metal-organic compounds
In centrosymmetric octamethyl-1κ2C,2κ2C,3κ2C,4κ2C-tetrakis-μ-dichloroacetato-1:2κ2O,O′;2:3κ2O,O′;3:4κ2O,O′;1:4-κ2O-bis-μ3-oxo-1:2:3:κ3O;1:3:4κ3O-tetratin(IV), [[(CH3)2SnO2CCHCl2]2O]2, two Sn atoms are six-coordinate in a C2SnO4 skew-trapezoidal bipyramidal geometry [C—Sn—C 145.7 (4)°]. The other two Sn atoms are five-coordinate [C—Sn—C 154.3 (4)°], but the geometry is better regarded as a trans-C2SnO4 octahedron owing to a long intermolecular Sn—O bond [Sn—O 2.846 (6) Å], which links the molecules into a linear chain.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803019421/bt6341sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803019421/bt6341Isup2.hkl |
CCDC reference: 225661
Computing details top
Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Bis[1,1,3,3-tetramethyl-1,3-bis(dichloroacetato)distannoxane] top
Crystal data top
[Sn4(C2HO2Cl2)4(CH3)8O2] | Z = 1 |
Mr = 1138.74 | F(000) = 540 |
Triclinic, P1 | Dx = 2.164 Mg m−3 |
a = 8.9026 (5) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 9.6131 (6) Å | Cell parameters from 3478 reflections |
c = 11.2145 (7) Å | θ = 2.5–28.3° |
α = 91.674 (1)° | µ = 3.48 mm−1 |
β = 113.129 (1)° | T = 298 K |
γ = 96.651 (1)° | Parallelepiped, colorless |
V = 873.73 (9) Å3 | 0.29 × 0.18 × 0.12 mm |
Data collection top
Bruker APEX area-detector diffractometer | 3977 independent reflections |
Radiation source: fine-focus sealed tube | 3218 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.037 |
φ and ω scan | θmax = 28.3°, θmin = 2.0° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −11→11 |
Tmin = 0.540, Tmax = 0.659 | k = −12→12 |
7696 measured reflections | l = −14→14 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.059 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.129 | H-atom parameters constrained |
S = 1.08 | w = 1/[σ2(Fo2) + (0.0466P)2] where P = (Fo2 + 2Fc2)/3 |
3977 reflections | (Δ/σ)max = 0.001 |
176 parameters | Δρmax = 0.98 e Å−3 |
0 restraints | Δρmin = −1.07 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Sn1 | 0.53413 (6) | 0.65625 (5) | 0.45625 (5) | 0.0347 (2) | |
Sn2 | 0.81844 (6) | 0.56161 (5) | 0.78598 (5) | 0.0359 (2) | |
Cl1 | 1.0390 (4) | 1.0824 (3) | 0.8366 (3) | 0.094 (1) | |
Cl2 | 1.1522 (4) | 0.9440 (4) | 0.6663 (4) | 0.107 (1) | |
Cl3 | 0.5971 (4) | 0.0404 (3) | 0.7906 (3) | 0.087 (1) | |
