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The title compound, [Co2(C25H22P2)(C8H18Sn2)(CO)4], was prepared by displacement of two mol­ecules of carbon monoxide in hexa­carbonyl­dicobalt­[μ,η2-bis-(tri­methyl­stannyl)]­acetyl­ene with a bidentate bis­(di­phenyl­phosphino)­methane ligand. The displacement of carbon monoxide yields the product with substantially increased thermal stability and brings about noticeable changes in the geometry of the dicobaltatetrahedrane moiety, viz. lengthening of the carbon–carbon bond and shortening of the cobalt–cobalt and cobalt–carbon bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801016166/ya6058sup1.cif
Contains datablocks I, c625

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801016166/ya6058Isup2.hkl
Contains datablock I

CCDC reference: 175982

Key indicators

  • Single-crystal X-ray study
  • T = 291 K
  • Mean [sigma](C-C) = 0.008 Å
  • R factor = 0.036
  • wR factor = 0.105
  • Data-to-parameter ratio = 19.9

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
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 0.891 Tmax scaled 0.891 Tmin scaled 0.730
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
2 Alert Level C = Please check

Comment top

The transformation of bis(trimethylstannyl)ethyne into a stannyl-substituted dicobaltatetrahedrane by treating it with dicobalt octacarbonyl `protects' the carbon–carbon triple bond and thus, as expected, also stabilizes the bond between tin and the tetrahedrane moiety. Nevertheless, Stille-type palladium-catalysed carbon–carbon coupling reactions are still possible using activated organyl halides (Zavgorodnii et al., 2000). However, unactivated organyl halides require more rigorous reaction conditions, under which the dicobaltatetrahedrane decomposes.

The title compound (I) was thus prepared by displacing two molecules of carbon monoxide in hexacarbonyldicobalt[µ,η2-bis-(trimethylstannyl)]acetylene (Seyferth & White, 1971; Zachwieja et al., 2001) with bis(diphenylphosphino)methane, a procedure, which, according to literature precedent (Iwasawa & Hiroishi, 1999), should increase the thermal stability of the dicobaltatetrahedrane.

This prediction was correct, the decomposition temperature being increased by 80 K. The differences between the structures of the title compound (Fig. 1) and its carbonyl precursor are subtle: the carbon–carbon bond in the dicobaltatetrahedrane moiety increased in length from 1.309 (5) to 1.335 (5) Å, while the cobalt–cobalt bond contracted slightly from 2.5043 (9) to 2.4972 (8) Å. The cobalt–carbon bonds in the tetrahedrane moiety decreased in length quite considerably, lying between 1.968 (4) and 1.990 (4) Å compared with 2.000 to 2.007 Å in the starting material.

These bond length changes also affect the bond angles in the dicobaltatetrahedrane moiety, particularly at the C(7) atom, where the Sn(1)—C(7)—C(8) angle decreases from 144.7 to 130.3 (3)°, while the Sn(2)—C(8)—C(7) angle remains almost unchanged at 145.3 (3) °. At the same time the angle Sn(1)—C(7)—Co(2) increases from 132.3° to 137.8 (2)°, while Sn(2)—C(8)—Co(1) somewhat decreases from 133.3° to 131.2 (2)°. This asymmetry in bond angles between C(7) and C(8) is reflected in the slightly asymmetric position of the diphosphinomethane moiety, the Co—P bond lengths being 2.2208 (12) and 2.2100 (12) Å respectively.

It is also noteworthy that the bonds between the cobalt atoms and the carbonyl carbons in the title compound are considerably shortened as compared to the analogous bonds in the starting carbonyl complex (the corresonding average values are 1.770 Å and 1.798 Å).

Experimental top

The compound was prepared by stirring hexacarbonyldicobalt[µ,η2-bis-(trimethylstannyl)]acetylene (126 mg, 0.2 mmol) with 79 mg (0.2 mmol) of bis(diphenylphosphino)methane in 10 ml of dry hexane for 5 h under reflux in an inert atmosphere. It was separated by column chromatography (silica gel, hexane/benzene) as a black solid, m.p. 446 K, yield 116 mg (60%).

Refinement top

Hydrogen atoms were placed in calculated positions 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 0.86 Å from Sn2.

