°Plate, red-brown
V = 1090.5 (6) Å30.40 × 0.30 × 0.05 mm
Data collection top
Nonius CAD-4
diffractometer
3813 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.019
Graphite monochromatorθmax = 21.0°, θmin = 3.0°
ω/2θ scansh = 1111
Absorption correction: ψ scan
(WinGX; Farrugia, 1999; North et al., 1968)
k = 1212
Tmin = 0.620, Tmax = 0.997l = 1616
9426 measured reflections3 standard reflections every 60 min
4713 independent reflections intensity decay: none
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.034H-atom parameters constrained
wR(F2) = 0.091 w = 1/[σ2(Fo2) + (0.0639P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.002
4713 reflectionsΔρmax = 1.15 e Å3
224 parametersΔρmin = 1.54 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0075 (11)
Crystal data top
[Co2(C8H18Sn2)(CO)6]γ = 109.09 (2)°
Mr = 637.52V = 1090.5 (6) Å3
Triclinic, P1Z = 2
a = 8.659 (4) ÅAg Kα radiation, λ = 0.56083 Å
b = 10.0360 (17) ŵ = 1.98 mm1
c = 13.292 (3) ÅT = 293 K
α = 91.731 (16)°0.40 × 0.30 × 0.05 mm
β = 91.17 (3)°
Data collection top
Nonius CAD-4
diffractometer
3813 reflections with I > 2σ(I)
Absorption correction: ψ scan
(WinGX; Farrugia, 1999; North et al., 1968)
Rint = 0.019
Tmin = 0.620, Tmax = 0.9973 standard reflections every 60 min
9426 measured reflections intensity decay: none
4713 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0340 restraints
wR(F2) = 0.091H-atom parameters constrained
S = 1.03Δρmax = 1.15 e Å3
4713 reflectionsΔρmin = 1.54 e Å3
224 parameters
Special details top

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*/Ueq
Sn10.23433 (3)0.46053 (3)0.251823 (19)0.04642 (10)
Sn20.54726 (3)0.94962 (3)0.21592 (2)0.04575 (10)
Co10.09136 (6)0.76295 (5)0.17469 (4)0.04472 (14)
Co20.16469 (6)0.78922 (6)0.35914 (4)0.04702 (14)
O10.0671 (6)1.0421 (4)0.1399 (4)0.1016 (13)
O20.2450 (5)0.5692 (5)0.1871 (4)0.1063 (15)
O30.1587 (6)0.6853 (6)0.0283 (3)0.1123 (15)
O40.1387 (6)0.5951 (6)0.4359 (4)0.126 (2)
O50.1589 (6)1.0769 (4)0.3971 (3)0.1030 (14)
O60.3909 (6)0.7805 (5)0.5218 (3)0.1100 (16)
C10.0780 (6)0.9363 (5)0.1549 (3)0.0631 (11)
C20.1150 (5)0.6445 (5)0.1830 (3)0.0638 (11)
C30.1323 (6)0.7160 (5)0.0501 (3)0.0666 (11)
C40.0236 (7)0.6703 (6)0.4058 (4)0.0759 (14)
C50.1607 (6)0.9664 (5)0.3817 (3)0.0643 (11)
C60.3017 (6)0.7841 (5)0.4595 (3)0.0662 (12)
C70.2264 (4)0.6713 (4)0.2535 (3)0.0418 (7)
C80.3120 (4)0.8039 (4)0.2425 (3)0.0412 (7)
C90.4148 (6)0.4613 (6)0.3624 (4)0.0697 (12)
H9A0.52130.50990.33810.105*
H9B0.40660.36600.37620.105*
H9C0.39800.50850.42310.105*
C100.3025 (8)0.4188 (6)0.1041 (4)0.0757 (14)
H10A0.41680.46820.09650.114*
