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In the solid state, the title compound, di-μ-hydroxo-1:2κ2O;-3:4κ2O-dihydroxo-1κO,4κO-octakis(2-methyl-2-phenyl­propyl)-1κ2C,2κ2C,3κ2C,4κ2C-di-μ3-oxo-1:2:3κ3O;2:3:4κ3O-tetratin(IV), [Sn4O2(OH)4(C10H13)8], forms centrosymmetric dimeric [(Neophyl2SnOH)(Neophyl2SnOH)O]2 mol­ecules (Neophyl = 2-methyl-2-phenylpropyl), with an almost planar Sn–O framework that adopts a ladder-type structure consisting of three four-membered rings. The hydroxyl groups are shielded by the organic groups, which prevent them from further condensation and from the formation of hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100006016/na1470sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100006016/na1470Isup2.hkl
Contains datablock I

CCDC reference: 147629

Comment top

Although the first step of the hydrolysis of diorganotin dihalides, R2SnX2, (1) (X = Cl, Br or I), namely, the formation of a dimeric `hydroxide halide' R2Sn(OH)X, (2) (Puff et al., 1985), is common to all kinds of organic groups R, further hydrolysis products depend on the size of the two organic ligands. Thus, the complete hydrolysis of (1) with bulky organic groups such as tert-butyl (Puff, Schuh et al., 1981) or mesityl (Weber et al., 1982) results in the formation of soluble trimeric `oxides' (R2SnO)3, (3), with tetrahedrally coordinated Sn. In the case of small organic groups such as isopropyl or phenyl, however, complete hydrolysis leads to the formation of insoluble polymeric `oxides' (R2SnO)n, (4), the structure of which is unknown. On the way to this final product, three intermediates can be isolated, all showing the so-called `ladder-type structure', because their inorganic framework consists of three four-membered rings, with fivefold trigonal-bipyramidally coordinated Sn. According to the degree of hydrolysis and condensation one can distinguish between the so-called `dihalides' [(R2SnX)(R2SnX)O]2, (5), `hydroxide halides' [(R2SnX)(R2SnOH)O]2, (6) and `dihydroxides' [(R2SnOH)(R2SnOH)O]2, (7). Although in the literature there are numerous examples described for compounds of types (5) (Harrison et al., 1980; Puff, Friedrichs & Visel, 1981; Graziani et al., 1983; Dakternieks et al., 1984; Vollano et al., 1984; Hamalainen & Turpeinen, 1987; Beckmann et al., 1998) and (6) (Vollano et al., 1984; Puff et al., 1983; Tiekink, 1991; Kresinski et al., 1994; Cox & Tiekink, 1994), only one compound with R = trimethylsilylmethyl (Puff, Friedrichs & Visel, 1981) is known to be of type (7), because this step in the course of the hydrolysis is difficult to prepare. Only by chance we found, in our study of tris(2,2-dimethyl-2-phenylethyl)tin halides (Neophyl3SnX, X = F, Cl, Br or I; Neophyl = 2,2-dimethyl-2-phenylethyl), a second compound of this type (7), the title compound, (I). \sch

The crystal structure of (I) consists of centrosymmetric [Neophyl2SnOH)(Neophyl2SnOH)O]2 molecules with an almost planar Sn—O framework. This is characterized by a central four-membered Sn—O ring with small O1—Sn1—O1i angles [73.19 (9)°] and broadened Sn1—O1—Sn1i angles [106.81 (9)°] [symmetry code: (i) 2 − x, 2 − y, 1 − z]. These values are typical for such a building unit and are also found for example in (5) and (6), as well as in cassiterite, SnO2 (Bolzan et al., 1997). The two outer four-membered Sn—O rings differ from this geometry because only the oxygen atom O1 is of the µ3-type; the other one belongs to a µ2-OH function and therefore the bond lengths and angles are different. In particular, the bridging OH group shows great differences in bond lengths: 2.325 (3) to the outer and 2.110 (2) Å to the inner Sn atom. The bond angles are O1—Sn1—O2 = 74.57 (19) and O1—Sn2—O2 = 70.34 (9)°; Sn1—O2—Sn2 = 100.87 (19) at the µ3-O and Sn2—O1—Sn1 = 114.13 (11)° at the µ2-OH group.