Cl4 | 0.5547 (5) | 0.2089 (4) | 0.9883 (4) | 0.103 (1) | |
O1 | 0.6257 (6) | 0.5365 (5) | 0.6092 (4) | 0.034 (1) | |
O2 | 0.7362 (8) | 0.8427 (6) | 0.5732 (6) | 0.067 (2) | |
O3 | 0.9055 (8) | 0.7784 (7) | 0.7596 (6) | 0.073 (2) | |
O4 | 0.9013 (7) | 0.3557 (6) | 0.9778 (6) | 0.060 (2) | |
O5 | 0.6993 (6) | 0.3439 (5) | 0.7862 (5) | 0.041 (1) | |
C1 | 0.376 (1) | 0.7754 (9) | 0.4970 (9) | 0.058 (2) | |
C2 | 0.678 (1) | 0.639 (1) | 0.3506 (9) | 0.058 (3) | |
C3 | 0.860 (1) | 0.8568 (9) | 0.6675 (8) | 0.049 (2) | |
C4 | 0.981 (1) | 0.9918 (9) | 0.6864 (9) | 0.055 (2) | |
C5 | 1.008 (1) | 0.498 (1) | 0.7458 (9) | 0.057 (2) | |
C6 | 0.715 (1) | 0.643 (1) | 0.9072 (9) | 0.059 (3) | |
C7 | 0.774 (1) | 0.2991 (7) | 0.8942 (8) | 0.041 (1) | |
C8 | 0.695 (1) | 0.1606 (9) | 0.9242 (8) | 0.056 (2) | |
H1a | 0.3983 | 0.7767 | 0.5882 | 0.086* | |
H1b | 0.2635 | 0.7346 | 0.4474 | 0.086* | |
H1c | 0.3925 | 0.8698 | 0.4743 | 0.086* | |
H2a | 0.7927 | 0.6579 | 0.4081 | 0.088* | |
H2b | 0.6539 | 0.7058 | 0.2857 | 0.088* | |
H2c | 0.6546 | 0.5458 | 0.3090 | 0.088* | |
H4 | 0.9282 | 1.0533 | 0.6185 | 0.066* | |
H5a | 0.9744 | 0.4842 | 0.6533 | 0.085* | |
H5b | 1.0353 | 0.4113 | 0.7840 | 0.085* | |
H5c | 1.1031 | 0.5686 | 0.7813 | 0.085* | |
H6a | 0.7268 | 0.7439 | 0.9078 | 0.089* | |
H6b | 0.7707 | 0.6171 | 0.9940 | 0.089* | |
H6c | 0.6001 | 0.6064 | 0.8753 | 0.089* | |
H8 | 0.7808 | 0.1179 | 0.9914 | 0.068* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Sn1 | 0.0364 (3) | 0.0281 (3) | 0.0320 (3) | 0.0019 (2) | 0.0063 (2) | 0.0030 (2) |
Sn2 | 0.0341 (3) | 0.0338 (3) | 0.0308 (3) | 0.0010 (2) | 0.0045 (2) | 0.0012 (2) |
Cl1 | 0.099 (2) | 0.059 (2) | 0.095 (2) | −0.006 (2) | 0.013 (2) | −0.028 (2) |
Cl2 | 0.072 (2) | 0.132 (3) | 0.129 (3) | 0.002 (2) | 0.055 (2) | 0.021 (3) |
Cl3 | 0.093 (2) | 0.048 (2) | 0.107 (2) | −0.020 (1) | 0.037 (2) | −0.008 (2) |
Cl4 | 0.129 (3) | 0.101 (2) | 0.120 (3) | 0.009 (2) | 0.094 (3) | 0.021 (2) |
O1 | 0.036 (3) | 0.028 (3) | 0.024 (3) | −0.004 (2) | −0.002 (2) | 0.003 (2) |
O2 | 0.056 (4) | 0.047 (4) | 0.061 (4) | −0.011 (3) | −0.013 (3) | 0.013 (3) |
O3 | 0.075 (5) | 0.054 (4) | 0.055 (4) | −0.016 (3) | −0.004 (4) | 0.026 (3) |
O4 | 0.056 (4) | 0.053 (4) | 0.049 (4) | −0.004 (3) | 0.000 (3) | 0.000 (3) |
O5 | 0.041 (3) | 0.037 (3) | 0.031 (3) | 0.001 (2) | 0.000 (2) | 0.011 (2) |
