Hexameric iso­propyl­oxotin acetate chloro­form tetrasolvate

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.

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

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Computing details

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)

Crystal data

[Sn6O6(C3H7)6(C2H3O2)6]·4CHCl3	F(000) = 1832
Mr = 1898.39	Dx = 2.022 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ybc	Cell parameters from 25440 reflections
a = 13.2736 (14) Å	θ = 1.5–30.1°
b = 13.5405 (16) Å	µ = 2.94 mm^−1
c = 17.3572 (19) Å	T = 193 K
β = 92.007 (3)°	Block, colourless
V = 3117.7 (6) Å^3	0.20 × 0.10 × 0.05 mm
Z = 2

Data collection

Bruker AXS SMART CCD diffractometer	9084 independent reflections
Radiation source: fine-focus sealed tube	6796 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.051
ω scans	θmax = 30.1°, θmin = 1.5°
Absorption correction: multi-scan (SADABS; Bruker, 2000)	h = −17→18
Tmin = 0.683, Tmax = 0.863	k = −15→19
25440 measured reflections	l = −24→20

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.042	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.091	H-atom parameters constrained
S = 1.01	w = 1/[σ^2(Fo^2) + (0.0368P)^2] where P = (Fo^2 + 2Fc^2)/3
9084 reflections	(Δ/σ)max = 0.001
316 parameters	Δρmax = 1.33 e Å^−3
0 restraints	Δρmin = −0.71 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Sn1	−0.15982 (2)	0.06291 (2)	0.551298 (16)	0.01713 (7)
Sn2	0.05108 (2)	0.01965 (2)	0.639897 (16)	0.01706 (7)
Sn3	0.09790 (2)	0.15655 (2)	0.495538 (16)	0.01682 (7)
Cl1	0.55261 (12)	0.21831 (13)	0.73749 (10)	0.0601 (4)
Cl2	0.44219 (14)	0.09192 (14)	0.63131 (10)	0.0616 (4)
Cl3	0.54342 (15)	0.00896 (14)	0.76583 (10)	0.0652 (5)
Cl4	0.45731 (13)	0.35390 (14)	0.55989 (12)	0.0687 (5)
Cl5	0.28630 (14)	0.48248 (13)	0.54934 (10)	0.0602 (4)
Cl6	0.38157 (15)	0.42224 (14)	0.41133 (10)	0.0673 (5)
O1	−0.0184 (2)	0.1262 (2)	0.57069 (16)	0.0183 (6)
O2	−0.0759 (2)	−0.0563 (2)	0.59474 (15)	0.0180 (6)
O3	0.1467 (2)	0.0252 (2)	0.54708 (16)	0.0191 (6)
O4	−0.1925 (2)	0.0999 (2)	0.66962 (17)	0.0253 (7)
O5	−0.0450 (2)	0.0671 (2)	0.73157 (17)	0.0235 (7)
O6	0.1410 (2)	0.1383 (2)	0.69017 (17)	0.0257 (7)
O7	0.1771 (2)	0.2330 (2)	0.58902 (16)	0.0249 (7)
O8	0.2487 (2)	0.1756 (2)	0.45239 (18)	0.0241 (7)