Computing details top

Data collection: CAD-4 Software (Nonius, 1989); cell refinement: CAD-4 Software; 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, 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 30% probability level. H atoms are omitted for clarity.
(I) top
Crystal data top
C37H40Co2O4P2Sn2F(000) = 1912
Mr = 965.87Dx = 1.624 Mg m3
Monoclinic, P21/nAg Kα radiation, λ = 0.56083 Å
a = 16.012 (3) ÅCell parameters from 25 reflections
b = 13.761 (2) Åθ = 10.8–12.6°
c = 18.126 (4) ŵ = 1.15 mm1
β = 98.49 (2)°T = 291 K
V = 3950.1 (13) Å3Plate, red-brown
Z = 40.35 × 0.35 × 0.10 mm
Data collection top
CAD-4 Software (Nonius, 1989)
diffractometer
5353 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.053
Graphite monochromatorθmax = 21.0°, θmin = 3.0°
ω scansh = 2020
Absorption correction: ψ scan
(WinGX; Farrugia, 1999; North et al., 1968)
k = 017
Tmin = 0.819, Tmax = 1.000l = 022
8838 measured reflections3 standard reflections every 60 min
8572 independent reflections intensity decay: none
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) = 0.105H-atom parameters constrained
S = 0.99 w = 1/[σ2(Fo2) + (0.054P)2]
where P = (Fo2 + 2Fc2)/3
8572 reflections(Δ/σ)max = 0.002
430 parametersΔρmax = 1.10 e Å3
0 restraintsΔρmin = 0.56 e Å3
Crystal data top
C37H40Co2O4P2Sn2V = 3950.1 (13) Å3
Mr = 965.87Z = 4
Monoclinic, P21/nAg Kα radiation, λ = 0.56083 Å
a = 16.012 (3) ŵ = 1.15 mm1
b = 13.761 (2) ÅT = 291 K
c = 18.126 (4) Å0.35 × 0.35 × 0.10 mm
β = 98.49 (2)°
Data collection top
CAD-4 Software (Nonius, 1989)
diffractometer
5353 reflections with I > 2σ(I)
Absorption correction: ψ scan
(WinGX; Farrugia, 1999; North et al., 1968)
Rint = 0.053
Tmin = 0.819, Tmax = 1.0003 standard reflections every 60 min
8838 measured reflections intensity decay: none
8572 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0360 restraints
wR(F2) = 0.105H-atom parameters constrained
S = 0.99Δρmax = 1.10 e Å3
8572 reflectionsΔρmin = 0.56 e Å3
430 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
Sn10.193158 (19)0.18340 (3)0.656614 (18)0.05000 (10)
Sn20.46323 (2)0.15971 (3)0.760026 (17)0.05477 (11)
Co10.38724 (3)0.14064 (4)0.55660 (3)0.03985 (14)
Co20.38246 (3)0.31459 (4)0.59499 (3)0.03782 (13)
P10.30053 (6)0.15049 (8)0.44928 (6)0.0364 (2)
P20.31796 (6)0.36042 (8)0.48421 (6)0.0374 (2)
O10.5640 (2)0.1503 (4)0.5356 (2)0.0986 (16)
O30.3682 (3)0.0609 (3)0.5990 (2)0.0874 (12)
O50.5627 (2)0.3603 (3)0.6211 (2)0.0827 (12)
O60.3101 (3)0.4638 (3)0.6794 (2)0.0910 (13)
C10.4941 (3)0.1439 (4)0.5415 (3)0.0628 (14)
C20.2429 (2)0.2670 (3)0.4460 (2)0.0373 (9)
H2A0.21950.28270.39490.045*
H2B0.19700.26270.47520.045*