C1 | 0.063 (6) | 0.051 (5) | 0.057 (6) | 0.024 (5) | 0.017 (5) | −0.009 (4) |
C2 | 0.050 (5) | 0.077 (7) | 0.057 (6) | 0.014 (5) | 0.029 (5) | 0.024 (5) |
C3 | 0.047 (5) | 0.045 (5) | 0.040 (5) | −0.013 (4) | 0.007 (4) | −0.015 (4) |
C4 | 0.047 (5) | 0.043 (5) | 0.055 (6) | −0.008 (4) | 0.002 (4) | −0.002 (4) |
C5 | 0.040 (5) | 0.071 (7) | 0.056 (6) | 0.009 (5) | 0.015 (4) | 0.007 (5) |
C6 | 0.068 (6) | 0.060 (6) | 0.047 (5) | 0.021 (5) | 0.017 (5) | −0.010 (4) |
C7 | 0.047 (5) | 0.018 (4) | 0.047 (5) | −0.003 (3) | 0.010 (4) | −0.011 (3) |
C8 | 0.062 (6) | 0.050 (6) | 0.047 (5) | 0.003 (5) | 0.011 (5) | 0.014 (4) |
Geometric parameters (Å, º) top
Sn1—C1 | 2.088 (8) | O4—C7 | 1.206 (9) |
Sn1—C2 | 2.076 (8) | O5—C7 | 1.249 (9) |
Sn1—O1 | 2.041 (4) | C3—C4 | 1.54 (1) |
Sn1—O1i | 2.118 (5) | C7—C8 | 1.54 (1) |
Sn1—O2 | 2.330 (6) | C1—H1a | 0.96 |
Sn1—O5i | 2.696 (5) | C1—H1b | 0.96 |
Sn2—C5 | 2.062 (8) | C1—H1c | 0.96 |
Sn2—C6 | 2.099 (8) | C2—H2a | 0.96 |
Sn2—O1 | 2.034 (4) | C2—H2b | 0.96 |
Sn2—O3 | 2.207 (6) | C2—H2c | 0.96 |
Sn2—O4ii | 2.846 (6) | C4—H4 | 0.98 |
Sn2—O5 | 2.234 (5) | C5—H5a | 0.96 |
Cl1—C4 | 1.730 (9) | C5—H5b | 0.96 |
Cl2—C4 | 1.733 (9) | C5—H5c | 0.96 |
Cl3—C8 | 1.726 (9) | C6—H6a | 0.96 |
Cl4—C8 | 1.76 (1) | C6—H6b | 0.96 |
O2—C3 | 1.180 (9) | C6—H6c | 0.96 |
O3—C3 | 1.26 (1) | C8—H8 | 0.98 |
C1—Sn1—C2 | 145.7 (4) | O3—C3—C4 | 114.2 (7) |
C1—Sn1—O1 | 106.6 (3) | C3—C4—Cl1 | 112.7 (7) |
C1—Sn1—O1i | 98.7 (3) | C3—C4—Cl2 | 107.7 (6) |
C1—Sn1—O2 | 84.0 (3) | Cl1—C4—Cl2 | 110.6 (5) |
C1—Sn1—O5i | 80.6 (3) | O4—C7—O5 | 125.7 (8) |
C2—Sn1—O1 | 105.4 (3) | O4—C7—C8 | 117.1 (8) |
C2—Sn1—O1i | 100.0 (3) | O5—C7—C8 | 117.2 (7) |
C2—Sn1—O2 | 84.4 (3) | C7—C8—Cl3 | 113.7 (6) |
C2—Sn1—O5i | 80.7 (3) | C7—C8—Cl4 | 105.7 (6) |
O1—Sn1—O1i | 77.2 (2) | Cl3—C8—Cl4 | 111.1 (5) |
O1—Sn1—O2 | 89.4 (2) | Sn1—C1—H1a | 109.5 |
O1—Sn1—O5i | 144.0 (2) | Sn1—C1—H1b | 109.5 |
O1i—Sn1—O2 | 166.6 (2) | H1a—C1—H1b | 109.5 |
O1i—Sn1—O5i | 66.9 (2) | Sn1—C1—H1c | 109.5 |
O2—Sn1—O5i | 126.6 (2) | H1a—C1—H1c | 109.5 |
C5—Sn2—C6 | 154.3 (4) | H1b—C1—H1c | 109.5 |
C5—Sn2—O1 | 103.2 (3) | Sn1—C2—H2a | 109.5 |
C5—Sn2—O3 | 87.9 (3) | Sn1—C2—H2b | 109.5 |
C5—Sn2—O4ii | 77.2 (3) | H2a—C2—H2b | 109.5 |
C5—Sn2—O5 | 94.9 (3) | Sn1—C2—H2c | 109.5 |
C6—Sn2—O1 | 102.5 (3) | H2a—C2—H2c | 109.5 |
