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The molecular structure of the centrosymmetric hexanuclear title compound, [iPrSn(O)(O2CCH3)]6·4CHCl3 or [Sn6O6(C3H7)6(C2H3O2)6]·4CHCl3, adopts the `drum' motif, in which two (iPrSnO)3 caps are linked via six μ3-oxo atoms and six acetate groups. The Sn atoms are in distorted octahedral environments, defined by a CO5 donor set for each of the three independent Sn atoms.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802008978/wn6099sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802008978/wn6099Isup2.hkl
Contains datablock I

CCDC reference: 189305

Key indicators

  • Single-crystal X-ray study
  • T = 193 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.042
  • wR factor = 0.091
  • Data-to-parameter ratio = 28.7

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry








Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SHELXTL (Bruker, 2000); program(s) used to solve structure: PATTY in DIRDIF92 (Beurskens et al., 1992); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2000).

(I) top
Crystal data top
[Sn6O6(C3H7)6(C2H3O2)6]·4CHCl3F(000) = 1832
Mr = 1898.39Dx = 2.022 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ybcCell parameters from 25440 reflections
a = 13.2736 (14) Åθ = 1.5–30.1°
b = 13.5405 (16) ŵ = 2.94 mm1
c = 17.3572 (19) ÅT = 193 K
β = 92.007 (3)°Block, colourless
V = 3117.7 (6) Å30.20 × 0.10 × 0.05 mm
Z = 2
Data collection top
Bruker AXS SMART CCD
diffractometer
9084 independent reflections
Radiation source: fine-focus sealed tube6796 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.051
ω scansθmax = 30.1°, θmin = 1.5°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 1718
Tmin = 0.683, Tmax = 0.863k = 1519
25440 measured reflectionsl = 2420
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)] = 0.042Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.091H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.0368P)2]
where P = (Fo2 + 2Fc2)/3
9084 reflections(Δ/σ)max = 0.001
316 parametersΔρmax = 1.33 e Å3
0 restraintsΔρmin = 0.71 e Å3
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
Sn10.15982 (2)0.06291 (2)0.551298 (16)0.01713 (7)
Sn20.05108 (2)0.01965 (2)0.639897 (16)0.01706 (7)
Sn30.09790 (2)0.15655 (2)0.495538 (16)0.01682 (7)
Cl10.55261 (12)0.21831 (13)0.73749 (10)0.0601 (4)
Cl20.44219 (14)0.09192 (14)0.63131 (10)0.0616 (4)
Cl30.54342 (15)0.00896 (14)0.76583 (10)0.0652 (5)
Cl40.45731 (13)0.35390 (14)0.55989 (12)0.0687 (5)
Cl50.28630 (14)0.48248 (13)0.54934 (10)0.0602 (4)
Cl60.38157 (15)0.42224 (14)0.41133 (10)0.0673 (5)
O10.0184 (2)0.1262 (2)0.57069 (16)0.0183 (6)
O20.0759 (2)0.0563 (2)0.59474 (15)0.0180 (6)
O30.1467 (2)0.0252 (2)0.54708 (16)0.0191 (6)
