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The centrosymmetric hexanuclear title compound, hexa-μ2-acetato-hexa-μ3-oxo-hexakis­[(tri­methyl­silyl­methyl)­tin], [Sn6O6(C2H3O2)6(C4H11Si)6], adopts a `drum' structure in which two [(Me3SiCH2)SnO]3 caps are linked to each other via six μ3-O atoms and six bidentate bridging acetate groups. A CO5 donor set defines a distorted octahedral environment for each of the three independent Sn atoms.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804011055/ng6029sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804011055/ng6029Isup2.hkl
Contains datablock I

CCDC reference: 242039

Key indicators

  • Single-crystal X-ray study
  • T = 223 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.044
  • wR factor = 0.093
  • Data-to-parameter ratio = 31.5

checkCIF/PLATON results

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Alert level C PLAT230_ALERT_2_C Hirshfeld Test Diff for O9 - C5 .. 5.48 su PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Si1 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Si2 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Si3 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.18 Ratio
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; 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.

(I) top
Crystal data top
[Sn6O6(C2H3O2)6(C4H11Si)6]F(000) = 1656
Mr = 1685.71Dx = 1.717 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ynCell parameters from 4788 reflections
a = 13.8888 (7) Åθ = 2.7–29.4°
b = 18.8359 (9) ŵ = 2.43 mm1
c = 13.9301 (7) ÅT = 223 K
β = 116.545 (1)°Plate, colourless
V = 3260.1 (3) Å30.23 × 0.18 × 0.07 mm
Z = 2
Data collection top
Bruker AXS SMART CCD
diffractometer
9482 independent reflections
Radiation source: fine-focus sealed tube7215 reflections with I > 2σ(I)'
Graphite monochromatorRint = 0.038
ω scansθmax = 30.1°, θmin = 1.7°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 1719
Tmin = 0.549, Tmax = 0.844k = 2326
27420 measured reflectionsl = 1919
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)] = 0.044Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.093H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.04P)2]
where P = (Fo2 + 2Fc2)/3
9482 reflections(Δ/σ)max = 0.001
301 parametersΔρmax = 1.12 e Å3
0 restraintsΔρmin = 0.71 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sn10.62141 (2)0.600200 (12)0.509165 (19)0.02594 (7)
Sn20.46104 (2)0.507660 (12)0.308208 (19)0.02607 (7)
Sn30.39091 (2)0.601436 (12)0.509042 (19)0.02534 (7)