Both Sn atoms have a distorted trigonal bipyramidal coordination, with two O atoms in the axial positions and two C and one further O in the equatorial positions. However, the axes of these trigonal bipyramids are to some extent bent, as shown by the angles O2—Sn1—O1i = 147.75 (9) and O2—Sn2—O3 = 159.0 (1)°. Similar distortion can also be found in the ladder-type structures of (5) and (6). The mean Sn—C distance is 2.152 Å, which is slightly shorter than the Sn—C distance in the corresponding tetraneopyhltin compound (2.186 Å; Reuter & Pawlak, 1998).

The organic groups in (I) shield the Sn—O framework and prevent it from further condensation and from the formation of intermolecular hydrogen bonding.

Experimental top

The title compound was obtained by chance during the preparation of trineophyltin iodide, Neophyl3SnI, from trineophyltin chloride via the corresponding distannoxane. For this purpose the chloride was hydrolyzed by concentrated potassium hydroxide solution in a heated toluene-water mixture. Most of the organic layer containing the distannoxane was decanted and worked up; the aqueous reaction mixture, which also contained a small amount of the organic solution, was left aside. After some weeks most of the solvent had evaporated and some clear transparent crystals of (I) had formed. It is known (Davies, 1997) that tetraorganodistannoxanes often separate from samples of triorganotin halides when stored for longer periods. A suitable single-crystal of (I) for X-ray structure determination was selected using a polarization microscope and mounted on top of a Lindemann capillary with a cyanoacrylate adhesive.

Refinement top

The positions of the H atoms on the OH groups were found in difference Fourier maps. Full ref?