O40.1925 (2)0.0999 (2)0.66962 (17)0.0253 (7)
O50.0450 (2)0.0671 (2)0.73157 (17)0.0235 (7)
O60.1410 (2)0.1383 (2)0.69017 (17)0.0257 (7)
O70.1771 (2)0.2330 (2)0.58902 (16)0.0249 (7)
O80.2487 (2)0.1756 (2)0.45239 (18)0.0241 (7)
O90.2959 (2)0.0207 (2)0.42572 (18)0.0235 (7)
C10.1356 (4)0.0937 (3)0.7296 (3)0.0241 (9)
C20.1815 (4)0.1204 (4)0.8043 (3)0.0361 (12)
H2A0.25210.13940.79480.054*
H2B0.14430.17580.82790.054*
H2C0.17810.06340.83910.054*
C30.1828 (3)0.2113 (4)0.6598 (3)0.0239 (9)
C40.2442 (4)0.2794 (4)0.7117 (3)0.0364 (12)
H4A0.27170.33310.68090.055*
H4B0.29960.24230.73670.055*
H4C0.20120.30700.75100.055*
C50.3115 (3)0.1124 (4)0.4301 (2)0.0241 (9)
C60.4113 (4)0.1502 (4)0.4049 (3)0.0389 (13)
H6A0.45280.09470.38860.058*
H6B0.44570.18460.44800.058*
H6C0.40050.19620.36180.058*
C70.2387 (3)0.1866 (3)0.5006 (3)0.0247 (9)
H70.19100.21930.46530.030*
C80.2667 (4)0.2636 (4)0.5601 (3)0.0428 (14)
H8A0.20650.28210.59110.064*
H8B0.31740.23610.59380.064*
H8C0.29420.32220.53370.064*
C90.3286 (4)0.1547 (5)0.4517 (3)0.0449 (14)
H9A0.30780.10500.41440.067*
H9B0.35710.21200.42420.067*
H9C0.37960.12630.48470.067*
C100.1208 (3)0.0964 (3)0.7072 (3)0.0252 (9)
H100.14120.14840.66990.030*
C110.0456 (4)0.1449 (4)0.7600 (3)0.0395 (13)
H11A0.01440.16540.72950.059*
H11B0.02600.09750.79950.059*
H11C0.07670.20280.78490.059*
C120.2162 (4)0.0639 (4)0.7504 (3)0.0400 (13)
H12A0.26210.03360.71430.060*
H12B0.24880.12130.77490.060*
H12C0.19920.01570.79000.060*
C130.0328 (3)0.2876 (3)0.4458 (3)0.0233 (9)
H130.02960.26650.41630.028*
C140.0014 (4)0.3583 (4)0.5089 (3)0.0390 (13)
H14A0.04440.32270.54430.059*
H14B0.03950.41310.48520.059*
H14C0.05780.38430.53750.059*
C150.0983 (4)0.3397 (4)0.3890 (3)0.0390 (13)
H15A0.11870.29280.34940.059*
H15B0.15850.36600.41610.059*
H15C0.06040.39400.36450.059*
C160.5475 (4)0.1013 (4)0.6944 (3)0.0390 (13)
H160.60960.09160.66440.047*
C170.3504 (4)0.3870 (4)0.5044 (3)0.0393 (12)
H170.30470.32830.50040.047*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn10.01496 (13)0.01916 (15)0.01732 (14)0.00026 (11)0.00110 (10)0.00110 (10)
Sn20.01705 (14)0.01957 (15)0.01451 (13)0.00099 (11)0.00036 (10)0.00010 (10)
Sn30.01678 (14)0.01707 (14)0.01664 (14)0.00179 (11)0.00096 (10)0.00014 (10)
Cl10.0550 (10)0.0567 (11)0.0685 (11)0.0016 (8)0.0039 (8)0.0209 (8)
Cl20.0696 (11)0.0547 (11)0.0596 (10)0.0042 (8)0.0134 (9)0.0054 (8)
Cl30.0835 (13)0.0673 (12)0.0456 (9)0.0087 (10)0.0125 (9)0.0129 (8)
Cl40.0573 (10)0.0604 (12)0.0866 (13)0.0059 (8)0.0240 (9)0.0128 (9)
Cl50.0739 (11)0.0438 (10)0.0636 (11)0.0094 (8)0.0143 (9)0.0074 (8)
Cl60.0941 (13)0.0589 (11)0.0503 (10)0.0209 (10)0.0238 (9)0.0023 (8)
O10.0163 (14)0.0199 (16)0.0186 (15)0.0003 (11)0.0019 (11)0.0013 (11)
O20.0186 (14)0.0203 (16)0.0150 (14)0.0007 (12)0.0005 (11)0.0007 (11)