Si10.86106 (10)0.69134 (6)0.65932 (9)0.0383 (3)
Si20.26655 (11)0.47971 (6)0.04809 (9)0.0396 (3)
Si30.12374 (10)0.61915 (6)0.45079 (10)0.0400 (3)
O10.6127 (2)0.50140 (11)0.4393 (2)0.0275 (6)
O20.4585 (2)0.59181 (12)0.40428 (19)0.0270 (5)
O30.5535 (2)0.58229 (12)0.61322 (19)0.0261 (5)
O40.6496 (2)0.64077 (14)0.3791 (2)0.0367 (6)
O50.5307 (2)0.58039 (14)0.2374 (2)0.0372 (7)
O60.5921 (2)0.71129 (13)0.5200 (2)0.0352 (6)
O70.4306 (2)0.71251 (13)0.5189 (2)0.0340 (6)
O80.5193 (2)0.43673 (14)0.2238 (2)0.0350 (6)
O90.6259 (2)0.36276 (13)0.3527 (2)0.0330 (6)
C10.6068 (4)0.6227 (2)0.2814 (3)0.0350 (9)
C20.6530 (4)0.6558 (3)0.2123 (4)0.0546 (13)
H2A0.71490.62860.21890.082*
H2B0.67480.70420.23560.082*
H2C0.59880.65590.13800.082*
C30.5150 (3)0.7419 (2)0.5266 (3)0.0342 (9)
C40.5250 (4)0.8205 (2)0.5461 (4)0.0533 (12)
H4A0.60000.83430.57450.080*
H4B0.49800.83270.59730.080*
H4C0.48330.84530.47910.080*
C50.5817 (3)0.3843 (2)0.2582 (3)0.0335 (9)
C60.6053 (4)0.3435 (2)0.1782 (3)0.0474 (12)
H6A0.67470.35780.18400.071*
H6B0.54990.35320.10630.071*
H6C0.60640.29310.19280.071*
C70.7872 (3)0.6051 (2)0.6175 (3)0.0366 (9)
H7A0.79610.58100.68330.044*
H7B0.82510.57640.58650.044*
C80.8469 (4)0.7459 (3)0.5429 (4)0.0678 (16)
H8A0.87030.71850.49810.102*
H8B0.89090.78820.56830.102*
H8C0.77210.75940.50140.102*
C90.8145 (5)0.7428 (3)0.7437 (4)0.0693 (16)
H9A0.82220.71420.80470.104*
H9B0.73950.75550.70170.104*
H9C0.85740.78560.76900.104*
C101.0059 (4)0.6690 (3)0.7421 (4)0.0638 (15)
H10A1.03200.64200.69920.096*
H10B1.01370.64100.80360.096*
H10C1.04730.71240.76670.096*
C110.3042 (3)0.5199 (2)0.1820 (3)0.0365 (9)
H11A0.25400.50120.20770.044*
H11B0.29040.57100.17090.044*
C120.3524 (6)0.5160 (3)0.0104 (5)0.081 (2)
H12A0.34650.56740.01390.122*
H12B0.32910.49710.08210.122*
H12C0.42670.50270.03420.122*
C130.2771 (5)0.3820 (2)0.0570 (5)0.0755 (18)
H13A0.35100.36860.10310.113*
H13B0.25510.36230.01410.113*
H13C0.23080.36380.08670.113*
C140.1233 (5)0.5031 (3)0.0410 (5)0.0751 (19)
H14A0.11600.55430.04740.113*
H14B0.07780.48470.01050.113*
H14C0.10180.48250.11150.113*
C150.2264 (3)0.6117 (2)0.3997 (3)0.0354 (9)
H15A0.21930.65380.35570.042*
H15B0.20710.57060.35160.042*
C160.0124 (4)0.6096 (3)0.3344 (4)0.0770 (18)
H16A0.01800.56340.30140.116*
H16B0.02250.64650.28220.116*
H16C0.06720.61390.35920.116*
C170.1405 (4)0.5482 (3)0.5514 (4)0.0581 (13)
H17A0.21020.55330.61310.087*
H17B0.13580.50190.51910.087*
H17C0.08410.55260.57410.087*
C180.1323 (4)0.7077 (2)0.5128 (4)0.0605 (14)
H18A0.20220.71300.57410.091*
H18B0.07640.71170.53620.091*