Computing details top

Data collection: XSCANS (Siemens, 1996); cell refinement: XSCANS; data reduction: SHELXTL (Sheldrick, 1997b); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. A perspective view of the asymmetric unit of (I) and the centrosymmetric atoms of the Sn—O framework. Sn and O atoms are plotted as displacement ellipsoids at the 50% probability level; other atoms are shown as small spheres of arbitrary radii. Some of the neophyl groups (R) are omitted for clarity [symmetry code: (i) 2 − x, 2 − y, 1 − z].
(I) top
Crystal data top
[Sn4O2(OH)4(C10H13)8]Z = 1
Mr = 1640.42F(000) = 836
Triclinic, P1Dx = 1.436 Mg m3
a = 10.878 (2) ÅMo Kα radiation, λ = 0.71073 Å
b = 11.598 (3) ÅCell parameters from 20 reflections
c = 17.077 (2) Åθ = 5.1–12.5°
α = 73.19 (2)°µ = 1.35 mm1
β = 81.944 (19)°T = 293 K
γ = 66.91 (2)°Block, colourless
V = 1896.4 (7) Å30.43 × 0.29 × 0.25 mm
Data collection top
Siemens P4
diffractometer
5394 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.033
Graphite monochromatorθmax = 25.0°, θmin = 2.0°
2θ/ω scansh = 121
Absorption correction: ψ-scan
SHELXTL (Sheldrick, 1997b)
k = 1312
Tmin = 0.652, Tmax = 0.713l = 2020
7739 measured reflections3 standard reflections every 97 reflections
6615 independent reflections intensity decay: none
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.028H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.072 w = 1/[σ2(Fo2) + (0.0339P)2 + 0.3893P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.011
6615 reflectionsΔρmax = 0.62 e Å3
408 parametersΔρmin = 0.51 e Å3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 1997a), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0007 (2)
Crystal data top
[Sn4O2(OH)4(C10H13)8]γ = 66.91 (2)°
Mr = 1640.42V = 1896.4 (7) Å3
Triclinic, P1Z = 1
a = 10.878 (2) ÅMo Kα radiation
b = 11.598 (3) ŵ = 1.35 mm1
c = 17.077 (2) ÅT = 293 K
α = 73.19 (2)°0.43 × 0.29 × 0.25 mm
β = 81.944 (19)°
Data collection top
Siemens P4
diffractometer
5394 reflections with I > 2σ(I)
Absorption correction: ψ-scan
SHELXTL (Sheldrick, 1997b)
Rint = 0.033
Tmin = 0.652, Tmax = 0.7133 standard reflections every 97 reflections
7739 measured reflections intensity decay: none
6615 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0280 restraints
wR(F2) = 0.072H atoms treated by a mixture of independent and constrained refinement
S = 1.03Δρmax = 0.62 e Å3
6615 reflectionsΔρmin = 0.51 e Å3
408 parameters
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
Sn10.96953 (2)0.86217 (2)0.54208 (1)0.03170 (7)
Sn20.89888 (2)1.03778 (2)0.68393 (1)0.03524 (8)
O10.9655 (2)1.0250 (2)0.56851 (13)0.0355 (5)
O20.9060 (3)0.8439 (3)0.66611 (15)0.0441 (6)
H20.93260.76930.69500.093 (3)*
O30.9227 (3)1.2114 (3)0.65745 (18)0.0542 (7)
H30.84971.27070.64820.093 (3)*
C1101.1459 (4)0.6894 (4)0.5483 (3)0.0526 (10)
H110A1.11600.61740.56000.093 (3)*
H110B1.18700.69630.49380.093 (3)*
C1111.2570 (4)0.6499 (4)0.6078 (3)0.0481 (9)
C1121.2946 (5)0.7673 (5)0.5966 (4)0.0781 (16)
H112A1.31670.79790.54000.093 (3)*
H112B1.37040.74300.62910.093 (3)*
