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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803019421/bt6341sup1.cif
Contains datablocks I, mma20

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803019421/bt6341Isup2.hkl
Contains datablock I

CCDC reference: 225661

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.013 Å
  • R factor = 0.059
  • wR factor = 0.129
  • Data-to-parameter ratio = 22.6

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.91
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.540 0.659 Tmin and Tmax expected: 0.481 0.659 RR = 1.121 Please check that your absorption correction is appropriate. REFLT03_ALERT_3_C Reflection count < 95% complete From the CIF: _diffrn_reflns_theta_max 28.30 From the CIF: _diffrn_reflns_theta_full 0.00 From the CIF: _reflns_number_total 3977 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 4345 Completeness (_total/calc) 91.53% PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.13 PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT230_ALERT_2_C Hirshfeld Test Diff for O5 - C7 = 5.17 su PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... O2 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... O3 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Sn1 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Sn2 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C3 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C4 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C8 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 13 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 9 O4 -SN2 -O1 -SN1 -179.00 1.00 2.767 1.555 1.555 2.666
1 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 15 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 8 ALERT type 2 Indicator that the structure model may be wrong or deficient 5 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

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 = 1138.74F(000) = 540
Triclinic, P1Dx = 2.164 Mg m3
a = 8.9026 (5) ÅMo Kα radiation, λ = 0.71073 Å
b = 9.6131 (6) ÅCell parameters from 3478 reflections
c = 11.2145 (7) Åθ = 2.5–28.3°
α = 91.674 (1)°µ = 3.48 mm1
β = 113.129 (1)°T = 298 K
γ = 96.651 (1)°Parallelepiped, colorless
V = 873.73 (9) Å30.29 × 0.18 × 0.12 mm
Data collection top
Bruker APEX area-detector
diffractometer
3977 independent reflections
Radiation source: fine-focus sealed tube3218 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.037
φ and ω scanθmax = 28.3°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1111
Tmin = 0.540, Tmax = 0.659k = 1212
7696 measured reflectionsl = 1414
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)] = 0.059Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.129H-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 parametersΔρmax = 0.98 e Å3