C30.3755 (3)0.0177 (4)0.5801 (3)0.0578 (12)
C50.4920 (3)0.3454 (3)0.6079 (3)0.0509 (11)
C60.3394 (3)0.4056 (4)0.6465 (2)0.0521 (11)
C70.3116 (2)0.2040 (3)0.6199 (2)0.0382 (9)
C80.3898 (3)0.1960 (3)0.6570 (2)0.0421 (9)
C90.2067 (4)0.2284 (5)0.7704 (3)0.0851 (18)
H9A0.24680.18720.80000.128*
H9B0.15310.22380.78790.128*
H9C0.22610.29440.77440.128*
C100.1627 (3)0.0327 (4)0.6441 (3)0.0687 (14)
H10A0.14820.01760.59210.103*
H10B0.11570.01820.66950.103*
H10C0.21050.00550.66510.103*
C110.0955 (3)0.2727 (4)0.5976 (3)0.0711 (15)
H11A0.11710.33690.59190.107*
H11B0.04880.27600.62520.107*
H11C0.07690.24520.54930.107*
C120.5897 (3)0.1339 (5)0.7425 (4)0.092 (2)
H12A0.58970.10430.69450.138*
H12B0.61680.09130.78060.138*
H12C0.61980.19440.74440.138*
C130.4582 (5)0.2781 (5)0.8348 (4)0.112 (3)
H13A0.47590.33650.81270.169*
H13B0.49500.26520.88060.169*
H13C0.40140.28590.84500.169*
C140.4105 (4)0.0339 (4)0.8038 (3)0.0823 (17)
H14A0.36410.05260.82870.123*
H14B0.45290.00230.83870.123*
H14C0.39080.01000.76380.123*
C210.2178 (3)0.0580 (3)0.4361 (2)0.0439 (10)
C220.2428 (3)0.0368 (3)0.4276 (3)0.0616 (13)
H220.29960.05080.42760.074*
C230.1845 (4)0.1108 (4)0.4191 (3)0.0832 (19)
H230.20200.17430.41290.100*
C240.1009 (4)0.0913 (5)0.4199 (3)0.0837 (19)
H240.06160.14140.41370.100*
C250.0755 (3)0.0004 (5)0.4296 (3)0.0789 (17)
H250.01880.01330.43120.095*
C260.1338 (3)0.0760 (4)0.4372 (3)0.0568 (12)
H260.11570.13940.44310.068*
C310.3353 (3)0.1461 (3)0.3574 (2)0.0418 (9)
C320.2758 (3)0.1456 (4)0.2926 (2)0.0566 (12)
H320.21840.14560.29610.068*
C330.3023 (4)0.1452 (4)0.2237 (3)0.0710 (15)
H330.26270.14430.18060.085*
C340.3865 (4)0.1461 (4)0.2186 (3)0.0753 (16)
H340.40420.14590.17190.090*
C350.4441 (4)0.1473 (4)0.2806 (3)0.0750 (16)
H350.50130.14940.27670.090*
C360.4188 (3)0.1456 (4)0.3501 (3)0.0575 (12)
H360.45920.14410.39250.069*
C410.3772 (3)0.3863 (3)0.4080 (2)0.0421 (9)
C420.3366 (3)0.4164 (4)0.3387 (2)0.0546 (11)
H420.27830.42510.33130.066*
C430.3817 (4)0.4336 (4)0.2808 (3)0.0704 (15)
H430.35380.45450.23490.084*
C440.4675 (4)0.4201 (4)0.2904 (3)0.0706 (15)
H440.49740.43040.25090.085*
C450.5090 (3)0.3911 (4)0.3589 (3)0.0660 (14)
H450.56740.38320.36600.079*
C460.4640 (3)0.3738 (4)0.4173 (3)0.0524 (11)
H460.49230.35360.46320.063*
C510.2527 (3)0.4695 (3)0.4834 (2)0.0431 (9)
C520.2942 (3)0.5569 (3)0.4991 (3)0.0636 (13)
H520.35290.55830.50480.076*
C530.2507 (5)0.6419 (4)0.5063 (3)0.0796 (18)
H530.27960.70020.51600.096*
C540.1644 (5)0.6393 (4)0.4991 (3)0.0780 (17)
H540.13480.69570.50680.094*
C550.1214 (4)0.5552 (4)0.4808 (3)0.0712 (15)
H550.06260.55500.47330.085*
C560.1655 (3)0.4702 (4)0.4733 (3)0.0571 (12)