O30.0183 (14)0.0206 (16)0.0185 (14)0.0003 (12)0.0012 (11)0.0004 (11)
O40.0239 (16)0.0331 (19)0.0193 (16)0.0017 (14)0.0059 (13)0.0021 (13)
O50.0226 (15)0.0293 (18)0.0185 (15)0.0012 (13)0.0001 (12)0.0011 (12)
O60.0283 (17)0.0304 (19)0.0184 (15)0.0073 (14)0.0009 (13)0.0021 (12)
O70.0299 (17)0.0263 (18)0.0183 (15)0.0078 (13)0.0009 (13)0.0025 (12)
O80.0189 (15)0.0251 (18)0.0287 (17)0.0047 (12)0.0038 (13)0.0028 (13)
O90.0176 (15)0.0271 (18)0.0261 (16)0.0012 (13)0.0043 (12)0.0026 (13)
C10.032 (2)0.020 (2)0.021 (2)0.0047 (18)0.0056 (19)0.0002 (16)
C20.030 (3)0.055 (4)0.024 (2)0.004 (2)0.007 (2)0.010 (2)
C30.018 (2)0.028 (3)0.025 (2)0.0005 (18)0.0006 (17)0.0047 (18)
C40.041 (3)0.039 (3)0.029 (3)0.016 (2)0.002 (2)0.004 (2)
C50.018 (2)0.035 (3)0.019 (2)0.0044 (19)0.0021 (17)0.0022 (18)
C60.023 (2)0.035 (3)0.060 (4)0.007 (2)0.013 (2)0.005 (3)
C70.020 (2)0.026 (2)0.029 (2)0.0011 (18)0.0021 (18)0.0039 (18)
C80.055 (4)0.032 (3)0.042 (3)0.018 (3)0.009 (3)0.004 (2)
C90.030 (3)0.049 (4)0.055 (4)0.005 (2)0.014 (3)0.013 (3)
C100.029 (2)0.025 (2)0.022 (2)0.0044 (19)0.0000 (18)0.0036 (17)
C110.045 (3)0.040 (3)0.034 (3)0.000 (2)0.007 (2)0.016 (2)
C120.030 (3)0.044 (3)0.045 (3)0.004 (2)0.015 (2)0.007 (3)
C130.022 (2)0.022 (2)0.026 (2)0.0017 (18)0.0021 (18)0.0025 (17)
C140.053 (3)0.022 (3)0.043 (3)0.005 (2)0.009 (3)0.001 (2)
C150.040 (3)0.041 (3)0.036 (3)0.004 (2)0.006 (2)0.020 (2)
C160.041 (3)0.040 (3)0.037 (3)0.002 (2)0.010 (2)0.002 (2)
C170.045 (3)0.031 (3)0.042 (3)0.007 (2)0.003 (3)0.001 (2)
Geometric parameters (Å, º) top
Sn1—O12.081 (3)C3—C41.507 (6)
Sn1—O22.087 (3)C4—H4A0.9800
Sn1—O3i2.096 (3)C4—H4B0.9800
Sn1—O42.172 (3)C4—H4C0.9800
Sn1—O9i2.180 (3)C5—C61.499 (6)
Sn1—C72.147 (5)C6—H6A0.9800
Sn2—O12.073 (3)C6—H6B0.9800
Sn2—O22.103 (3)C6—H6C0.9800
Sn2—O32.087 (3)C7—C81.523 (7)
Sn2—O52.171 (3)C7—C91.504 (7)
Sn2—O62.166 (3)C7—H71.0000
Sn2—C102.148 (4)C8—H8A0.9800
Sn3—O12.096 (3)C8—H8B0.9800
Sn3—O2i2.086 (3)C8—H8C0.9800
Sn3—O32.083 (3)C9—H9A0.9800
Sn3—O72.166 (3)C9—H9B0.9800
Sn3—O82.177 (3)C9—H9C0.9800
Sn3—C132.142 (4)C10—C121.514 (6)
Cl1—C161.752 (6)C10—C111.527 (6)
Cl2—C161.750 (6)C10—H101.0000
Cl3—C161.762 (6)C11—H11A0.9800
Cl4—C171.745 (6)C11—H11B0.9800
Cl5—C171.747 (6)C11—H11C0.9800
Cl6—C171.748 (6)C12—H12A0.9800
O2—Sn3i2.086 (3)C12—H12B0.9800
O3—Sn1i2.096 (3)C12—H12C0.9800
O4—C11.267 (5)C13—C151.513 (6)
O5—C11.255 (5)C13—C141.535 (7)
O6—C31.259 (5)C13—H131.0000
O7—C31.263 (5)C14—H14A0.9800
O8—C51.265 (5)C14—H14B0.9800
O9—C51.261 (6)C14—H14C0.9800
O9—Sn1i2.180 (3)C15—H15A0.9800
C1—C21.496 (6)C15—H15B0.9800
C2—H2A0.9800C15—H15C0.9800
C2—H2B0.9800C16—H161.0000
C2—H2C0.9800C17—H171.0000
O1—Sn1—O278.08 (11)H4B—C4—H4C109.5
O1—Sn1—O3i105.45 (11)O8—C5—O9125.2 (4)
O1—Sn1—O487.76 (11)O8—C5—C6117.1 (4)
O1—Sn1—O9i158.91 (11)O9—C5—C6117.7 (4)