O9	0.2959 (2)	0.0207 (2)	0.42572 (18)	0.0235 (7)
C1	−0.1356 (4)	0.0937 (3)	0.7296 (3)	0.0241 (9)
C2	−0.1815 (4)	0.1204 (4)	0.8043 (3)	0.0361 (12)
H2A	−0.2521	0.1394	0.7948	0.054*
H2B	−0.1443	0.1758	0.8279	0.054*
H2C	−0.1781	0.0634	0.8391	0.054*
C3	0.1828 (3)	0.2113 (4)	0.6598 (3)	0.0239 (9)
C4	0.2442 (4)	0.2794 (4)	0.7117 (3)	0.0364 (12)
H4A	0.2717	0.3331	0.6809	0.055*
H4B	0.2996	0.2423	0.7367	0.055*
H4C	0.2012	0.3070	0.7510	0.055*
C5	0.3115 (3)	0.1124 (4)	0.4301 (2)	0.0241 (9)
C6	0.4113 (4)	0.1502 (4)	0.4049 (3)	0.0389 (13)
H6A	0.4528	0.0947	0.3886	0.058*
H6B	0.4457	0.1846	0.4480	0.058*
H6C	0.4005	0.1962	0.3618	0.058*
C7	−0.2387 (3)	0.1866 (3)	0.5006 (3)	0.0247 (9)
H7	−0.1910	0.2193	0.4653	0.030*
C8	−0.2667 (4)	0.2636 (4)	0.5601 (3)	0.0428 (14)
H8A	−0.2065	0.2821	0.5911	0.064*
H8B	−0.3174	0.2361	0.5938	0.064*
H8C	−0.2942	0.3222	0.5337	0.064*
C9	−0.3286 (4)	0.1547 (5)	0.4517 (3)	0.0449 (14)
H9A	−0.3078	0.1050	0.4144	0.067*
H9B	−0.3571	0.2120	0.4242	0.067*
H9C	−0.3796	0.1263	0.4847	0.067*
C10	0.1208 (3)	−0.0964 (3)	0.7072 (3)	0.0252 (9)
H10	0.1412	−0.1484	0.6699	0.030*
C11	0.0456 (4)	−0.1449 (4)	0.7600 (3)	0.0395 (13)
H11A	−0.0144	−0.1654	0.7295	0.059*
H11B	0.0260	−0.0975	0.7995	0.059*
H11C	0.0767	−0.2028	0.7849	0.059*
C12	0.2162 (4)	−0.0639 (4)	0.7504 (3)	0.0400 (13)
H12A	0.2621	−0.0336	0.7143	0.060*
H12B	0.2488	−0.1213	0.7749	0.060*
H12C	0.1992	−0.0157	0.7900	0.060*
C13	0.0328 (3)	0.2876 (3)	0.4458 (3)	0.0233 (9)
H13	−0.0296	0.2665	0.4163	0.028*
C14	−0.0014 (4)	0.3583 (4)	0.5089 (3)	0.0390 (13)
H14A	−0.0444	0.3227	0.5443	0.059*
H14B	−0.0395	0.4131	0.4852	0.059*
H14C	0.0578	0.3843	0.5375	0.059*
C15	0.0983 (4)	0.3397 (4)	0.3890 (3)	0.0390 (13)
H15A	0.1187	0.2928	0.3494	0.059*
H15B	0.1585	0.3660	0.4161	0.059*
H15C	0.0604	0.3940	0.3645	0.059*
C16	0.5475 (4)	0.1013 (4)	0.6944 (3)	0.0390 (13)
H16	0.6096	0.0916	0.6644	0.047*
C17	0.3504 (4)	0.3870 (4)	0.5044 (3)	0.0393 (12)
H17	0.3047	0.3283	0.5004	0.047*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sn1	0.01496 (13)	0.01916 (15)	0.01732 (14)	0.00026 (11)	0.00110 (10)	−0.00110 (10)
Sn2	0.01705 (14)	0.01957 (15)	0.01451 (13)	−0.00099 (11)	−0.00036 (10)	0.00010 (10)
Sn3	0.01678 (14)	0.01707 (14)	0.01664 (14)	−0.00179 (11)	0.00096 (10)	−0.00014 (10)