H560.13600.41270.46140.068*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn10.04056 (16)0.0610 (2)0.05002 (18)0.00602 (14)0.01182 (13)0.00162 (15)
Sn20.0606 (2)0.0592 (2)0.03853 (17)0.00040 (16)0.01251 (14)0.00117 (14)
Co10.0348 (3)0.0470 (3)0.0357 (3)0.0069 (2)0.0018 (2)0.0045 (2)
Co20.0352 (3)0.0430 (3)0.0341 (3)0.0035 (2)0.0015 (2)0.0011 (2)
P10.0318 (5)0.0405 (6)0.0355 (5)0.0001 (4)0.0001 (4)0.0022 (4)
P20.0357 (5)0.0406 (6)0.0349 (5)0.0008 (4)0.0023 (4)0.0013 (4)
O10.0362 (19)0.170 (5)0.089 (3)0.020 (2)0.0071 (18)0.036 (3)
O30.129 (4)0.053 (2)0.080 (3)0.013 (2)0.016 (2)0.008 (2)
O50.0404 (19)0.097 (3)0.107 (3)0.0188 (19)0.0006 (19)0.006 (2)
O60.122 (4)0.089 (3)0.066 (2)0.020 (3)0.026 (2)0.025 (2)
C10.044 (3)0.089 (4)0.053 (3)0.010 (3)0.001 (2)0.018 (3)
C20.0307 (19)0.043 (2)0.036 (2)0.0025 (16)0.0009 (15)0.0007 (17)
C30.067 (3)0.061 (3)0.043 (2)0.016 (3)0.000 (2)0.005 (2)
C50.050 (3)0.054 (3)0.047 (2)0.003 (2)0.000 (2)0.001 (2)
C60.060 (3)0.058 (3)0.038 (2)0.002 (2)0.005 (2)0.001 (2)
C70.039 (2)0.041 (2)0.035 (2)0.0033 (17)0.0087 (16)0.0052 (17)
C80.041 (2)0.050 (2)0.033 (2)0.0010 (18)0.0013 (16)0.0020 (18)
C90.091 (4)0.110 (5)0.061 (3)0.014 (4)0.032 (3)0.020 (3)
C100.063 (3)0.070 (3)0.072 (3)0.022 (3)0.006 (3)0.011 (3)
C110.048 (3)0.078 (4)0.089 (4)0.011 (3)0.014 (3)0.000 (3)
C120.055 (3)0.104 (5)0.107 (5)0.001 (3)0.019 (3)0.016 (4)
C130.133 (6)0.108 (6)0.084 (5)0.001 (5)0.025 (4)0.043 (4)
C140.099 (4)0.075 (4)0.075 (4)0.004 (3)0.018 (3)0.026 (3)
C210.040 (2)0.050 (3)0.037 (2)0.0080 (19)0.0067 (17)0.0059 (18)
C220.060 (3)0.050 (3)0.069 (3)0.004 (2)0.007 (2)0.003 (2)
C230.101 (5)0.047 (3)0.093 (4)0.018 (3)0.016 (4)0.010 (3)
C240.087 (5)0.082 (5)0.077 (4)0.047 (4)0.007 (3)0.013 (3)
C250.049 (3)0.111 (5)0.073 (4)0.032 (3)0.002 (2)0.008 (4)
C260.041 (2)0.067 (3)0.060 (3)0.008 (2)0.002 (2)0.005 (2)
C310.046 (2)0.042 (2)0.037 (2)0.0007 (18)0.0024 (17)0.0054 (17)
C320.056 (3)0.071 (3)0.041 (2)0.001 (2)0.000 (2)0.002 (2)
C330.099 (4)0.071 (4)0.038 (3)0.008 (3)0.006 (3)0.008 (2)
C340.101 (5)0.081 (4)0.049 (3)0.007 (3)0.031 (3)0.010 (3)
C350.070 (3)0.099 (5)0.062 (3)0.005 (3)0.028 (3)0.019 (3)
C360.051 (3)0.074 (3)0.048 (3)0.001 (2)0.010 (2)0.009 (2)
C410.043 (2)0.046 (2)0.038 (2)0.0068 (18)0.0050 (17)0.0049 (18)
C420.053 (3)0.064 (3)0.044 (2)0.005 (2)0.001 (2)0.009 (2)
C430.084 (4)0.087 (4)0.040 (3)0.006 (3)0.007 (2)0.013 (3)
C440.077 (4)0.086 (4)0.054 (3)0.010 (3)0.028 (3)0.003 (3)
C450.055 (3)0.086 (4)0.061 (3)0.010 (3)0.023 (2)0.007 (3)
C460.048 (2)0.065 (3)0.046 (3)0.008 (2)0.011 (2)0.003 (2)
C510.050 (2)0.044 (2)0.035 (2)0.0068 (19)0.0050 (17)0.0048 (18)