H112C1.22050.83490.61380.093 (3)*
C1131.3800 (5)0.5422 (5)0.5817 (4)0.0803 (17)
H113A1.40470.57340.52570.093 (3)*
H113B1.35830.46750.58720.093 (3)*
H113C1.45330.51900.61590.093 (3)*
C1141.2210 (5)0.5970 (4)0.6965 (3)0.0567 (11)
C1151.1225 (8)0.5486 (7)0.7188 (4)0.099 (2)
H1151.07360.54670.67900.093 (3)*
C1161.0946 (12)0.5018 (10)0.8014 (6)0.162 (5)
H1161.02730.46840.81620.093 (3)*
C1171.1619 (16)0.5040 (11)0.8586 (6)0.183 (8)
H1171.13810.47660.91330.093 (3)*
C1181.2660 (14)0.5457 (9)0.8395 (5)0.153 (6)
H1181.31790.54140.88000.093 (3)*
C1191.2907 (8)0.5939 (6)0.7589 (4)0.100 (2)
H1191.35860.62670.74520.093 (3)*
C1200.7838 (4)0.8892 (3)0.4948 (2)0.0400 (7)
H120A0.71260.95020.52020.093 (3)*
H120B0.78490.93110.43680.093 (3)*
C1210.7441 (4)0.7717 (4)0.5045 (2)0.0410 (8)
C1220.8472 (5)0.6789 (5)0.4575 (3)0.0642 (13)
H122A0.85380.72510.40150.093 (3)*
H122B0.81940.60900.45970.093 (3)*
H122C0.93280.64460.48200.093 (3)*
C1230.6102 (5)0.8214 (5)0.4628 (3)0.0617 (12)
H123A0.61960.86330.40610.093 (3)*
H123B0.54310.88230.48920.093 (3)*
H123C0.58410.74970.46690.093 (3)*
C1240.7278 (4)0.7055 (4)0.5943 (3)0.0456 (8)
C1250.8010 (7)0.5764 (5)0.6290 (4)0.0800 (16)
H1250.86550.52750.59730.093 (3)*
C1260.7802 (13)0.5198 (9)0.7085 (5)0.140 (4)
H1260.83060.43250.72990.093 (3)*
C1270.6902 (12)0.5848 (11)0.7568 (5)0.136 (4)
H1270.67740.54360.81100.093 (3)*
C1280.6151 (8)0.7156 (10)0.7253 (4)0.106 (3)
H1280.55270.76270.75860.093 (3)*
C1290.6338 (5)0.7759 (6)0.6434 (3)0.0680 (13)
H1290.58320.86310.62200.093 (3)*
C2100.6841 (4)1.1042 (4)0.6894 (2)0.0456 (8)
H210A0.65091.18020.64410.093 (3)*
H210B0.65961.03750.68010.093 (3)*
C2110.6086 (4)1.1391 (4)0.7683 (2)0.0474 (9)
C2120.4584 (5)1.1717 (7)0.7597 (3)0.0750 (15)
H212A0.44611.09720.75360.093 (3)*
H212B0.42601.24260.71240.093 (3)*
H212C0.40971.19540.80760.093 (3)*
C2130.6257 (5)1.2592 (5)0.7779 (3)0.0626 (12)
H213A0.59481.32920.72990.093 (3)*
H213B0.71841.23980.78470.093 (3)*
H213C0.57451.28390.82500.093 (3)*
C2140.6568 (4)1.0241 (4)0.8438 (3)0.0510 (9)
C2150.6991 (7)0.8980 (6)0.8386 (4)0.0809 (17)
H2150.70180.88140.78810.093 (3)*
C2160.7379 (9)0.7947 (7)0.9084 (5)0.115 (3)
H2160.76840.70980.90400.093 (3)*
C2170.7309 (9)0.8186 (10)0.9830 (5)0.124 (3)
H2170.75340.74991.02970.093 (3)*
C2180.6923 (10)0.9392 (9)0.9890 (4)0.120 (3)
H2180.68980.95491.03970.093 (3)*
C2190.6554 (7)1.0424 (7)0.9197 (3)0.0845 (18)
H2190.62901.12640.92500.093 (3)*
C2201.0341 (4)0.9157 (4)0.7812 (2)0.0512 (9)
H220A0.98410.87440.82350.093 (3)*
H220B1.10220.84750.75980.093 (3)*
C2211.1078 (4)0.9687 (5)0.8242 (2)0.0513 (10)
C2221.0077 (6)1.0730 (5)0.8635 (3)0.0765 (16)
H222A0.95161.03680.90270.093 (3)*
H222B0.95351.14330.82190.093 (3)*
H222C1.05501.10450.89040.093 (3)*
C2231.1962 (6)1.0253 (7)0.7624 (4)0.0871 (19)
H223A1.25900.95950.73780.093 (3)*
H223B1.24361.05680.78930.093 (3)*
H223C1.14211.09560.72080.093 (3)*
C2241.1910 (4)0.8556 (5)0.8928 (2)0.0538 (10)
C2251.1296 (5)0.7897 (6)0.9551 (3)0.0694 (14)
H2251.03740.81340.95530.093 (3)*
C2261.2025 (7)0.6880 (7)1.0180 (3)0.0905 (19)