H18C0.12270.74440.46060.091*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn10.03009 (14)0.02280 (12)0.02725 (13)0.00153 (10)0.01489 (11)0.00009 (10)
Sn20.03226 (15)0.02612 (13)0.02143 (13)0.00152 (10)0.01343 (11)0.00080 (9)
Sn30.02978 (14)0.02320 (12)0.02516 (13)0.00236 (10)0.01417 (11)0.00028 (10)
Si10.0379 (7)0.0363 (6)0.0379 (6)0.0074 (5)0.0143 (5)0.0006 (5)
Si20.0438 (7)0.0409 (6)0.0299 (6)0.0013 (5)0.0127 (5)0.0043 (5)
Si30.0332 (7)0.0420 (7)0.0486 (7)0.0022 (5)0.0217 (6)0.0070 (6)
O10.0330 (15)0.0247 (13)0.0266 (13)0.0006 (10)0.0151 (11)0.0001 (10)
O20.0327 (15)0.0250 (13)0.0239 (13)0.0008 (10)0.0132 (11)0.0017 (10)
O30.0310 (15)0.0244 (12)0.0245 (13)0.0000 (10)0.0138 (11)0.0012 (10)
O40.0454 (18)0.0359 (15)0.0349 (15)0.0050 (13)0.0234 (13)0.0019 (12)
O50.0475 (19)0.0364 (15)0.0322 (15)0.0048 (13)0.0218 (13)0.0039 (12)
O60.0366 (17)0.0244 (13)0.0464 (17)0.0001 (12)0.0203 (13)0.0006 (12)
O70.0402 (17)0.0245 (13)0.0384 (15)0.0035 (12)0.0184 (13)0.0027 (11)
O80.0425 (17)0.0377 (15)0.0296 (14)0.0049 (13)0.0203 (13)0.0012 (12)
O90.0446 (18)0.0309 (14)0.0278 (14)0.0040 (12)0.0199 (13)0.0016 (11)
C10.044 (3)0.031 (2)0.040 (2)0.0035 (18)0.029 (2)0.0049 (18)
C20.072 (4)0.056 (3)0.053 (3)0.015 (3)0.044 (3)0.003 (2)
C30.045 (3)0.0247 (19)0.029 (2)0.0009 (17)0.0128 (18)0.0013 (16)
C40.055 (3)0.028 (2)0.078 (3)0.003 (2)0.030 (3)0.006 (2)
C50.038 (2)0.034 (2)0.039 (2)0.0053 (17)0.0262 (19)0.0068 (17)
C60.070 (3)0.047 (3)0.036 (2)0.012 (2)0.034 (2)0.006 (2)
C70.033 (2)0.033 (2)0.041 (2)0.0023 (17)0.0149 (18)0.0001 (18)
C80.064 (4)0.071 (4)0.065 (3)0.018 (3)0.025 (3)0.023 (3)
C90.079 (4)0.062 (3)0.054 (3)0.006 (3)0.017 (3)0.018 (3)
C100.042 (3)0.063 (3)0.073 (4)0.008 (2)0.013 (3)0.003 (3)
C110.039 (2)0.041 (2)0.028 (2)0.0080 (19)0.0135 (18)0.0004 (17)
C120.099 (5)0.111 (5)0.045 (3)0.019 (4)0.043 (3)0.004 (3)
C130.054 (4)0.047 (3)0.107 (5)0.000 (3)0.019 (3)0.016 (3)
C140.065 (4)0.077 (4)0.051 (3)0.021 (3)0.003 (3)0.017 (3)
C150.035 (2)0.041 (2)0.033 (2)0.0036 (18)0.0172 (18)0.0016 (17)
C160.042 (3)0.114 (5)0.072 (4)0.006 (3)0.023 (3)0.014 (4)
C170.063 (4)0.055 (3)0.070 (3)0.013 (3)0.042 (3)0.007 (3)
C180.058 (3)0.049 (3)0.082 (4)0.010 (2)0.038 (3)0.007 (3)
Geometric parameters (Å, º) top
Sn1—O12.078 (2)C2—H2A0.9700
Sn1—O22.079 (3)C2—H2B0.9700
Sn1—O32.080 (2)C2—H2C0.9700
Sn1—O42.157 (3)C3—C41.501 (5)
Sn1—O62.150 (2)C4—H4A0.9700
Sn1—C72.117 (4)C4—H4B0.9700
Sn2—O12.085 (3)C4—H4C0.9700
Sn2—O22.085 (2)C5—C61.506 (5)
Sn2—O3i2.075 (2)C6—H6A0.9700
Sn2—O52.153 (3)C6—H6B0.9700
Sn2—O82.162 (3)C6—H6C0.9700
Sn2—C112.113 (4)C7—H7A0.9800
Sn3—O1i2.075 (2)C7—H7B0.9800
