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Acta Crystallogr Sect E Struct Rep Online. 2008 November 1; 64(Pt 11): m1430.
Published online 2008 October 18. doi:  10.1107/S1600536808032832
PMCID: PMC2959587

Di-μ-hydroxido-bis­[aqua­trichlorido­tin(IV)] diethyl ether disolvate

Abstract

The title compound, [Sn2Cl6(OH)2(H2O)2]·2C4H10O, consists of a centrosymmetric molecule and two additional solvent molecules and has an infinite two-dimensional network extending parallel to (101). The Sn atom is six-coordinate with a distorted octa­hedral geometry. Additional O—H(...)O hydrogen bonding leads to stabilization of the crystal structure.

Related literature

For a related structure, see: Janas et al. (1991 [triangle])

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Object name is e-64-m1430-scheme1.jpg

Experimental

Crystal data

  • [Sn2Cl6(OH)2(H2O)2]·2C4H10O
  • M r = 668.36
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-m1430-efi1.jpg
  • a = 10.1171 (15) Å
  • b = 10.0212 (15) Å
  • c = 11.2641 (18) Å
  • β = 103.536 (1)°
  • V = 1110.3 (3) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 2.99 mm−1
  • T = 298 (2) K
  • 0.46 × 0.32 × 0.30 mm

Data collection

  • Siemens SMART CCD area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996 [triangle]) T min = 0.340, T max = 0.468 (expected range = 0.297–0.408)
  • 5168 measured reflections
  • 1909 independent reflections
  • 1685 reflections with I > 2σ(I)
  • R int = 0.027

Refinement

  • R[F 2 > 2σ(F 2)] = 0.023
  • wR(F 2) = 0.063
  • S = 0.84
  • 1909 reflections
  • 102 parameters
  • H-atom parameters constrained
  • Δρmax = 1.05 e Å−3
  • Δρmin = −0.68 e Å−3

Data collection: SMART (Siemens, 1996 [triangle]); cell refinement: SAINT (Siemens, 1996 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL.

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808032832/sg2266sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808032832/sg2266Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

We thank the National Natural Science Foundation of China (grant No. 20771053) for financial support.

supplementary crystallographic information

Comment

We have synthesized the title compound unexpectedly, (I), and present its crystal structure here. The title compound consist of a centrosymmetric dimer (Fig. 1) in which the tin atoms have a distorted octahedral arrangement formed by three chlorine atoms, two hydroxy oxygen bridges and one water molecule. A further two water molecules are hydrogen-bonded to the hydroxyl oxygen atoms of the µ-OH bridges. The Sn—O distances in (I) (Table 1), are similar to those in related organotin carboxylates. The Sn—Cl bond lengths and the interbond angles lie within the ranges observed for other related complexes. The Sn1—O1 (2.072 (2) Å) and Sn1—O2 distance (2.183 (2) Å), (Table 1), are close to those reported for organotin carboxylates (Janas et al., 1991).

Experimental

The reaction was carried out under nitrogen atmosphere. 3-Thiophenemalonic acid (1 mmol) and sodium ethoxide (2.2 mmol) were added to the solution of benzene (30 ml) in a Schlenk flask and stirred for 0.5 h. Phenyltin trichloride (1 mmol) was then added to the reactor and the mixture was stirred for 12 h at 338 K.The resulting clear solution was evaporated under vacuum. The product was crystallized from a mixture of diethylether/petroleum ether (1:1).Unexpectedly,a dimeric complex, was isolated from the filtrate. (yield 52%; m.p. 446 K). Analysis calculated (%) for C4H13Cl3O3Sn (Mr = 334.18): C,46.72; H, 4.49; O, 9.57. found: C, 46.52; H, 4.55; O, 9.62.

Refinement

H atoms were positioned geometrically, with O—H = 0.85 and 0.93 Å and C—H = 0.96 and 0.97 Å for aromatic, methyl and methylene H atoms, respectively, and constrained to ride on their parent atoms, with Uiso(H) = xUeq(C,O) where x = 1.5 for methyl H and x = 1.2 for all other H atoms.