H2261.15870.64511.05950.093 (3)*
C2271.3371 (7)0.6517 (7)1.0188 (4)0.091 (2)
H2271.38560.58341.06050.093 (3)*
C2281.4005 (6)0.7147 (7)0.9589 (4)0.091 (2)
H2281.49280.68990.95950.093 (3)*
C2291.3286 (5)0.8163 (6)0.8966 (3)0.0718 (14)
H2291.37370.85930.85610.093 (3)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn10.03413 (12)0.03008 (12)0.03403 (12)0.01365 (9)0.00007 (9)0.01091 (9)
Sn20.03640 (13)0.04182 (14)0.03069 (12)0.01563 (10)0.00221 (9)0.01395 (9)
O10.0442 (13)0.0367 (12)0.0320 (11)0.0205 (10)0.0059 (10)0.0138 (9)
O20.0587 (16)0.0450 (14)0.0352 (12)0.0269 (12)0.0035 (11)0.0115 (10)
O30.0604 (18)0.0539 (17)0.0576 (17)0.0292 (14)0.0028 (14)0.0191 (14)
C1100.057 (2)0.044 (2)0.049 (2)0.0029 (18)0.0052 (18)0.0215 (17)
C1110.0381 (19)0.0386 (19)0.057 (2)0.0037 (16)0.0035 (16)0.0102 (17)
C1120.048 (3)0.063 (3)0.119 (5)0.021 (2)0.014 (3)0.012 (3)
C1130.059 (3)0.064 (3)0.087 (4)0.010 (2)0.000 (3)0.020 (3)
C1140.057 (2)0.041 (2)0.057 (2)0.0021 (18)0.012 (2)0.0079 (18)
C1150.098 (5)0.091 (5)0.090 (4)0.043 (4)0.002 (4)0.015 (4)
C1160.159 (10)0.150 (9)0.114 (7)0.060 (8)0.018 (7)0.050 (7)
C1170.239 (17)0.109 (8)0.076 (5)0.016 (9)0.030 (8)0.028 (5)
C1180.234 (15)0.095 (6)0.075 (5)0.021 (7)0.066 (7)0.024 (5)
C1190.133 (6)0.069 (4)0.076 (4)0.002 (4)0.049 (4)0.019 (3)
C1200.0386 (18)0.0370 (17)0.0461 (19)0.0162 (15)0.0049 (14)0.0087 (14)
C1210.0434 (19)0.0400 (18)0.0477 (19)0.0212 (16)0.0007 (15)0.0153 (15)
C1220.070 (3)0.067 (3)0.083 (3)0.040 (2)0.021 (2)0.048 (3)
C1230.062 (3)0.069 (3)0.070 (3)0.039 (2)0.015 (2)0.015 (2)
C1240.047 (2)0.046 (2)0.055 (2)0.0300 (18)0.0005 (17)0.0133 (17)
C1250.109 (5)0.045 (3)0.087 (4)0.038 (3)0.016 (3)0.000 (2)
C1260.239 (13)0.094 (6)0.099 (6)0.103 (8)0.049 (7)0.037 (5)
C1270.215 (12)0.164 (10)0.071 (4)0.147 (10)0.004 (6)0.013 (5)
C1280.119 (6)0.177 (8)0.074 (4)0.106 (6)0.038 (4)0.054 (5)
C1290.064 (3)0.091 (4)0.063 (3)0.042 (3)0.014 (2)0.030 (3)
C2100.0390 (19)0.060 (2)0.0410 (18)0.0204 (17)0.0020 (15)0.0162 (17)
C2110.0381 (19)0.060 (2)0.045 (2)0.0180 (17)0.0034 (15)0.0173 (17)
C2120.038 (2)0.113 (5)0.071 (3)0.023 (3)0.006 (2)0.031 (3)
C2130.059 (3)0.056 (3)0.067 (3)0.012 (2)0.004 (2)0.025 (2)
C2140.042 (2)0.061 (2)0.051 (2)0.0236 (19)0.0055 (17)0.0139 (19)
C2150.103 (5)0.068 (3)0.072 (3)0.042 (3)0.027 (3)0.017 (3)
C2160.120 (6)0.068 (4)0.128 (7)0.035 (4)0.026 (5)0.002 (4)
C2170.128 (7)0.128 (7)0.085 (5)0.058 (6)0.010 (5)0.035 (5)
C2180.183 (9)0.132 (7)0.057 (3)0.083 (7)0.023 (4)0.003 (4)
C2190.115 (5)0.095 (4)0.051 (3)0.049 (4)0.004 (3)0.015 (3)
C2200.056 (2)0.056 (2)0.0403 (19)0.0179 (19)0.0104 (17)0.0095 (17)
C2210.046 (2)0.068 (3)0.0433 (19)0.019 (2)0.0057 (16)0.0198 (19)
C2220.084 (4)0.073 (3)0.070 (3)0.008 (3)0.023 (3)0.036 (3)
C2230.066 (3)0.123 (5)0.075 (3)0.054 (4)0.017 (3)0.006 (3)
C2240.048 (2)0.072 (3)0.041 (2)0.016 (2)0.0050 (17)0.023 (2)
C2250.056 (3)0.091 (4)0.048 (2)0.018 (3)0.003 (2)0.012 (2)
C2260.102 (5)0.100 (5)0.051 (3)0.026 (4)0.012 (3)0.004 (3)
C2270.090 (4)0.087 (4)0.068 (3)0.004 (3)0.032 (3)0.019 (3)