Sn3—O22.066 (2)C8—H8A0.9700
Sn3—O32.099 (3)C8—H8B0.9700
Sn3—O72.152 (3)C8—H8C0.9700
Sn3—O9i2.149 (2)C9—H9A0.9700
Sn3—C152.114 (4)C9—H9B0.9700
Sn1—Sn23.2036 (4)C9—H9C0.9700
Sn1—Sn33.2007 (4)C10—H10A0.9700
Sn2—Sn3i3.2020 (4)C10—H10B0.9700
Sn3—Sn2i3.2020 (4)C10—H10C0.9700
Si1—C91.849 (5)C11—H11A0.9800
Si1—C81.855 (5)C11—H11B0.9800
Si1—C71.869 (4)C12—H12A0.9700
Si1—C101.865 (5)C12—H12B0.9700
Si2—C131.845 (5)C12—H12C0.9700
Si2—C141.867 (6)C13—H13A0.9700
Si2—C111.858 (4)C13—H13B0.9700
Si2—C121.850 (6)C13—H13C0.9700
Si3—C161.870 (5)C14—H14A0.9700
Si3—C181.857 (5)C14—H14B0.9700
Si3—C151.862 (4)C14—H14C0.9700
Si3—C171.875 (5)C15—H15A0.9800
O1—Sn3i2.075 (2)C15—H15B0.9800
O3—Sn2i2.075 (2)C16—H16A0.9700
O4—C11.264 (5)C16—H16B0.9700
O5—C11.245 (5)C16—H16C0.9700
O6—C31.255 (5)C17—H17A0.9700
O7—C31.258 (5)C17—H17B0.9700
O8—C51.259 (5)C17—H17C0.9700
O9—C51.246 (5)C18—H18A0.9700
O9—Sn3i2.149 (2)C18—H18B0.9700
C1—C21.509 (5)C18—H18C0.9700
O1—Sn1—O6158.61 (10)Sn1—O3—Sn2i132.93 (12)
O2—Sn1—C7178.06 (12)Sn1—O3—Sn399.97 (10)
O3—Sn1—O4162.12 (10)Sn2i—O3—Sn3100.19 (10)
O1—Sn2—C11175.60 (12)C1—O4—Sn1129.4 (3)
O2—Sn2—O8159.53 (10)C1—O5—Sn2129.7 (2)
O3i—Sn2—O5158.49 (10)C3—O6—Sn1130.3 (3)
O1i—Sn3—O7158.53 (10)C3—O7—Sn3129.4 (3)
O2—Sn3—O9i157.81 (10)C5—O8—Sn2129.7 (2)
O3—Sn3—C15175.13 (13)C5—O9—Sn3i130.2 (2)
O1—Sn1—O3103.37 (10)O5—C1—O4126.1 (4)
O1—Sn1—O277.60 (10)O5—C1—C2117.4 (4)
O3—Sn1—O277.73 (10)O4—C1—C2116.5 (4)
O1—Sn1—C7100.98 (13)C1—C2—H2A109.5
O3—Sn1—C7101.41 (14)C1—C2—H2B109.5
O1—Sn1—O485.33 (10)H2A—C2—H2B109.5
O2—Sn1—O489.17 (10)C1—C2—H2C109.5
C7—Sn1—O492.03 (14)H2A—C2—H2C109.5
O3—Sn1—O687.14 (10)H2B—C2—H2C109.5
O2—Sn1—O686.72 (10)O6—C3—O7125.9 (4)
C7—Sn1—O694.98 (13)O6—C3—C4117.0 (4)
O4—Sn1—O679.92 (10)O7—C3—C4117.1 (4)
O1—Sn1—Sn399.04 (7)C3—C4—H4A109.5
O3—Sn1—Sn340.23 (7)C3—C4—H4B109.5
O2—Sn1—Sn339.31 (6)H4A—C4—H4B109.5
C7—Sn1—Sn3140.27 (12)C3—C4—H4C109.5
O4—Sn1—Sn3123.63 (8)H4A—C4—H4C109.5
O6—Sn1—Sn376.85 (7)H4B—C4—H4C109.5
O1—Sn1—Sn239.76 (8)O9—C5—O8126.0 (3)
O3—Sn1—Sn299.55 (7)O9—C5—C6116.7 (4)
O2—Sn1—Sn239.77 (6)O8—C5—C6117.3 (4)
C7—Sn1—Sn2139.18 (11)C5—C6—H6A109.5
O4—Sn1—Sn277.01 (7)C5—C6—H6B109.5
O6—Sn1—Sn2120.76 (7)H6A—C6—H6B109.5
Sn3—Sn1—Sn272.472 (9)C5—C6—H6C109.5
O3i—Sn2—O2104.40 (10)H6A—C6—H6C109.5
O3i—Sn2—O177.88 (9)H6B—C6—H6C109.5
O2—Sn2—O177.34 (9)Si1—C7—Sn1122.1 (2)
O3i—Sn2—C11102.75 (14)Si1—C7—H7A106.8
O2—Sn2—C1198.33 (12)Sn1—C7—H7A106.8
O2—Sn2—O587.12 (10)Si1—C7—H7B106.8
O1—Sn2—O587.28 (10)Sn1—C7—H7B106.8
C11—Sn2—O593.24 (14)H7A—C7—H7B106.7
O3i—Sn2—O886.01 (10)Si1—C8—H8A109.5
O1—Sn2—O887.97 (10)Si1—C8—H8B109.5