Figures

Fig. 1.
The molecular structure of (I), showing 50% probability displacement ellipsoids and the atom-numbering scheme. H atoms have been omitted for clarity.
Fig. 2.
The infinite two-dimensional network structure of (I), H atoms have been omitted for clarity.

Crystal data

[Sn2Cl6(OH)2(H2O)2]·2C4H10OF(000) = 648
Mr = 668.36Dx = 1.999 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 10.1171 (15) ÅCell parameters from 4261 reflections
b = 10.0212 (15) Åθ = 2.4–28.2°
c = 11.2641 (18) ŵ = 2.99 mm1
β = 103.536 (1)°T = 298 K
V = 1110.3 (3) Å3Block, colorless
Z = 20.46 × 0.32 × 0.30 mm

Data collection

Siemens SMART CCD area-detector diffractometer1909 independent reflections
Radiation source: fine-focus sealed tube1685 reflections with I > 2σ(I)
graphiteRint = 0.027
[var phi] and ω scansθmax = 25.0°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −11→12
Tmin = 0.340, Tmax = 0.468k = −11→11
5168 measured reflectionsl = −7→13

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.023Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.063H-atom parameters constrained
S = 0.84w = 1/[σ2(Fo2) + (0.0489P)2 + 0.9726P] where P = (Fo2 + 2Fc2)/3
1909 reflections(Δ/σ)max = 0.001
102 parametersΔρmax = 1.05 e Å3
0 restraintsΔρmin = −0.68 e Å3

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 (Å2)

xyzUiso*/Ueq
Sn10.53184 (2)0.46950 (2)0.361848 (19)0.02338 (10)
Cl10.66543 (10)0.58991 (10)0.25532 (9)0.0421 (2)
Cl20.70089 (10)0.30829 (10)0.44565 (9)0.0434 (2)
Cl30.41097 (10)0.33403 (10)0.20324 (9)0.0470 (2)
O10.4121 (2)0.4148 (2)0.48000 (19)0.0261 (5)
H10.34470.34970.46510.031*
O20.3762 (3)0.6222 (3)0.3036 (2)0.0402 (6)
H2D0.35430.66360.23600.048*
H2E0.34250.66440.35490.048*
O30.8141 (2)0.7541 (2)0.5809 (2)0.0367 (6)
C10.7894 (5)0.8615 (4)0.4926 (4)0.0518 (11)
H1A0.77980.82600.41090.062*
H1B0.86530.92330.50910.062*
C20.6621 (6)0.9321 (5)0.5016 (5)0.0660 (14)
H2A0.58840.86940.48950.099*
H2B0.64151.00030.44020.099*
H2C0.67460.97200.58100.099*
C30.9279 (4)0.6715 (5)0.5690 (4)0.0537 (12)
H3A1.00750.72670.57300.064*
H3B0.90660.62630.49070.064*
C40.9561 (5)0.5717 (6)0.6692 (5)0.0720 (15)
H4A0.97150.61680.74640.108*
H4B1.03550.52100.66500.108*
H4C0.87970.51280.66100.108*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Sn10.02419 (15)0.02519 (15)0.02104 (15)0.00006 (8)0.00583 (10)−0.00080 (8)
Cl10.0446 (5)0.0476 (5)0.0398 (5)−0.0069 (4)0.0216 (4)0.0052 (4)
Cl20.0438 (5)0.0454 (5)0.0423 (5)0.0216 (4)0.0127 (4)0.0053 (4)
Cl30.0515 (6)0.0523 (6)0.0348 (5)−0.0129 (5)0.0053 (4)−0.0163 (4)
O10.0273 (12)0.0281 (12)0.0234 (12)−0.0074 (10)0.0069 (9)−0.0028 (9)
O20.0460 (15)0.0483 (15)0.0274 (13)0.0203 (12)0.0108 (11)0.0104 (11)
O30.0334 (13)0.0435 (14)0.0355 (14)−0.0047 (11)0.0125 (11)−0.0029 (11)
C10.071 (3)0.047 (2)0.037 (2)−0.023 (2)0.013 (2)−0.0013 (19)
C20.076 (4)0.048 (2)0.063 (3)0.002 (2)−0.008 (3)0.011 (2)
C30.034 (2)0.074 (3)0.056 (3)−0.002 (2)0.015 (2)−0.025 (2)
C40.056 (3)0.064 (3)0.088 (4)0.020 (3)0.003 (3)−0.012 (3)