C520.069 (3)0.047 (3)0.070 (3)0.002 (2)0.005 (3)0.001 (2)
C530.113 (5)0.043 (3)0.079 (4)0.008 (3)0.000 (4)0.002 (3)
C540.111 (5)0.063 (4)0.066 (4)0.030 (4)0.030 (3)0.012 (3)
C550.063 (3)0.080 (4)0.075 (4)0.021 (3)0.024 (3)0.020 (3)
C560.053 (3)0.052 (3)0.068 (3)0.006 (2)0.017 (2)0.012 (2)
Geometric parameters (Å, º) top
Sn1—C72.119 (4)C14—H14A0.9600
Sn1—C92.133 (5)C14—H14B0.9600
Sn1—C102.135 (5)C14—H14C0.9600
Sn1—C112.146 (5)C21—C261.371 (6)
Sn2—C82.115 (4)C21—C221.380 (6)
Sn2—C122.126 (6)C22—C231.374 (7)
Sn2—C132.129 (6)C22—H220.9300
Sn2—C142.131 (5)C23—C241.367 (9)
Co1—C31.761 (6)C23—H230.9300
Co1—C11.772 (5)C24—C251.345 (9)
Co1—C81.968 (4)C24—H240.9300
Co1—C71.989 (4)C25—C261.391 (7)
Co1—P12.2208 (12)C25—H250.9300
Co1—Co22.4972 (8)C26—H260.9300
Co2—C61.762 (5)C31—C361.362 (6)
Co2—C51.786 (5)C31—C321.400 (6)
Co2—C81.975 (4)C32—C331.377 (7)
Co2—C71.990 (4)C32—H320.9300
Co2—P22.2100 (12)C33—C341.366 (8)
P1—C211.827 (4)C33—H330.9300
P1—C311.833 (4)C34—C351.345 (8)
P1—C21.846 (4)C34—H340.9300
P2—C411.823 (4)C35—C361.379 (7)
P2—C21.825 (4)C35—H350.9300
P2—C511.827 (4)C36—H360.9300
O1—C11.145 (6)C41—C461.385 (6)
O3—C31.146 (6)C41—C421.389 (6)
O5—C51.141 (5)C42—C431.382 (7)
O6—C61.140 (6)C42—H420.9300
C2—H2A0.9700C43—C441.371 (7)
C2—H2B0.9700C43—H430.9300
C7—C81.335 (5)C44—C451.379 (7)
C9—H9A0.9600C44—H440.9300
C9—H9B0.9600C45—C461.386 (6)
C9—H9C0.9600C45—H450.9300
C10—H10A0.9600C46—H460.9300
C10—H10B0.9600C51—C561.382 (6)
C10—H10C0.9600C51—C521.384 (6)
C11—H11A0.9600C52—C531.377 (7)
C11—H11B0.9600C52—H520.9300
C11—H11C0.9600C53—C541.369 (8)
C12—H12A0.9600C53—H530.9300
C12—H12B0.9600C54—C551.363 (8)
C12—H12C0.9600C54—H540.9300
C13—H13A0.9600C55—C561.384 (7)
C13—H13B0.9600C55—H550.9300
C13—H13C0.9600C56—H560.9300
C7—Sn1—C9107.26 (19)H11A—C11—H11C109.5
C7—Sn1—C10107.31 (18)H11B—C11—H11C109.5
C9—Sn1—C10111.9 (2)Sn2—C12—H12A109.5
C7—Sn1—C11112.76 (19)Sn2—C12—H12B109.5
C9—Sn1—C11106.1 (2)H12A—C12—H12B109.5
C10—Sn1—C11111.4 (2)Sn2—C12—H12C109.5
C8—Sn2—C12109.0 (2)H12A—C12—H12C109.5
C8—Sn2—C13108.3 (2)H12B—C12—H12C109.5
C12—Sn2—C13110.5 (3)Sn2—C13—H13A109.5
C8—Sn2—C14108.8 (2)Sn2—C13—H13B109.5
C12—Sn2—C14111.0 (2)H13A—C13—H13B109.5
C13—Sn2—C14109.3 (3)Sn2—C13—H13C109.5
C3—Co1—C1101.6 (2)H13A—C13—H13C109.5
C3—Co1—C897.87 (19)H13B—C13—H13C109.5
C1—Co1—C8104.2 (2)Sn2—C14—H14A109.5
C3—Co1—C7100.7 (2)Sn2—C14—H14B109.5
C1—Co1—C7139.65 (19)H14A—C14—H14B109.5
C8—Co1—C739.43 (16)Sn2—C14—H14C109.5
C3—Co1—P1101.25 (15)H14A—C14—H14C109.5
C1—Co1—P1110.84 (16)H14B—C14—H14C109.5
C8—Co1—P1135.34 (12)C26—C21—C22118.2 (4)
C7—Co1—P197.10 (12)C26—C21—P1124.5 (4)
C3—Co1—Co2147.64 (15)C22—C21—P1117.2 (3)