C6—Sn2—O3 | 89.0 (3) | H2b—C2—H2c | 109.5 |
C6—Sn2—O4ii | 77.2 (3) | C3—C4—H4 | 108.6 |
C6—Sn2—O5 | 91.7 (3) | Cl1—C4—H4 | 108.6 |
O1—Sn2—O3 | 93.7 (2) | Cl2—C4—H4 | 108.6 |
O1—Sn2—O4ii | 170.2 (2) | Sn2—C5—H5a | 109.5 |
O1—Sn2—O5 | 78.2 (2) | Sn2—C5—H5b | 109.5 |
O3—Sn2—O4ii | 76.5 (2) | H5a—C5—H5b | 109.5 |
O3—Sn2—O5 | 171.8 (2) | Sn2—C5—H5c | 109.5 |
O4ii—Sn2—O5 | 111.6 (2) | H5a—C5—H5c | 109.5 |
Sn1—O1—Sn1i | 102.8 (2) | H5b—C5—H5c | 109.5 |
Sn1—O1—Sn2 | 136.1 (2) | Sn2—C6—H6a | 109.5 |
Sn1i—O1—Sn2 | 121.0 (2) | Sn2—C6—H6b | 109.5 |
Sn1i—O5—Sn2 | 93.8 (2) | H6a—C6—H6b | 109.5 |
C3—O2—Sn1 | 136.1 (6) | Sn2—C6—H6c | 109.5 |
C3—O3—Sn2 | 133.9 (6) | H6a—C6—H6c | 109.5 |
C7—O5—Sn2 | 108.5 (4) | H6b—C6—H6c | 109.5 |
C7—O5—Sn1i | 157.6 (5) | C7—C8—H8 | 108.7 |
O2—C3—O3 | 128.7 (8) | Cl3—C8—H8 | 108.7 |
O2—C3—C4 | 117.0 (8) | Cl4—C8—H8 | 108.7 |
C5—Sn2—O1—Sn1 | −88.4 (4) | C6—Sn2—O3—C3 | −106 (1) |
C6—Sn2—O1—Sn1 | 90.1 (4) | O4ii—Sn2—O3—C3 | 177 (1) |
O3—Sn2—O1—Sn1 | 0.3 (4) | O1—Sn2—O5—C7 | −176.2 (6) |
O5—Sn2—O1—Sn1 | 179.3 (4) | C5—Sn2—O5—C7 | 81.3 (6) |
C5—Sn2—O1—Sn1i | 89.5 (4) | C6—Sn2—O5—C7 | −73.8 (6) |
C6—Sn2—O1—Sn1i | −92.0 (4) | O4ii—Sn2—O5—C7 | 3.1 (6) |
O3—Sn2—O1—Sn1i | 178.1 (3) | O1—Sn2—O5—Sn1i | 1.9 (2) |
O5—Sn2—O1—Sn1i | −2.9 (3) | C5—Sn2—O5—Sn1i | −100.6 (3) |
O4ii—Sn2—O1—Sn1i | −179 (1) | C6—Sn2—O5—Sn1i | 104.3 (3) |
C2—Sn1—O1—Sn2 | 81.1 (5) | O4ii—Sn2—O5—Sn1i | −178.8 (2) |
C1—Sn1—O1—Sn2 | −86.5 (4) | Sn1—O2—C3—O3 | −21 (2) |
O1i—Sn1—O1—Sn2 | 178.1 (5) | Sn1—O2—C3—C4 | 161.8 (6) |
O2—Sn1—O1—Sn2 | −2.9 (4) | Sn2—O3—C3—O2 | 14 (2) |
O5i—Sn1—O1—Sn2 | 176.5 (2) | Sn2—O3—C3—C4 | −169.0 (6) |
C2—Sn1—O1—Sn1i | −97.0 (3) | O2—C3—C4—Cl1 | 127.2 (8) |
C1—Sn1—O1—Sn1i | 95.4 (3) | O3—C3—C4—Cl1 | −50 (1) |
O1i—Sn1—O1—Sn1i | 0.0 | O2—C3—C4—Cl2 | −110.5 (9) |
O2—Sn1—O1—Sn1i | 178.9 (3) | O3—C3—C4—Cl2 | 72.1 (9) |
O5i—Sn1—O1—Sn1i | −1.6 (4) | Sn2—O5—C7—O4 | −9 (1) |
O1—Sn1—O2—C3 | 14 (1) | Sn1i—O5—C7—O4 | 175.8 (9) |
C2—Sn1—O2—C3 | −92 (1) | Sn2—O5—C7—C8 | 170.0 (6) |
C1—Sn1—O2—C3 | 121 (1) | Sn1i—O5—C7—C8 | −5 (2) |
O1i—Sn1—O2—C3 | 19 (2) | O4—C7—C8—Cl3 | −144.9 (7) |
O5i—Sn1—O2—C3 | −165.5 (9) | O5—C7—C8—Cl3 | 36 (1) |
O1—Sn2—O3—C3 | −3 (1) | O4—C7—C8—Cl4 | 93.0 (8) |
C5—Sn2—O3—C3 | 100 (1) | O5—C7—C8—Cl4 | −86.2 (8) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+2, −y+1, −z+2. |