Cl1	0.0550 (10)	0.0567 (11)	0.0685 (11)	0.0016 (8)	0.0039 (8)	−0.0209 (8)
Cl2	0.0696 (11)	0.0547 (11)	0.0596 (10)	0.0042 (8)	−0.0134 (9)	−0.0054 (8)
Cl3	0.0835 (13)	0.0673 (12)	0.0456 (9)	0.0087 (10)	0.0125 (9)	0.0129 (8)
Cl4	0.0573 (10)	0.0604 (12)	0.0866 (13)	0.0059 (8)	−0.0240 (9)	−0.0128 (9)
Cl5	0.0739 (11)	0.0438 (10)	0.0636 (11)	0.0094 (8)	0.0143 (9)	−0.0074 (8)
Cl6	0.0941 (13)	0.0589 (11)	0.0503 (10)	−0.0209 (10)	0.0238 (9)	0.0023 (8)
O1	0.0163 (14)	0.0199 (16)	0.0186 (15)	−0.0003 (11)	0.0019 (11)	−0.0013 (11)
O2	0.0186 (14)	0.0203 (16)	0.0150 (14)	−0.0007 (12)	−0.0005 (11)	−0.0007 (11)
O3	0.0183 (14)	0.0206 (16)	0.0185 (14)	0.0003 (12)	0.0012 (11)	−0.0004 (11)
O4	0.0239 (16)	0.0331 (19)	0.0193 (16)	0.0017 (14)	0.0059 (13)	−0.0021 (13)
O5	0.0226 (15)	0.0293 (18)	0.0185 (15)	−0.0012 (13)	−0.0001 (12)	−0.0011 (12)
O6	0.0283 (17)	0.0304 (19)	0.0184 (15)	−0.0073 (14)	−0.0009 (13)	−0.0021 (12)
O7	0.0299 (17)	0.0263 (18)	0.0183 (15)	−0.0078 (13)	−0.0009 (13)	−0.0025 (12)
O8	0.0189 (15)	0.0251 (18)	0.0287 (17)	−0.0047 (12)	0.0038 (13)	−0.0028 (13)
O9	0.0176 (15)	0.0271 (18)	0.0261 (16)	−0.0012 (13)	0.0043 (12)	−0.0026 (13)
C1	0.032 (2)	0.020 (2)	0.021 (2)	−0.0047 (18)	0.0056 (19)	−0.0002 (16)
C2	0.030 (3)	0.055 (4)	0.024 (2)	−0.004 (2)	0.007 (2)	−0.010 (2)
C3	0.018 (2)	0.028 (3)	0.025 (2)	−0.0005 (18)	−0.0006 (17)	−0.0047 (18)
C4	0.041 (3)	0.039 (3)	0.029 (3)	−0.016 (2)	−0.002 (2)	−0.004 (2)
C5	0.018 (2)	0.035 (3)	0.019 (2)	−0.0044 (19)	0.0021 (17)	−0.0022 (18)
C6	0.023 (2)	0.035 (3)	0.060 (4)	−0.007 (2)	0.013 (2)	−0.005 (3)
C7	0.020 (2)	0.026 (2)	0.029 (2)	−0.0011 (18)	−0.0021 (18)	0.0039 (18)
C8	0.055 (4)	0.032 (3)	0.042 (3)	0.018 (3)	0.009 (3)	0.004 (2)
C9	0.030 (3)	0.049 (4)	0.055 (4)	0.005 (2)	−0.014 (3)	0.013 (3)
C10	0.029 (2)	0.025 (2)	0.022 (2)	0.0044 (19)	0.0000 (18)	0.0036 (17)
C11	0.045 (3)	0.040 (3)	0.034 (3)	0.000 (2)	0.007 (2)	0.016 (2)
C12	0.030 (3)	0.044 (3)	0.045 (3)	0.004 (2)	−0.015 (2)	0.007 (3)
C13	0.022 (2)	0.022 (2)	0.026 (2)	−0.0017 (18)	−0.0021 (18)	0.0025 (17)
C14	0.053 (3)	0.022 (3)	0.043 (3)	0.005 (2)	0.009 (3)	−0.001 (2)
C15	0.040 (3)	0.041 (3)	0.036 (3)	−0.004 (2)	0.006 (2)	0.020 (2)
C16	0.041 (3)	0.040 (3)	0.037 (3)	0.002 (2)	0.010 (2)	−0.002 (2)
C17	0.045 (3)	0.031 (3)	0.042 (3)	−0.007 (2)	0.003 (3)	−0.001 (2)