Geometric parameters (Å, °)

Sn1—O12.072 (2)C1—C21.493 (7)
Sn1—O1i2.090 (2)C1—H1A0.9700
Sn1—O22.183 (2)C1—H1B0.9700
Sn1—Cl12.3413 (9)C2—H2A0.9600
Sn1—Cl32.3469 (9)C2—H2B0.9600
Sn1—Cl22.3813 (9)C2—H2C0.9600
O1—Sn1i2.090 (2)C3—C41.485 (7)
O1—H10.9300C3—H3A0.9700
O2—H2D0.8500C3—H3B0.9700
O2—H2E0.8500C4—H4A0.9600
O3—C11.447 (5)C4—H4B0.9600
O3—C31.449 (5)C4—H4C0.9600
O1—Sn1—O1i71.48 (9)O3—C1—H1A110.0
O1—Sn1—O283.66 (9)C2—C1—H1A110.0
O1i—Sn1—O284.28 (9)O3—C1—H1B110.0
O1—Sn1—Cl1163.72 (7)C2—C1—H1B110.0
O1i—Sn1—Cl194.40 (6)H1A—C1—H1B108.4
O2—Sn1—Cl186.96 (7)C1—C2—H2A109.5
O1—Sn1—Cl393.27 (6)C1—C2—H2B109.5
O1i—Sn1—Cl3163.56 (6)H2A—C2—H2B109.5
O2—Sn1—Cl388.04 (8)C1—C2—H2C109.5
Cl1—Sn1—Cl399.69 (4)H2A—C2—H2C109.5
O1—Sn1—Cl292.27 (7)H2B—C2—H2C109.5
O1i—Sn1—Cl290.68 (7)O3—C3—C4109.3 (4)
O2—Sn1—Cl2174.32 (7)O3—C3—H3A109.8
Cl1—Sn1—Cl296.06 (4)C4—C3—H3A109.8
Cl3—Sn1—Cl296.16 (4)O3—C3—H3B109.8
Sn1—O1—Sn1i108.52 (9)C4—C3—H3B109.8
Sn1—O1—H1125.7H3A—C3—H3B108.3
Sn1i—O1—H1125.7C3—C4—H4A109.5
Sn1—O2—H2D129.1C3—C4—H4B109.5
Sn1—O2—H2E121.4H4A—C4—H4B109.5
H2D—O2—H2E107.7C3—C4—H4C109.5
C1—O3—C3112.0 (3)H4A—C4—H4C109.5
O3—C1—C2108.6 (3)H4B—C4—H4C109.5

Symmetry codes: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O1—H1···O3i0.931.882.799 (3)169.
O2—H2D···O3ii0.851.892.736 (3)176.
O2—H2E···Cl2i0.852.403.179 (3)152.

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x−1/2, −y+3/2, z−1/2.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SG2266).

References

  • Janas, Z., Sobota, P. & Lis, T. (1991). J. Chem. Soc. Dalton Trans. pp. 2429–2434.
  • Sheldrick, G. M. (1996). SADABS University of Göttingen, Germany.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Siemens (1996). SMART and SAINT Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.

Articles from Acta Crystallographica Section E: Structure Reports Online are provided here courtesy of International Union of Crystallography