H10B0.23980.45000.05540.114*
H10C0.28150.31920.09380.114*
C110.0033 (6)0.3260 (5)0.2861 (4)0.0756 (14)
H11A0.00110.23430.30100.113*
H11B0.07650.31790.22930.113*
H11C0.04180.36500.34340.113*
C120.5244 (6)1.1542 (4)0.2171 (4)0.0655 (11)
H12A0.41921.14820.18900.098*
H12B0.60851.21500.17770.098*
H12C0.53511.19180.28510.098*
C130.7062 (6)0.9255 (6)0.3335 (4)0.0750 (13)
H13A0.66630.94390.39750.113*
H13B0.81410.99070.32550.113*
H13C0.70970.83080.33040.113*
C140.6169 (7)0.8873 (7)0.0737 (4)0.0803 (15)
H14A0.63230.79720.07860.120*
H14B0.71710.95610.05470.120*
H14C0.53260.88050.02390.120*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn10.04805 (17)0.04004 (15)0.05211 (17)0.01603 (11)0.00076 (11)0.00017 (10)
Sn20.03709 (15)0.04657 (16)0.05209 (16)0.01188 (11)0.00044 (10)0.00039 (10)
Co10.0395 (3)0.0487 (3)0.0464 (3)0.0152 (2)0.00260 (19)0.0017 (2)
Co20.0472 (3)0.0536 (3)0.0437 (3)0.0215 (2)0.0020 (2)0.0023 (2)
O10.120 (4)0.073 (2)0.127 (4)0.053 (3)0.000 (3)0.019 (2)
O20.052 (2)0.123 (4)0.116 (3)0.008 (2)0.001 (2)0.009 (3)
O30.129 (4)0.156 (4)0.054 (2)0.052 (3)0.002 (2)0.013 (2)
O40.085 (3)0.158 (5)0.101 (3)0.010 (3)0.039 (3)0.016 (3)
O50.136 (4)0.078 (3)0.113 (3)0.063 (3)0.021 (3)0.028 (2)
O60.126 (4)0.160 (5)0.066 (2)0.082 (3)0.028 (2)0.009 (3)
C10.058 (3)0.070 (3)0.067 (3)0.029 (2)0.008 (2)0.005 (2)
C20.046 (2)0.075 (3)0.064 (3)0.012 (2)0.0060 (18)0.002 (2)
C30.064 (3)0.088 (3)0.048 (2)0.026 (2)0.0059 (19)0.004 (2)
C40.071 (3)0.094 (4)0.057 (3)0.020 (3)0.014 (2)0.003 (2)
C50.067 (3)0.077 (3)0.060 (2)0.042 (2)0.007 (2)0.010 (2)
C60.080 (3)0.083 (3)0.044 (2)0.040 (3)0.003 (2)0.0070 (19)
C70.0419 (18)0.0432 (17)0.0431 (17)0.0182 (14)0.0008 (13)0.0003 (13)
C80.0364 (16)0.0440 (17)0.0446 (18)0.0153 (14)0.0009 (13)0.0002 (14)
C90.069 (3)0.078 (3)0.071 (3)0.038 (3)0.011 (2)0.001 (2)
C100.096 (4)0.076 (3)0.063 (3)0.040 (3)0.008 (2)0.011 (2)
C110.061 (3)0.057 (3)0.096 (4)0.002 (2)0.002 (2)0.010 (2)
C120.064 (3)0.043 (2)0.086 (3)0.0130 (19)0.004 (2)0.000 (2)
C130.055 (3)0.090 (3)0.080 (3)0.024 (2)0.017 (2)0.007 (3)
C140.081 (4)0.101 (4)0.064 (3)0.038 (3)0.015 (3)0.007 (3)
Geometric parameters (Å, º) top
Sn1—C92.121 (5)O4—C41.125 (6)
Sn1—C112.127 (5)O5—C51.127 (6)
Sn1—C102.131 (5)O6—C61.130 (6)
Sn1—C72.138 (3)C7—C81.309 (5)
Sn2—C122.126 (4)C9—H9A0.9600
Sn2—C82.127 (4)C9—H9B0.9600
Sn2—C132.133 (5)C9—H9C0.9600
Sn2—C142.133 (5)C10—H10A0.9600
Co1—C31.781 (5)C10—H10B0.9600
Co1—C21.801 (5)C10—H10C0.9600
Co1—C11.808 (5)C11—H11A0.9600
Co1—C72.006 (4)C11—H11B0.9600
Co1—C82.006 (4)C11—H11C0.9600
Co1—Co22.5043 (9)C12—H12A0.9600
Co2—C61.780 (5)C12—H12B0.9600
Co2—C51.806 (5)C12—H12C0.9600