C1—Co1—Co295.10 (18)C23—C22—C21120.7 (5)
C8—Co1—Co250.83 (12)C23—C22—H22119.7
C7—Co1—Co251.14 (11)C21—C22—H22119.7
P1—Co1—Co298.31 (4)C24—C23—C22120.2 (6)
C6—Co2—C5102.4 (2)C24—C23—H23119.9
C6—Co2—C8106.28 (19)C22—C23—H23119.9
C5—Co2—C898.47 (19)C25—C24—C23120.1 (5)
C6—Co2—C798.15 (19)C25—C24—H24120.0
C5—Co2—C7137.22 (19)C23—C24—H24120.0
C8—Co2—C739.35 (16)C24—C25—C26120.2 (6)
C6—Co2—P296.42 (15)C24—C25—H25119.9
C5—Co2—P2111.67 (15)C26—C25—H25119.9
C8—Co2—P2137.17 (12)C21—C26—C25120.6 (5)
C7—Co2—P2102.66 (12)C21—C26—H26119.7
C6—Co2—Co1149.22 (16)C25—C26—H26119.7
C5—Co2—Co1101.22 (15)C36—C31—C32118.3 (4)
C8—Co2—Co150.58 (12)C36—C31—P1121.5 (3)
C7—Co2—Co151.12 (11)C32—C31—P1120.1 (3)
P2—Co2—Co192.85 (4)C33—C32—C31119.9 (5)
C21—P1—C3199.74 (19)C33—C32—H32120.1
C21—P1—C2104.58 (19)C31—C32—H32120.1
C31—P1—C2102.51 (18)C34—C33—C32120.1 (5)
C21—P1—Co1114.82 (13)C34—C33—H33120.0
C31—P1—Co1123.99 (14)C32—C33—H33120.0
C2—P1—Co1109.05 (12)C35—C34—C33120.3 (5)
C41—P2—C2103.70 (18)C35—C34—H34119.8
C41—P2—C51101.19 (19)C33—C34—H34119.8
C2—P2—C51103.40 (18)C34—C35—C36120.4 (5)
C41—P2—Co2121.26 (14)C34—C35—H35119.8
C2—P2—Co2109.71 (13)C36—C35—H35119.8
C51—P2—Co2115.59 (13)C31—C36—C35121.0 (5)
O1—C1—Co1175.4 (4)C31—C36—H36119.5
P2—C2—P1107.55 (18)C35—C36—H36119.5
P2—C2—H2A110.2C46—C41—C42118.4 (4)
P1—C2—H2A110.2C46—C41—P2120.5 (3)
P2—C2—H2B110.2C42—C41—P2121.1 (3)
P1—C2—H2B110.2C43—C42—C41120.7 (5)
H2A—C2—H2B108.5C43—C42—H42119.7
O3—C3—Co1176.5 (4)C41—C42—H42119.7
O5—C5—Co2174.4 (4)C44—C43—C42120.5 (5)
O6—C6—Co2178.8 (5)C44—C43—H43119.8
C8—C7—Co169.4 (2)C42—C43—H43119.8
C8—C7—Co269.7 (2)C43—C44—C45119.7 (5)
Co1—C7—Co277.74 (14)C43—C44—H44120.2
C8—C7—Sn1130.3 (3)C45—C44—H44120.2
Co1—C7—Sn1140.5 (2)C44—C45—C46120.0 (5)
Co2—C7—Sn1137.8 (2)C44—C45—H45120.0
C7—C8—Co171.1 (2)C46—C45—H45120.0
C7—C8—Co270.9 (2)C41—C46—C45120.8 (4)
Co1—C8—Co278.59 (15)C41—C46—H46119.6
C7—C8—Sn2145.3 (3)C45—C46—H46119.6
Co1—C8—Sn2131.2 (2)C56—C51—C52117.8 (4)
Co2—C8—Sn2132.6 (2)C56—C51—P2124.9 (3)
Sn1—C9—H9A109.5C52—C51—P2117.1 (3)
Sn1—C9—H9B109.5C53—C52—C51121.6 (5)
H9A—C9—H9B109.5C53—C52—H52119.2
Sn1—C9—H9C109.5C51—C52—H52119.2
H9A—C9—H9C109.5C54—C53—C52119.1 (6)
H9B—C9—H9C109.5C54—C53—H53120.4
Sn1—C10—H10A109.5C52—C53—H53120.4
Sn1—C10—H10B109.5C55—C54—C53120.8 (5)
H10A—C10—H10B109.5C55—C54—H54119.6
Sn1—C10—H10C109.5C53—C54—H54119.6
H10A—C10—H10C109.5C54—C55—C56119.7 (5)
H10B—C10—H10C109.5C54—C55—H55120.2
Sn1—C11—H11A109.5C56—C55—H55120.2
Sn1—C11—H11B109.5C51—C56—C55120.9 (5)
H11A—C11—H11B109.5C51—C56—H56119.5
Sn1—C11—H11C109.5C55—C56—H56119.5
C3—Co1—Co2—C630.7 (4)Co1—C7—C8—Co284.09 (12)
C1—Co1—Co2—C6152.0 (3)Sn1—C7—C8—Co2136.2 (3)