C11—Sn2—O896.41 (13)H8A—C8—H8B109.5
O5—Sn2—O877.90 (11)Si1—C8—H8C109.5
O3i—Sn2—Sn3i40.18 (7)H8A—C8—H8C109.5
O2—Sn2—Sn3i99.59 (7)H8B—C8—H8C109.5
O1—Sn2—Sn3i39.54 (6)Si1—C9—H9A109.5
C11—Sn2—Sn3i142.02 (12)Si1—C9—H9B109.5
O5—Sn2—Sn3i120.81 (8)H9A—C9—H9B109.5
O8—Sn2—Sn3i76.85 (7)Si1—C9—H9C109.5
O3i—Sn2—Sn1100.19 (7)H9A—C9—H9C109.5
O2—Sn2—Sn139.64 (7)H9B—C9—H9C109.5
O1—Sn2—Sn139.62 (6)Si1—C10—H10A109.5
C11—Sn2—Sn1136.34 (11)Si1—C10—H10B109.5
O5—Sn2—Sn176.98 (7)H10A—C10—H10B109.5
O8—Sn2—Sn1121.92 (8)Si1—C10—H10C109.5
Sn3i—Sn2—Sn172.889 (9)H10A—C10—H10C109.5
O2—Sn3—O1i104.59 (9)H10B—C10—H10C109.5
O2—Sn3—O377.59 (10)Si2—C11—Sn2120.9 (2)
O1i—Sn3—O377.58 (10)Si2—C11—H11A107.1
O2—Sn3—C15100.68 (12)Sn2—C11—H11A107.1
O1i—Sn3—C1598.60 (14)Si2—C11—H11B107.1
O1i—Sn3—O9i87.32 (10)Sn2—C11—H11B107.1
O3—Sn3—O9i87.05 (10)H11A—C11—H11B106.8
C15—Sn3—O9i95.84 (13)Si2—C12—H12A109.5
O2—Sn3—O786.92 (10)Si2—C12—H12B109.5
O3—Sn3—O787.56 (10)H12A—C12—H12B109.5
C15—Sn3—O796.92 (13)Si2—C12—H12C109.5
O9i—Sn3—O776.41 (10)H12A—C12—H12C109.5
O2—Sn3—Sn139.60 (7)H12B—C12—H12C109.5
O1i—Sn3—Sn199.90 (7)Si2—C13—H13A109.5
O3—Sn3—Sn139.80 (6)Si2—C13—H13B109.5
C15—Sn3—Sn1139.46 (10)H13A—C13—H13B109.5
O9i—Sn3—Sn1120.73 (8)Si2—C13—H13C109.5
O7—Sn3—Sn177.27 (7)H13A—C13—H13C109.5
O2—Sn3—Sn2i99.91 (7)H13B—C13—H13C109.5
O1i—Sn3—Sn2i39.78 (8)Si2—C14—H14A109.5
O3—Sn3—Sn2i39.63 (6)Si2—C14—H14B109.5
C15—Sn3—Sn2i137.30 (11)H14A—C14—H14B109.5
O9i—Sn3—Sn2i77.13 (7)Si2—C14—H14C109.5
O7—Sn3—Sn2i121.21 (7)H14A—C14—H14C109.5
Sn1—Sn3—Sn2i73.030 (9)H14B—C14—H14C109.5
C9—Si1—C8109.6 (3)Si3—C15—Sn3119.8 (2)
C9—Si1—C7110.7 (2)Si3—C15—H15A107.4
C8—Si1—C7112.3 (2)Sn3—C15—H15A107.4
C9—Si1—C10108.2 (3)Si3—C15—H15B107.4
C8—Si1—C10109.2 (2)Sn3—C15—H15B107.4
C7—Si1—C10106.7 (2)H15A—C15—H15B106.9
C13—Si2—C14108.0 (2)Si3—C16—H16A109.5
C13—Si2—C11111.1 (2)Si3—C16—H16B109.5
C14—Si2—C11108.0 (2)H16A—C16—H16B109.5
C13—Si2—C12110.5 (3)Si3—C16—H16C109.5
C14—Si2—C12109.0 (3)H16A—C16—H16C109.5
C11—Si2—C12110.1 (2)H16B—C16—H16C109.5
C16—Si3—C18108.6 (3)Si3—C17—H17A109.5
C16—Si3—C15108.1 (2)Si3—C17—H17B109.5
C18—Si3—C15110.2 (2)H17A—C17—H17B109.5
C16—Si3—C17108.6 (3)Si3—C17—H17C109.5
C18—Si3—C17109.4 (2)H17A—C17—H17C109.5
C15—Si3—C17111.8 (2)H17B—C17—H17C109.5
Sn1—O1—Sn3i132.77 (13)Si3—C18—H18A109.5
Sn1—O1—Sn2100.62 (10)Si3—C18—H18B109.5
Sn3i—O1—Sn2100.68 (10)H18A—C18—H18B109.5
Sn3—O2—Sn2131.55 (12)Si3—C18—H18C109.5
Sn3—O2—Sn1101.08 (10)H18A—C18—H18C109.5
Sn2—O2—Sn1100.60 (10)H18B—C18—H18C109.5
Symmetry code: (i) x+1, y+1, z+1.
 

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