O1—Sn1—C799.73 (14)C5—C6—H6A109.5
O2—Sn1—O3i78.19 (11)C5—C6—H6B109.5
O2—Sn1—O487.63 (11)H6A—C6—H6B109.5
O2—Sn1—C7176.09 (14)C5—C6—H6C109.5
O2—Sn1—O9i88.13 (11)H6A—C6—H6C109.5
O3i—Sn1—O4157.93 (12)H6B—C6—H6C109.5
O3i—Sn1—O9i86.93 (11)C8—C7—C9111.8 (4)
O3i—Sn1—C799.41 (15)C8—C7—Sn1112.5 (3)
O4—Sn1—O9i75.68 (12)C9—C7—Sn1111.9 (3)
O4—Sn1—C795.55 (15)C8—C7—H7106.7
O9i—Sn1—C794.85 (15)C9—C7—H7106.7
O1—Sn2—O277.87 (11)Sn1—C7—H7106.7
O1—Sn2—O378.33 (11)C7—C8—H8A109.5
O1—Sn2—O587.59 (11)C7—C8—H8B109.5
O1—Sn2—O686.84 (12)H8A—C8—H8B109.5
O1—Sn2—C10177.03 (15)C7—C8—H8C109.5
O2—Sn2—O3103.38 (11)H8A—C8—H8C109.5
O2—Sn2—O586.21 (11)H8B—C8—H8C109.5
O2—Sn2—O6159.38 (12)C7—C9—H9A109.5
O2—Sn2—C1099.76 (15)C7—C9—H9B109.5
O3—Sn2—O5160.70 (12)H9A—C9—H9B109.5
O3—Sn2—O686.71 (11)C7—C9—H9C109.5
O3—Sn2—C10100.62 (14)H9A—C9—H9C109.5
O5—Sn2—O679.33 (12)H9B—C9—H9C109.5
O5—Sn2—C1094.06 (15)C12—C10—C11112.4 (4)
O6—Sn2—C1095.89 (15)C12—C10—Sn2113.2 (3)
O1—Sn3—O377.90 (11)C11—C10—Sn2111.2 (3)
O1—Sn3—O2i104.68 (11)C12—C10—H10106.5
O1—Sn3—O788.63 (11)C11—C10—H10106.5
O1—Sn3—O8160.61 (11)Sn2—C10—H10106.5
O1—Sn3—C1396.74 (14)C10—C11—H11A109.5
O2i—Sn3—O378.48 (11)C10—C11—H11B109.5
O2i—Sn3—O7157.70 (11)H11A—C11—H11B109.5
O2i—Sn3—O885.68 (11)C10—C11—H11C109.5
O2i—Sn3—C13101.11 (14)H11A—C11—H11C109.5
O3—Sn3—O787.17 (12)H11B—C11—H11C109.5
O3—Sn3—O888.45 (11)C10—C12—H12A109.5
O3—Sn3—C13174.24 (14)C10—C12—H12B109.5
O7—Sn3—O876.88 (11)H12A—C12—H12B109.5
O7—Sn3—C1394.85 (15)C10—C12—H12C109.5
O8—Sn3—C1397.25 (14)H12A—C12—H12C109.5
Sn1—O1—Sn2100.79 (12)H12B—C12—H12C109.5
Sn1—O1—Sn3131.30 (14)C15—C13—C14111.5 (4)
Sn2—O1—Sn3100.05 (12)C15—C13—Sn3114.6 (3)
Sn1—O2—Sn299.63 (12)C14—C13—Sn3110.8 (3)
Sn1—O2—Sn3i99.98 (11)C15—C13—H13106.5
Sn2—O2—Sn3i133.42 (13)C14—C13—H13106.5
Sn1i—O3—Sn2132.72 (15)Sn3—C13—H13106.5
Sn1i—O3—Sn399.77 (12)C13—C14—H14A109.5
Sn2—O3—Sn3100.02 (12)C13—C14—H14B109.5
Sn1—O4—C1128.9 (3)H14A—C14—H14B109.5
Sn2—O5—C1130.7 (3)C13—C14—H14C109.5
Sn2—O6—C3131.2 (3)H14A—C14—H14C109.5
Sn3—O7—C3129.0 (3)H14B—C14—H14C109.5
Sn3—O8—C5130.4 (3)C13—C15—H15A109.5
Sn1i—O9—C5129.5 (3)C13—C15—H15B109.5
O4—C1—O5125.8 (4)H15A—C15—H15B109.5
O5—C1—C2117.6 (4)C13—C15—H15C109.5
O4—C1—C2116.5 (4)H15A—C15—H15C109.5
C1—C2—H2A109.5H15B—C15—H15C109.5
C1—C2—H2B109.5Cl2—C16—Cl1110.5 (3)
H2A—C2—H2B109.5Cl2—C16—Cl3110.2 (3)
C1—C2—H2C109.5Cl1—C16—Cl3110.1 (3)
H2A—C2—H2C109.5Cl2—C16—H16108.7
H2B—C2—H2C109.5Cl1—C16—H16108.7
O6—C3—O7125.3 (4)Cl3—C16—H16108.7
O6—C3—C4117.9 (4)Cl5—C17—Cl4110.1 (3)
O7—C3—C4116.8 (4)Cl5—C17—Cl6110.2 (3)
C3—C4—H4A109.5Cl4—C17—Cl6111.4 (3)
C3—C4—H4B109.5Cl5—C17—H17108.4
H4A—C4—H4B109.5Cl4—C17—H17108.4
C3—C4—H4C109.5Cl6—C17—H17108.4
H4A—C4—H4C109.5
Symmetry code: (i) x, y, z+1.
 

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