0 restraintsΔρmin = 1.07 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sn10.53413 (6)0.65625 (5)0.45625 (5)0.0347 (2)
Sn20.81844 (6)0.56161 (5)0.78598 (5)0.0359 (2)
Cl11.0390 (4)1.0824 (3)0.8366 (3)0.094 (1)
Cl21.1522 (4)0.9440 (4)0.6663 (4)0.107 (1)
Cl30.5971 (4)0.0404 (3)0.7906 (3)0.087 (1)
Cl40.5547 (5)0.2089 (4)0.9883 (4)0.103 (1)
O10.6257 (6)0.5365 (5)0.6092 (4)0.034 (1)
O20.7362 (8)0.8427 (6)0.5732 (6)0.067 (2)
O30.9055 (8)0.7784 (7)0.7596 (6)0.073 (2)
O40.9013 (7)0.3557 (6)0.9778 (6)0.060 (2)
O50.6993 (6)0.3439 (5)0.7862 (5)0.041 (1)
C10.376 (1)0.7754 (9)0.4970 (9)0.058 (2)
C20.678 (1)0.639 (1)0.3506 (9)0.058 (3)
C30.860 (1)0.8568 (9)0.6675 (8)0.049 (2)
C40.981 (1)0.9918 (9)0.6864 (9)0.055 (2)
C51.008 (1)0.498 (1)0.7458 (9)0.057 (2)
C60.715 (1)0.643 (1)0.9072 (9)0.059 (3)
C70.774 (1)0.2991 (7)0.8942 (8)0.041 (1)
C80.695 (1)0.1606 (9)0.9242 (8)0.056 (2)
H1a0.39830.77670.58820.086*
H1b0.26350.73460.44740.086*
H1c0.39250.86980.47430.086*
H2a0.79270.65790.40810.088*
H2b0.65390.70580.28570.088*
H2c0.65460.54580.30900.088*
H40.92821.05330.61850.066*
H5a0.97440.48420.65330.085*
H5b1.03530.41130.78400.085*
H5c1.10310.56860.78130.085*
H6a0.72680.74390.90780.089*
H6b0.77070.61710.99400.089*
H6c0.60010.60640.87530.089*
H80.78080.11790.99140.068*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn10.0364 (3)0.0281 (3)0.0320 (3)0.0019 (2)0.0063 (2)0.0030 (2)
Sn20.0341 (3)0.0338 (3)0.0308 (3)0.0010 (2)0.0045 (2)0.0012 (2)
Cl10.099 (2)0.059 (2)0.095 (2)0.006 (2)0.013 (2)0.028 (2)
Cl20.072 (2)0.132 (3)0.129 (3)0.002 (2)0.055 (2)0.021 (3)
Cl30.093 (2)0.048 (2)0.107 (2)0.020 (1)0.037 (2)0.008 (2)
Cl40.129 (3)0.101 (2)0.120 (3)0.009 (2)0.094 (3)0.021 (2)
O10.036 (3)0.028 (3)0.024 (3)0.004 (2)0.002 (2)0.003 (2)
O20.056 (4)0.047 (4)0.061 (4)0.011 (3)0.013 (3)0.013 (3)
O30.075 (5)0.054 (4)0.055 (4)0.016 (3)0.004 (4)0.026 (3)
O40.056 (4)0.053 (4)0.049 (4)0.004 (3)0.000 (3)0.000 (3)
O50.041 (3)0.037 (3)0.031 (3)0.001 (2)0.000 (2)0.011 (2)
C10.063 (6)0.051 (5)0.057 (6)0.024 (5)0.017 (5)0.009 (4)
C20.050 (5)0.077 (7)0.057 (6)0.014 (5)0.029 (5)0.024 (5)
C30.047 (5)0.045 (5)0.040 (5)0.013 (4)0.007 (4)0.015 (4)
C40.047 (5)0.043 (5)0.055 (6)0.008 (4)0.002 (4)0.002 (4)
C50.040 (5)0.071 (7)0.056 (6)0.009 (5)0.015 (4)0.007 (5)
C60.068 (6)0.060 (6)0.047 (5)0.021 (5)0.017 (5)0.010 (4)
C70.047 (5)0.018 (4)0.047 (5)0.003 (3)0.010 (4)0.011 (3)
C80.062 (6)0.050 (6)0.047 (5)0.003 (5)0.011 (5)0.014 (4)
Geometric parameters (Å, º) top
Sn1—C12.088 (8)O4—C71.206 (9)
Sn1—C22.076 (8)O5—C71.249 (9)
Sn1—O12.041 (4)C3—C41.54 (1)
Sn1—O1i2.118 (5)C7—C81.54 (1)
Sn1—O22.330 (6)C1—H1a0.96
Sn1—O5i2.696 (5)C1—H1b0.96
Sn2—C52.062 (8)C1—H1c0.96
Sn2—C62.099 (8)C2—H2a0.96
Sn2—O12.034 (4)C2—H2b0.96
Sn2—O32.207 (6)C2—H2c0.96
Sn2—O4ii2.846 (6)C4—H40.98