Co2—C41.811 (5)C13—H13A0.9600
Co2—C72.000 (3)C13—H13B0.9600
Co2—C82.007 (4)C13—H13C0.9600
O1—C11.119 (6)C14—H14A0.9600
O2—C21.136 (6)C14—H14B0.9600
O3—C31.127 (6)C14—H14C0.9600
C9—Sn1—C11112.9 (2)C8—C7—Co271.2 (2)
C9—Sn1—C10112.0 (2)C8—C7—Co171.0 (2)
C11—Sn1—C10112.4 (2)Co2—C7—Co177.38 (12)
C9—Sn1—C7105.74 (17)C8—C7—Sn1144.7 (3)
C11—Sn1—C7107.10 (18)Co2—C7—Sn1132.34 (18)
C10—Sn1—C7106.14 (17)Co1—C7—Sn1132.51 (18)
C12—Sn2—C8107.24 (17)C7—C8—Co170.9 (2)
C12—Sn2—C13113.1 (2)C7—C8—Co270.7 (2)
C8—Sn2—C13106.30 (17)Co1—C8—Co277.22 (13)
C12—Sn2—C14113.0 (2)C7—C8—Sn2145.7 (3)
C8—Sn2—C14106.23 (19)Co1—C8—Sn2133.33 (18)
C13—Sn2—C14110.5 (2)Co2—C8—Sn2130.94 (17)
C3—Co1—C299.2 (2)Sn1—C9—H9A109.5
C3—Co1—C1100.1 (2)Sn1—C9—H9B109.5
C2—Co1—C1106.8 (2)H9A—C9—H9B109.5
C3—Co1—C799.67 (19)Sn1—C9—H9C109.5
C2—Co1—C7104.20 (19)H9A—C9—H9C109.5
C1—Co1—C7139.71 (18)H9B—C9—H9C109.5
C3—Co1—C8100.80 (19)Sn1—C10—H10A109.5
C2—Co1—C8139.81 (18)Sn1—C10—H10B109.5
C1—Co1—C8103.50 (18)H10A—C10—H10B109.5
C7—Co1—C838.10 (14)Sn1—C10—H10C109.5
C3—Co1—Co2149.37 (16)H10A—C10—H10C109.5
C2—Co1—Co297.65 (15)H10B—C10—H10C109.5
C1—Co1—Co299.27 (15)Sn1—C11—H11A109.5
C7—Co1—Co251.21 (10)Sn1—C11—H11B109.5
C8—Co1—Co251.39 (10)H11A—C11—H11B109.5
C6—Co2—C599.0 (2)Sn1—C11—H11C109.5
C6—Co2—C499.5 (2)H11A—C11—H11C109.5
C5—Co2—C4107.0 (3)H11B—C11—H11C109.5
C6—Co2—C7100.43 (18)Sn2—C12—H12A109.5
C5—Co2—C7140.47 (19)Sn2—C12—H12B109.5
C4—Co2—C7103.3 (2)H12A—C12—H12B109.5
C6—Co2—C899.72 (19)Sn2—C12—H12C109.5
C5—Co2—C8104.60 (19)H12A—C12—H12C109.5
C4—Co2—C8139.60 (19)H12B—C12—H12C109.5
C7—Co2—C838.15 (14)Sn2—C13—H13A109.5
C6—Co2—Co1149.34 (15)Sn2—C13—H13B109.5
C5—Co2—Co198.63 (15)H13A—C13—H13B109.5
C4—Co2—Co199.08 (17)Sn2—C13—H13C109.5
C7—Co2—Co151.41 (10)H13A—C13—H13C109.5
C8—Co2—Co151.39 (10)H13B—C13—H13C109.5
O1—C1—Co1177.9 (5)Sn2—C14—H14A109.5
O2—C2—Co1179.2 (5)Sn2—C14—H14B109.5
O3—C3—Co1179.3 (5)H14A—C14—H14B109.5
O4—C4—Co2178.6 (6)Sn2—C14—H14C109.5
O5—C5—Co2179.0 (4)H14A—C14—H14C109.5
O6—C6—Co2178.6 (5)H14B—C14—H14C109.5
C3—Co1—Co2—C66.1 (5)C11—Sn1—C7—C8179.0 (5)
C2—Co1—Co2—C6129.0 (4)C10—Sn1—C7—C860.8 (5)
C1—Co1—Co2—C6122.5 (4)C9—Sn1—C7—Co263.9 (3)
C7—Co1—Co2—C626.9 (4)C11—Sn1—C7—Co256.7 (3)
C8—Co1—Co2—C622.5 (4)C10—Sn1—C7—Co2177.0 (3)
C3—Co1—Co2—C5130.5 (4)C9—Sn1—C7—Co1179.6 (2)
C2—Co1—Co2—C5106.6 (2)C11—Sn1—C7—Co159.0 (3)
C1—Co1—Co2—C51.9 (2)C10—Sn1—C7—Co161.3 (3)
C7—Co1—Co2—C5151.3 (2)Co2—C7—C8—Co182.72 (10)
C8—Co1—Co2—C5101.8 (2)Sn1—C7—C8—Co1138.6 (4)
C3—Co1—Co2—C4120.6 (4)Co1—C7—C8—Co282.72 (10)
C2—Co1—Co2—C42.3 (2)Sn1—C7—C8—Co2138.6 (4)
C1—Co1—Co2—C4110.8 (3)Co2—C7—C8—Sn2135.9 (5)
C7—Co1—Co2—C499.8 (2)Co1—C7—C8—Sn2141.4 (5)