C2280.060 (3)0.108 (5)0.090 (4)0.008 (3)0.025 (3)0.025 (4)
C2290.051 (3)0.095 (4)0.063 (3)0.015 (3)0.010 (2)0.024 (3)
Geometric parameters (Å, º) top
Sn1—O12.049 (2)C124—C1291.385 (7)
Sn1—O22.110 (2)C125—C1261.357 (10)
Sn1—C1102.151 (4)C126—C1271.328 (14)
Sn1—C1202.155 (4)C127—C1281.391 (13)
Sn1—O1i2.168 (2)C128—C1291.396 (8)
Sn2—O12.029 (2)C210—C2111.549 (5)
Sn2—O32.043 (3)C211—C2131.531 (6)
Sn2—C2202.149 (4)C211—C2141.536 (6)
Sn2—C2102.151 (4)C211—C2121.545 (6)
Sn2—O22.325 (3)C214—C2191.370 (7)
O1—Sn1i2.168 (2)C214—C2151.375 (7)
C110—C1111.530 (6)C215—C2161.397 (9)
C111—C1141.519 (6)C216—C2171.366 (12)
C111—C1121.525 (7)C217—C2181.324 (12)
C111—C1131.546 (6)C218—C2191.390 (9)
C114—C1151.358 (8)C220—C2211.539 (6)
C114—C1191.378 (8)C221—C2231.510 (7)
C115—C1161.393 (10)C221—C2221.527 (6)
C116—C1171.312 (18)C221—C2241.545 (6)
C117—C1181.363 (18)C224—C2251.376 (7)
C118—C1191.360 (12)C224—C2291.388 (7)
C120—C1211.543 (5)C225—C2261.395 (8)
C121—C1241.523 (5)C226—C2271.356 (10)
C121—C1231.536 (6)C227—C2281.350 (10)
C121—C1221.537 (5)C228—C2291.384 (8)
C124—C1251.383 (7)
O1—Sn1—O274.57 (10)C123—C121—C122106.6 (4)
O1—Sn1—C110123.75 (15)C124—C121—C120111.6 (3)
O2—Sn1—C110102.28 (14)C123—C121—C120107.8 (3)
O1—Sn1—C120112.75 (12)C122—C121—C120109.0 (3)
O2—Sn1—C12097.29 (13)C125—C124—C129118.0 (5)
C110—Sn1—C120123.19 (16)C125—C124—C121122.8 (4)
O1—Sn1—O1i73.19 (9)C129—C124—C121119.2 (4)
O2—Sn1—O1i147.75 (9)C126—C125—C124121.0 (8)
C110—Sn1—O1i94.94 (14)C127—C126—C125122.2 (9)
C120—Sn1—O1i95.71 (12)C126—C127—C128119.1 (7)
O1—Sn2—O388.71 (11)C127—C128—C129119.9 (7)
O1—Sn2—C220117.14 (14)C124—C129—C128119.8 (6)
O3—Sn2—C220104.28 (15)C211—C210—Sn2118.6 (3)
O1—Sn2—C210109.07 (12)C213—C211—C214111.5 (4)
O3—Sn2—C21099.93 (15)C213—C211—C212108.5 (4)
C220—Sn2—C210127.61 (16)C214—C211—C212107.8 (4)
O1—Sn2—O270.34 (9)C213—C211—C210109.5 (3)
O3—Sn2—O2159.00 (10)C214—C211—C210111.2 (3)
C220—Sn2—O284.83 (14)C212—C211—C210108.3 (4)
C210—Sn2—O288.70 (14)C219—C214—C215116.9 (5)
Sn2—O1—Sn1114.13 (11)C219—C214—C211121.6 (5)
Sn2—O1—Sn1i139.02 (12)C215—C214—C211121.5 (4)
Sn1—O1—Sn1i106.81 (9)C214—C215—C216120.7 (6)
Sn1—O2—Sn2100.87 (10)C217—C216—C215119.9 (8)
C111—C110—Sn1121.9 (3)C218—C217—C216120.2 (7)
C114—C111—C112111.9 (4)C217—C218—C219120.1 (7)
C114—C111—C110114.0 (4)C214—C219—C218122.1 (7)
C112—C111—C110107.5 (4)C221—C220—Sn2122.4 (3)
C114—C111—C113107.9 (4)C223—C221—C222109.6 (5)
C112—C111—C113107.8 (4)C223—C221—C220109.3 (4)
C110—C111—C113107.5 (4)C222—C221—C220110.4 (4)
C115—C114—C119116.5 (6)C223—C221—C224111.2 (4)
C115—C114—C111123.0 (5)C222—C221—C224108.2 (4)
C119—C114—C111120.5 (6)C220—C221—C224108.1 (4)
C114—C115—C116120.0 (9)C225—C224—C229116.4 (5)
C117—C116—C115121.1 (12)C225—C224—C221120.5 (4)
C116—C117—C118121.3 (10)C229—C224—C221123.1 (5)
C119—C118—C117117.2 (11)C224—C225—C226121.5 (5)
C118—C119—C114123.8 (10)C227—C226—C225120.1 (6)
C121—C120—Sn1120.2 (2)C228—C227—C226119.9 (6)
C124—C121—C123108.9 (3)C227—C228—C229120.2 (6)
C124—C121—C122112.7 (4)C228—C229—C224121.8 (6)
Symmetry code: (i) x+2, y+2, z+1.