Geometric parameters (Å, º)

Sn1—O1	2.081 (3)	C3—C4	1.507 (6)
Sn1—O2	2.087 (3)	C4—H4A	0.9800
Sn1—O3^i	2.096 (3)	C4—H4B	0.9800
Sn1—O4	2.172 (3)	C4—H4C	0.9800
Sn1—O9^i	2.180 (3)	C5—C6	1.499 (6)
Sn1—C7	2.147 (5)	C6—H6A	0.9800
Sn2—O1	2.073 (3)	C6—H6B	0.9800
Sn2—O2	2.103 (3)	C6—H6C	0.9800
Sn2—O3	2.087 (3)	C7—C8	1.523 (7)
Sn2—O5	2.171 (3)	C7—C9	1.504 (7)
Sn2—O6	2.166 (3)	C7—H7	1.0000
Sn2—C10	2.148 (4)	C8—H8A	0.9800
Sn3—O1	2.096 (3)	C8—H8B	0.9800
Sn3—O2^i	2.086 (3)	C8—H8C	0.9800
Sn3—O3	2.083 (3)	C9—H9A	0.9800
Sn3—O7	2.166 (3)	C9—H9B	0.9800
Sn3—O8	2.177 (3)	C9—H9C	0.9800
Sn3—C13	2.142 (4)	C10—C12	1.514 (6)
Cl1—C16	1.752 (6)	C10—C11	1.527 (6)
Cl2—C16	1.750 (6)	C10—H10	1.0000
Cl3—C16	1.762 (6)	C11—H11A	0.9800
Cl4—C17	1.745 (6)	C11—H11B	0.9800
Cl5—C17	1.747 (6)	C11—H11C	0.9800
Cl6—C17	1.748 (6)	C12—H12A	0.9800
O2—Sn3^i	2.086 (3)	C12—H12B	0.9800
O3—Sn1^i	2.096 (3)	C12—H12C	0.9800
O4—C1	1.267 (5)	C13—C15	1.513 (6)
O5—C1	1.255 (5)	C13—C14	1.535 (7)
O6—C3	1.259 (5)	C13—H13	1.0000
O7—C3	1.263 (5)	C14—H14A	0.9800
O8—C5	1.265 (5)	C14—H14B	0.9800
O9—C5	1.261 (6)	C14—H14C	0.9800
O9—Sn1^i	2.180 (3)	C15—H15A	0.9800
C1—C2	1.496 (6)	C15—H15B	0.9800
C2—H2A	0.9800	C15—H15C	0.9800
C2—H2B	0.9800	C16—H16	1.0000
C2—H2C	0.9800	C17—H17	1.0000
O1—Sn1—O2	78.08 (11)	H4B—C4—H4C	109.5
O1—Sn1—O3^i	105.45 (11)	O8—C5—O9	125.2 (4)
O1—Sn1—O4	87.76 (11)	O8—C5—C6	117.1 (4)
O1—Sn1—O9^i	158.91 (11)	O9—C5—C6	117.7 (4)
O1—Sn1—C7	99.73 (14)	C5—C6—H6A	109.5
O2—Sn1—O3^i	78.19 (11)	C5—C6—H6B	109.5
O2—Sn1—O4	87.63 (11)	H6A—C6—H6B	109.5
O2—Sn1—C7	176.09 (14)	C5—C6—H6C	109.5
O2—Sn1—O9^i	88.13 (11)	H6A—C6—H6C	109.5
O3^i—Sn1—O4	157.93 (12)	H6B—C6—H6C	109.5
O3^i—Sn1—O9^i	86.93 (11)	C8—C7—C9	111.8 (4)
O3^i—Sn1—C7	99.41 (15)	C8—C7—Sn1	112.5 (3)
O4—Sn1—O9^i	75.68 (12)	C9—C7—Sn1	111.9 (3)
O4—Sn1—C7	95.55 (15)	C8—C7—H7	106.7
O9^i—Sn1—C7	94.85 (15)	C9—C7—H7	106.7
O1—Sn2—O2	77.87 (11)	Sn1—C7—H7	106.7
O1—Sn2—O3	78.33 (11)	C7—C8—H8A	109.5
O1—Sn2—O5	87.59 (11)	C7—C8—H8B	109.5
O1—Sn2—O6	86.84 (12)	H8A—C8—H8B	109.5
O1—Sn2—C10	177.03 (15)	C7—C8—H8C	109.5
O2—Sn2—O3	103.38 (11)	H8A—C8—H8C	109.5
O2—Sn2—O5	86.21 (11)	H8B—C8—H8C	109.5
O2—Sn2—O6	159.38 (12)	C7—C9—H9A	109.5
O2—Sn2—C10	99.76 (15)	C7—C9—H9B	109.5