C8—Co1—Co2—C4149.2 (2)Sn1—C7—C8—Sn22.8 (8)
C3—Co1—Co2—C720.8 (3)C3—Co1—C8—C791.9 (3)
C2—Co1—Co2—C7102.1 (2)C2—Co1—C8—C726.6 (4)
C1—Co1—Co2—C7149.4 (2)C1—Co1—C8—C7164.9 (3)
C8—Co1—Co2—C749.44 (18)Co2—Co1—C8—C773.7 (2)
C3—Co1—Co2—C828.6 (4)C3—Co1—C8—Co2165.62 (18)
C2—Co1—Co2—C8151.5 (2)C2—Co1—C8—Co247.1 (3)
C1—Co1—Co2—C899.9 (2)C1—Co1—C8—Co291.17 (18)
C7—Co1—Co2—C849.44 (18)C7—Co1—C8—Co273.7 (2)
C6—Co2—C7—C892.5 (3)C3—Co1—C8—Sn259.2 (3)
C5—Co2—C7—C825.7 (4)C2—Co1—C8—Sn2177.7 (3)
C4—Co2—C7—C8165.0 (3)C1—Co1—C8—Sn244.1 (3)
Co1—Co2—C7—C873.9 (2)C7—Co1—C8—Sn2151.1 (4)
C6—Co2—C7—Co1166.43 (19)Co2—Co1—C8—Sn2135.2 (3)
C5—Co2—C7—Co148.3 (3)C6—Co2—C8—C794.6 (3)
C4—Co2—C7—Co191.1 (2)C5—Co2—C8—C7163.5 (2)
C8—Co2—C7—Co173.9 (2)C4—Co2—C8—C722.8 (4)
C6—Co2—C7—Sn156.4 (3)Co1—Co2—C8—C774.0 (2)
C5—Co2—C7—Sn1174.6 (3)C6—Co2—C8—Co1168.56 (18)
C4—Co2—C7—Sn146.0 (3)C5—Co2—C8—Co189.44 (17)
C8—Co2—C7—Sn1148.9 (4)C4—Co2—C8—Co151.2 (4)
Co1—Co2—C7—Sn1137.1 (3)C7—Co2—C8—Co174.0 (2)
C3—Co1—C7—C895.2 (3)C6—Co2—C8—Sn254.1 (3)
C2—Co1—C7—C8162.6 (2)C5—Co2—C8—Sn247.9 (3)
C1—Co1—C7—C823.1 (4)C4—Co2—C8—Sn2171.5 (3)
Co2—Co1—C7—C874.2 (2)C7—Co2—C8—Sn2148.7 (4)
C3—Co1—C7—Co2169.41 (18)Co1—Co2—C8—Sn2137.3 (3)
C2—Co1—C7—Co288.44 (18)C12—Sn2—C8—C7179.1 (5)
C1—Co1—C7—Co251.1 (3)C13—Sn2—C8—C757.9 (5)
C8—Co1—C7—Co274.2 (2)C14—Sn2—C8—C759.8 (5)
C3—Co1—C7—Sn153.6 (3)C12—Sn2—C8—Co155.0 (3)
C2—Co1—C7—Sn148.5 (3)C13—Sn2—C8—Co1176.3 (3)
C1—Co1—C7—Sn1172.0 (3)C14—Sn2—C8—Co166.0 (3)
C8—Co1—C7—Sn1148.8 (4)C12—Sn2—C8—Co259.5 (3)
Co2—Co1—C7—Sn1137.0 (3)C13—Sn2—C8—Co261.7 (3)
C9—Sn1—C7—C858.3 (5)C14—Sn2—C8—Co2179.4 (3)

Experimental details

Crystal data
Chemical formula[Co2(C8H18Sn2)(CO)6]
Mr637.52
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)8.659 (4), 10.0360 (17), 13.292 (3)
α, β, γ (°)91.731 (16), 91.17 (3), 109.09 (2)
V3)1090.5 (6)
Z2
Radiation typeAg Kα, λ = 0.56083 Å
µ (mm1)1.98
Crystal size (mm)0.40 × 0.30 × 0.05
Data collection
DiffractometerNonius CAD-4
Absorption correctionψ scan
(WinGX; Farrugia, 1999; North et al., 1968)
Tmin, Tmax0.620, 0.997
No. of measured, independent and
observed [I > 2σ(I)] reflections
9426, 4713, 3813
Rint0.019
(sin θ/λ)max1)0.639
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.034, 0.091, 1.03
No. of reflections4713
No. of parameters224
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.15, 1.54

Computer programs: CAD4 Version 5.0 (Nonius, 1989), XCAD4 (Harms, 1996), SHELXS97 (Sheldrick, 1990), SHELXTL-Plus (Sheldrick, 1991), SHELXL97 (Sheldrick, 1997), PARST95 (Nardelli, 1995).

 

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