C8—Co1—Co2—C647.8 (3)Co1—C7—C8—Sn2136.7 (5)
C7—Co1—Co2—C63.6 (3)Co2—C7—C8—Sn2139.2 (5)
P1—Co1—Co2—C696.1 (3)Sn1—C7—C8—Sn23.0 (8)
C3—Co1—Co2—C5108.9 (3)C3—Co1—C8—C797.3 (3)
C1—Co1—Co2—C512.3 (2)C1—Co1—C8—C7158.5 (3)
C8—Co1—Co2—C591.8 (2)P1—Co1—C8—C717.5 (3)
C7—Co1—Co2—C5143.3 (2)Co2—Co1—C8—C773.5 (2)
P1—Co1—Co2—C5124.30 (15)C3—Co1—C8—Co2170.85 (18)
C3—Co1—Co2—C817.1 (3)C1—Co1—C8—Co285.0 (2)
C1—Co1—Co2—C8104.1 (2)C7—Co1—C8—Co273.5 (2)
C7—Co1—Co2—C851.5 (2)P1—Co1—C8—Co256.0 (2)
P1—Co1—Co2—C8143.91 (16)C3—Co1—C8—Sn251.4 (3)
C3—Co1—Co2—C734.4 (3)C1—Co1—C8—Sn252.7 (3)
C1—Co1—Co2—C7155.6 (2)C7—Co1—C8—Sn2148.7 (4)
C8—Co1—Co2—C751.5 (2)P1—Co1—C8—Sn2166.25 (15)
P1—Co1—Co2—C792.44 (15)Co2—Co1—C8—Sn2137.7 (3)
C3—Co1—Co2—P2138.3 (3)C6—Co2—C8—C782.9 (3)
C1—Co1—Co2—P2100.43 (17)C5—Co2—C8—C7171.4 (3)
C8—Co1—Co2—P2155.45 (16)P2—Co2—C8—C736.2 (3)
C7—Co1—Co2—P2103.98 (15)Co1—Co2—C8—C773.8 (2)
P1—Co1—Co2—P211.54 (5)C6—Co2—C8—Co1156.72 (17)
C3—Co1—P1—C2122.8 (2)C5—Co2—C8—Co197.60 (18)
C1—Co1—P1—C21130.0 (2)C7—Co2—C8—Co173.8 (2)
C8—Co1—P1—C2190.7 (2)P2—Co2—C8—Co137.6 (2)
C7—Co1—P1—C2179.6 (2)C6—Co2—C8—Sn266.7 (3)
Co2—Co1—P1—C21131.26 (17)C5—Co2—C8—Sn239.0 (3)
C3—Co1—P1—C3199.6 (2)C7—Co2—C8—Sn2149.6 (4)
C1—Co1—P1—C317.6 (3)P2—Co2—C8—Sn2174.19 (14)
C8—Co1—P1—C31146.8 (2)Co1—Co2—C8—Sn2136.6 (3)
C7—Co1—P1—C31157.9 (2)C12—Sn2—C8—C7162.7 (6)
Co2—Co1—P1—C31106.29 (16)C13—Sn2—C8—C777.1 (6)
C3—Co1—P1—C2139.8 (2)C14—Sn2—C8—C741.6 (6)
C1—Co1—P1—C2113.1 (2)C12—Sn2—C8—Co142.2 (3)
C8—Co1—P1—C226.2 (2)C13—Sn2—C8—Co1162.4 (3)
C7—Co1—P1—C237.31 (18)C14—Sn2—C8—Co178.9 (3)
Co2—Co1—P1—C214.32 (14)C12—Sn2—C8—Co274.2 (3)
C6—Co2—P2—C41125.5 (2)C13—Sn2—C8—Co246.0 (4)
C5—Co2—P2—C4119.3 (2)C14—Sn2—C8—Co2164.6 (3)
C8—Co2—P2—C41112.1 (2)C31—P1—C21—C26115.8 (4)
C7—Co2—P2—C41134.7 (2)C2—P1—C21—C2610.1 (4)
Co1—Co2—P2—C4183.92 (16)Co1—P1—C21—C26109.4 (4)
C6—Co2—P2—C2113.7 (2)C31—P1—C21—C2267.0 (4)
C5—Co2—P2—C2140.1 (2)C2—P1—C21—C22172.8 (4)
C8—Co2—P2—C28.7 (2)Co1—P1—C21—C2267.7 (4)
C7—Co2—P2—C213.87 (18)C26—C21—C22—C231.2 (7)
Co1—Co2—P2—C236.86 (14)P1—C21—C22—C23178.5 (4)
C6—Co2—P2—C512.6 (2)C21—C22—C23—C240.7 (9)
C5—Co2—P2—C51103.5 (2)C22—C23—C24—C250.6 (9)
C8—Co2—P2—C51125.1 (2)C23—C24—C25—C261.4 (9)
C7—Co2—P2—C51102.5 (2)C22—C21—C26—C250.3 (7)
Co1—Co2—P2—C51153.24 (16)P1—C21—C26—C25177.4 (4)
C41—P2—C2—P178.1 (2)C24—C25—C26—C211.0 (8)
C51—P2—C2—P1176.58 (19)C21—P1—C31—C36135.4 (4)
Co2—P2—C2—P152.7 (2)C2—P1—C31—C36117.2 (4)
C21—P1—C2—P2164.34 (19)Co1—P1—C31—C366.4 (5)
C31—P1—C2—P292.0 (2)C21—P1—C31—C3246.3 (4)
Co1—P1—C2—P241.1 (2)C2—P1—C31—C3261.2 (4)
C3—Co1—C7—C889.4 (3)Co1—P1—C31—C32175.3 (3)
C1—Co1—C7—C833.2 (4)C36—C31—C32—C330.3 (7)