O3—Sn2—O5	160.70 (12)	H9A—C9—H9B	109.5
O3—Sn2—O6	86.71 (11)	C7—C9—H9C	109.5
O3—Sn2—C10	100.62 (14)	H9A—C9—H9C	109.5
O5—Sn2—O6	79.33 (12)	H9B—C9—H9C	109.5
O5—Sn2—C10	94.06 (15)	C12—C10—C11	112.4 (4)
O6—Sn2—C10	95.89 (15)	C12—C10—Sn2	113.2 (3)
O1—Sn3—O3	77.90 (11)	C11—C10—Sn2	111.2 (3)
O1—Sn3—O2^i	104.68 (11)	C12—C10—H10	106.5
O1—Sn3—O7	88.63 (11)	C11—C10—H10	106.5
O1—Sn3—O8	160.61 (11)	Sn2—C10—H10	106.5
O1—Sn3—C13	96.74 (14)	C10—C11—H11A	109.5
O2^i—Sn3—O3	78.48 (11)	C10—C11—H11B	109.5
O2^i—Sn3—O7	157.70 (11)	H11A—C11—H11B	109.5
O2^i—Sn3—O8	85.68 (11)	C10—C11—H11C	109.5
O2^i—Sn3—C13	101.11 (14)	H11A—C11—H11C	109.5
O3—Sn3—O7	87.17 (12)	H11B—C11—H11C	109.5
O3—Sn3—O8	88.45 (11)	C10—C12—H12A	109.5
O3—Sn3—C13	174.24 (14)	C10—C12—H12B	109.5
O7—Sn3—O8	76.88 (11)	H12A—C12—H12B	109.5
O7—Sn3—C13	94.85 (15)	C10—C12—H12C	109.5
O8—Sn3—C13	97.25 (14)	H12A—C12—H12C	109.5
Sn1—O1—Sn2	100.79 (12)	H12B—C12—H12C	109.5
Sn1—O1—Sn3	131.30 (14)	C15—C13—C14	111.5 (4)
Sn2—O1—Sn3	100.05 (12)	C15—C13—Sn3	114.6 (3)
Sn1—O2—Sn2	99.63 (12)	C14—C13—Sn3	110.8 (3)
Sn1—O2—Sn3^i	99.98 (11)	C15—C13—H13	106.5
Sn2—O2—Sn3^i	133.42 (13)	C14—C13—H13	106.5
Sn1^i—O3—Sn2	132.72 (15)	Sn3—C13—H13	106.5
Sn1^i—O3—Sn3	99.77 (12)	C13—C14—H14A	109.5
Sn2—O3—Sn3	100.02 (12)	C13—C14—H14B	109.5
Sn1—O4—C1	128.9 (3)	H14A—C14—H14B	109.5
Sn2—O5—C1	130.7 (3)	C13—C14—H14C	109.5
Sn2—O6—C3	131.2 (3)	H14A—C14—H14C	109.5
Sn3—O7—C3	129.0 (3)	H14B—C14—H14C	109.5
Sn3—O8—C5	130.4 (3)	C13—C15—H15A	109.5
Sn1^i—O9—C5	129.5 (3)	C13—C15—H15B	109.5
O4—C1—O5	125.8 (4)	H15A—C15—H15B	109.5
O5—C1—C2	117.6 (4)	C13—C15—H15C	109.5
O4—C1—C2	116.5 (4)	H15A—C15—H15C	109.5
C1—C2—H2A	109.5	H15B—C15—H15C	109.5
C1—C2—H2B	109.5	Cl2—C16—Cl1	110.5 (3)
H2A—C2—H2B	109.5	Cl2—C16—Cl3	110.2 (3)
C1—C2—H2C	109.5	Cl1—C16—Cl3	110.1 (3)
H2A—C2—H2C	109.5	Cl2—C16—H16	108.7
H2B—C2—H2C	109.5	Cl1—C16—H16	108.7
O6—C3—O7	125.3 (4)	Cl3—C16—H16	108.7
O6—C3—C4	117.9 (4)	Cl5—C17—Cl4	110.1 (3)
O7—C3—C4	116.8 (4)	Cl5—C17—Cl6	110.2 (3)
C3—C4—H4A	109.5	Cl4—C17—Cl6	111.4 (3)
C3—C4—H4B	109.5	Cl5—C17—H17	108.4
H4A—C4—H4B	109.5	Cl4—C17—H17	108.4
C3—C4—H4C	109.5	Cl6—C17—H17	108.4
H4A—C4—H4C	109.5

Symmetry code: (i) −x, −y, −z+1.