Sn2—O52.234 (5)C5—H5a0.96
Cl1—C41.730 (9)C5—H5b0.96
Cl2—C41.733 (9)C5—H5c0.96
Cl3—C81.726 (9)C6—H6a0.96
Cl4—C81.76 (1)C6—H6b0.96
O2—C31.180 (9)C6—H6c0.96
O3—C31.26 (1)C8—H80.98
C1—Sn1—C2145.7 (4)O3—C3—C4114.2 (7)
C1—Sn1—O1106.6 (3)C3—C4—Cl1112.7 (7)
C1—Sn1—O1i98.7 (3)C3—C4—Cl2107.7 (6)
C1—Sn1—O284.0 (3)Cl1—C4—Cl2110.6 (5)
C1—Sn1—O5i80.6 (3)O4—C7—O5125.7 (8)
C2—Sn1—O1105.4 (3)O4—C7—C8117.1 (8)
C2—Sn1—O1i100.0 (3)O5—C7—C8117.2 (7)
C2—Sn1—O284.4 (3)C7—C8—Cl3113.7 (6)
C2—Sn1—O5i80.7 (3)C7—C8—Cl4105.7 (6)
O1—Sn1—O1i77.2 (2)Cl3—C8—Cl4111.1 (5)
O1—Sn1—O289.4 (2)Sn1—C1—H1a109.5
O1—Sn1—O5i144.0 (2)Sn1—C1—H1b109.5
O1i—Sn1—O2166.6 (2)H1a—C1—H1b109.5
O1i—Sn1—O5i66.9 (2)Sn1—C1—H1c109.5
O2—Sn1—O5i126.6 (2)H1a—C1—H1c109.5
C5—Sn2—C6154.3 (4)H1b—C1—H1c109.5
C5—Sn2—O1103.2 (3)Sn1—C2—H2a109.5
C5—Sn2—O387.9 (3)Sn1—C2—H2b109.5
C5—Sn2—O4ii77.2 (3)H2a—C2—H2b109.5
C5—Sn2—O594.9 (3)Sn1—C2—H2c109.5
C6—Sn2—O1102.5 (3)H2a—C2—H2c109.5
C6—Sn2—O389.0 (3)H2b—C2—H2c109.5
C6—Sn2—O4ii77.2 (3)C3—C4—H4108.6
C6—Sn2—O591.7 (3)Cl1—C4—H4108.6
O1—Sn2—O393.7 (2)Cl2—C4—H4108.6
O1—Sn2—O4ii170.2 (2)Sn2—C5—H5a109.5
O1—Sn2—O578.2 (2)Sn2—C5—H5b109.5
O3—Sn2—O4ii76.5 (2)H5a—C5—H5b109.5
O3—Sn2—O5171.8 (2)Sn2—C5—H5c109.5
O4ii—Sn2—O5111.6 (2)H5a—C5—H5c109.5
Sn1—O1—Sn1i102.8 (2)H5b—C5—H5c109.5
Sn1—O1—Sn2136.1 (2)Sn2—C6—H6a109.5
Sn1i—O1—Sn2121.0 (2)Sn2—C6—H6b109.5
Sn1i—O5—Sn293.8 (2)H6a—C6—H6b109.5
C3—O2—Sn1136.1 (6)Sn2—C6—H6c109.5
C3—O3—Sn2133.9 (6)H6a—C6—H6c109.5
C7—O5—Sn2108.5 (4)H6b—C6—H6c109.5
C7—O5—Sn1i157.6 (5)C7—C8—H8108.7
O2—C3—O3128.7 (8)Cl3—C8—H8108.7
O2—C3—C4117.0 (8)Cl4—C8—H8108.7
C5—Sn2—O1—Sn188.4 (4)C6—Sn2—O3—C3106 (1)
C6—Sn2—O1—Sn190.1 (4)O4ii—Sn2—O3—C3177 (1)
O3—Sn2—O1—Sn10.3 (4)O1—Sn2—O5—C7176.2 (6)
O5—Sn2—O1—Sn1179.3 (4)C5—Sn2—O5—C781.3 (6)
C5—Sn2—O1—Sn1i89.5 (4)C6—Sn2—O5—C773.8 (6)
C6—Sn2—O1—Sn1i92.0 (4)O4ii—Sn2—O5—C73.1 (6)
O3—Sn2—O1—Sn1i178.1 (3)O1—Sn2—O5—Sn1i1.9 (2)
O5—Sn2—O1—Sn1i2.9 (3)C5—Sn2—O5—Sn1i100.6 (3)
O4ii—Sn2—O1—Sn1i179 (1)C6—Sn2—O5—Sn1i104.3 (3)
C2—Sn1—O1—Sn281.1 (5)O4ii—Sn2—O5—Sn1i178.8 (2)
C1—Sn1—O1—Sn286.5 (4)Sn1—O2—C3—O321 (2)
O1i—Sn1—O1—Sn2178.1 (5)Sn1—O2—C3—C4161.8 (6)
O2—Sn1—O1—Sn22.9 (4)Sn2—O3—C3—O214 (2)
O5i—Sn1—O1—Sn2176.5 (2)Sn2—O3—C3—C4169.0 (6)
C2—Sn1—O1—Sn1i97.0 (3)O2—C3—C4—Cl1127.2 (8)
C1—Sn1—O1—Sn1i95.4 (3)O3—C3—C4—Cl150 (1)
O1i—Sn1—O1—Sn1i0.0O2—C3—C4—Cl2110.5 (9)
O2—Sn1—O1—Sn1i178.9 (3)O3—C3—C4—Cl272.1 (9)
O5i—Sn1—O1—Sn1i1.6 (4)Sn2—O5—C7—O49 (1)
O1—Sn1—O2—C314 (1)Sn1i—O5—C7—O4175.8 (9)
C2—Sn1—O2—C392 (1)Sn2—O5—C7—C8170.0 (6)
C1—Sn1—O2—C3121 (1)Sn1i—O5—C7—C85 (2)
O1i—Sn1—O2—C319 (2)O4—C7—C8—Cl3144.9 (7)
O5i—Sn1—O2—C3165.5 (9)O5—C7—C8—Cl336 (1)
O1—Sn2—O3—C33 (1)O4—C7—C8—Cl493.0 (8)
C5—Sn2—O3—C3100 (1)O5—C7—C8—Cl486.2 (8)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+2, y+1, z+2.
 

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