Experimental details

Crystal data
Chemical formula[Sn4O2(OH)4(C10H13)8]
Mr1640.42
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)10.878 (2), 11.598 (3), 17.077 (2)
α, β, γ (°)73.19 (2), 81.944 (19), 66.91 (2)
V3)1896.4 (7)
Z1
Radiation typeMo Kα
µ (mm1)1.35
Crystal size (mm)0.43 × 0.29 × 0.25
Data collection
DiffractometerSiemens P4
diffractometer
Absorption correctionψ-scan
SHELXTL (Sheldrick, 1997b)
Tmin, Tmax0.652, 0.713
No. of measured, independent and
observed [I > 2σ(I)] reflections
7739, 6615, 5394
Rint0.033
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.028, 0.072, 1.03
No. of reflections6615
No. of parameters408
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.62, 0.51

Computer programs: XSCANS (Siemens, 1996), XSCANS, SHELXTL (Sheldrick, 1997b), SHELXS97 (Sheldrick, 1997a), SHELXL97 (Sheldrick, 1997a), SHELXTL.

Selected geometric parameters (Å, º) top
Sn1—O12.049 (2)Sn2—O12.029 (2)
Sn1—O22.110 (2)Sn2—O32.043 (3)
Sn1—C1102.151 (4)Sn2—C2202.149 (4)
Sn1—C1202.155 (4)Sn2—C2102.151 (4)
Sn1—O1i2.168 (2)Sn2—O22.325 (3)
O1—Sn1—O274.57 (10)O3—Sn2—C220104.28 (15)
O1—Sn1—C110123.75 (15)O1—Sn2—C210109.07 (12)
O2—Sn1—C110102.28 (14)O3—Sn2—C21099.93 (15)
O1—Sn1—C120112.75 (12)C220—Sn2—C210127.61 (16)
O2—Sn1—C12097.29 (13)O1—Sn2—O270.34 (9)
C110—Sn1—C120123.19 (16)O3—Sn2—O2159.00 (10)
O1—Sn1—O1i73.19 (9)C220—Sn2—O284.83 (14)
O2—Sn1—O1i147.75 (9)C210—Sn2—O288.70 (14)
C110—Sn1—O1i94.94 (14)Sn2—O1—Sn1114.13 (11)
C120—Sn1—O1i95.71 (12)Sn2—O1—Sn1i139.02 (12)
O1—Sn2—O388.71 (11)Sn1—O1—Sn1i106.81 (9)
O1—Sn2—C220117.14 (14)Sn1—O2—Sn2100.87 (10)
Symmetry code: (i) x+2, y+2, z+1.
 

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