P1—Co1—C7—C8167.7 (2)P1—C31—C32—C33178.1 (4)
Co2—Co1—C7—C872.7 (2)C31—C32—C33—C340.6 (8)
C3—Co1—C7—Co2162.10 (16)C32—C33—C34—C350.1 (9)
C1—Co1—C7—Co239.5 (4)C33—C34—C35—C361.4 (9)
C8—Co1—C7—Co272.7 (2)C32—C31—C36—C351.7 (7)
P1—Co1—C7—Co294.98 (9)P1—C31—C36—C35176.6 (4)
C3—Co1—C7—Sn139.8 (4)C34—C35—C36—C312.3 (9)
C1—Co1—C7—Sn1162.4 (3)C2—P2—C41—C46120.9 (4)
C8—Co1—C7—Sn1129.2 (5)C51—P2—C41—C46132.1 (4)
P1—Co1—C7—Sn163.1 (3)Co2—P2—C41—C462.7 (4)
Co2—Co1—C7—Sn1158.1 (4)C2—P2—C41—C4257.3 (4)
C6—Co2—C7—C8105.8 (3)C51—P2—C41—C4249.7 (4)
C5—Co2—C7—C812.6 (4)Co2—P2—C41—C42179.1 (3)
P2—Co2—C7—C8155.7 (2)C46—C41—C42—C430.2 (7)
Co1—Co2—C7—C872.4 (2)P2—C41—C42—C43178.4 (4)
C6—Co2—C7—Co1178.13 (16)C41—C42—C43—C440.8 (8)
C5—Co2—C7—Co159.8 (3)C42—C43—C44—C451.4 (9)
C8—Co2—C7—Co172.4 (2)C43—C44—C45—C461.4 (9)
P2—Co2—C7—Co183.37 (10)C42—C41—C46—C450.2 (7)
C6—Co2—C7—Sn122.5 (3)P2—C41—C46—C45178.4 (4)
C5—Co2—C7—Sn1140.9 (3)C44—C45—C46—C410.8 (8)
C8—Co2—C7—Sn1128.3 (4)C41—P2—C51—C56121.2 (4)
P2—Co2—C7—Sn176.0 (3)C2—P2—C51—C5614.0 (4)
Co1—Co2—C7—Sn1159.4 (4)Co2—P2—C51—C56105.9 (4)
C9—Sn1—C7—C833.3 (5)C41—P2—C51—C5263.4 (4)
C10—Sn1—C7—C887.1 (4)C2—P2—C51—C52170.6 (4)
C11—Sn1—C7—C8149.8 (4)Co2—P2—C51—C5269.5 (4)
C9—Sn1—C7—Co1141.1 (3)C56—C51—C52—C531.5 (7)
C10—Sn1—C7—Co120.7 (4)P2—C51—C52—C53174.2 (4)
C11—Sn1—C7—Co1102.4 (4)C51—C52—C53—C541.1 (9)
C9—Sn1—C7—Co271.7 (3)C52—C53—C54—C553.8 (9)
C10—Sn1—C7—Co2167.9 (3)C53—C54—C55—C563.6 (9)
C11—Sn1—C7—Co244.8 (3)C52—C51—C56—C551.7 (7)
Co2—C7—C8—Co184.09 (12)P2—C51—C56—C55173.6 (4)
Sn1—C7—C8—Co1139.7 (3)C54—C55—C56—C510.8 (8)

Experimental details

Crystal data
Chemical formulaC37H40Co2O4P2Sn2
Mr965.87
Crystal system, space groupMonoclinic, P21/n
Temperature (K)291
a, b, c (Å)16.012 (3), 13.761 (2), 18.126 (4)
β (°) 98.49 (2)
V3)3950.1 (13)
Z4
Radiation typeAg Kα, λ = 0.56083 Å
µ (mm1)1.15
Crystal size (mm)0.35 × 0.35 × 0.10
Data collection
DiffractometerCAD-4 Software (Nonius, 1989)
diffractometer
Absorption correctionψ scan
(WinGX; Farrugia, 1999; North et al., 1968)
Tmin, Tmax0.819, 1.000
No. of measured, independent and
observed [I > 2σ(I)] reflections
8838, 8572, 5353
Rint0.053
(sin θ/λ)max1)0.639
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.036, 0.105, 0.99
No. of reflections8572
No. of parameters430
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.10, 0.56

Computer programs: CAD-4 Software (Nonius, 1989), CAD-4 Software, XCAD4 (Harms, 1996), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), SHELXTL-Plus (Sheldrick, 1991), SHELXL97, PARST95 (Nardelli, 1995).

 

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