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Volume 69 
Part 2 
Page i10  
February 2013  

Received 21 December 2012
Accepted 14 January 2013
Online 19 January 2013

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Key indicators
Single-crystal X-ray study
T = 100 K
Mean [sigma](Sn-Cl) = 0.0004 Å
R = 0.013
wR = 0.028
Data-to-parameter ratio = 30.4
Details
Open access

Redetermination of dipotassium trichloridostannate(II) chloride monohydrate

Fei Yea and Hans Reutera*

aInstitut für Chemie neuer Materialien, Anorganische Chemie II, Universität Osnabrück, Barbarastrasse 7, 49069 Osnabrück, Germany
Correspondence e-mail: hreuter@uos.de

The title compound, K2[SnCl3]Cl·H2O, is the prototype of some isostructural compounds of composition M2[SnX3]X·H2O (M = large monovalent cation; X = halogen). In comparison with a previous study based on photographic data [Kamenar & Grdenic (1962[Kamenar, B. & Grdenic, D. (1962). J. Inorg. Nucl. Chem. 24, 1039-1045.]). J. Inorg. Nucl. Chem. 24, 1039-1045], its crystal structure has now been redetermined using CCD-based data in order to gain more accurate values for bond lengths and angles within the [SnCl3]- anion and to locate the H atoms. The [SnCl3]- anion has a trigonal-pyramidal shape and exhibits crystallographic mirror symmetry. With the exception of the K+ ion which is located on a general position, all other atoms are situated on crystallographic mirror planes. The coordination polyhedron of the cation may be described by means of nine atoms in the form of a monocapped square antiprism with seven typical K-Cl/O distances and two additional atoms at considerably longer distances. The positions of the H atoms of the water molecule (also lying on a crystallographic mirror plane) could be determined and confirm the existence of a bifurcated O-H...Cl hydrogen bond to neighbouring Cl atoms.

Related literature

For a previous crystallographic investigation of the title compound, see: Kamenar & Grdenic (1962[Kamenar, B. & Grdenic, D. (1962). J. Inorg. Nucl. Chem. 24, 1039-1045.]). For IR-spectra of the title compound, see: Falk et al. (1974[Falk, M., Huang, C.-H. & Knop, O. (1974). Can. J. Chem. 52, 2380-2388.]).

Experimental

Crystal data

  • K2[SnCl3]Cl·H2O

  • Mr = 356.71

  • Orthorhombic, P n m a

  • a = 11.9233 (9) Å

  • b = 9.0768 (7) Å

  • c = 8.1737 (6) Å

  • V = 884.60 (12) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 4.95 mm-1

  • T = 100 K

  • 0.24 × 0.06 × 0.04 mm
Data collection

  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2009[Bruker (2009). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.388, Tmax = 0.823

  • 27095 measured reflections

  • 1367 independent reflections

  • 1265 reflections with I > 2[sigma](I)

  • Rint = 0.052
Refinement

  • R[F2 > 2[sigma](F2)] = 0.013

  • wR(F2) = 0.028

  • S = 1.12

  • 1367 reflections

  • 45 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 0.34 e Å-3

  • [Delta][rho]min = -0.48 e Å-3

Table 1
Selected geometric parameters (Å, °)

Sn1-Cl2 2.5745 (3)
Sn1-Cl2i 2.5745 (3)
Sn1-Cl1 2.6034 (5)
Cl2-Sn1-Cl2i 87.945 (16)
Cl2-Sn1-Cl1 87.376 (11)
Cl2i-Sn1-Cl1 87.376 (11)
Symmetry code: (i) [x, -y+{\script{3\over 2}}, z].

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O1-H1...Cl3ii 0.96 2.34 3.2920 (16) 174
O1-H2...Cl2iii 0.96 2.61 3.3687 (12) 137
O1-H2...Cl2iv 0.96 2.61 3.3687 (12) 137
Symmetry codes: (ii) [x+{\script{1\over 2}}, -y+{\script{1\over 2}}, -z+{\script{1\over 2}}]; (iii) -x+2, -y+1, -z+1; (iv) [-x+2, y-{\script{1\over 2}}, -z+1].

Data collection: APEX2 (Bruker, 2009[Bruker (2009). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2009[Bruker (2009). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: DIAMOND (Brandenburg, 2006[Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.]) and Mercury (Macrae et al., 2008[Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P., Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood, P. A. (2008). J. Appl. Cryst. 41, 466-470.]); software used to prepare material for publication: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2717 ).

References

Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Bruker (2009). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Falk, M., Huang, C.-H. & Knop, O. (1974). Can. J. Chem. 52, 2380-2388.  [CrossRef] [ChemPort] [ISI]
Kamenar, B. & Grdenic, D. (1962). J. Inorg. Nucl. Chem. 24, 1039-1045.  [CrossRef] [ChemPort] [ISI]
Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P., Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood, P. A. (2008). J. Appl. Cryst. 41, 466-470.  [ISI] [CrossRef] [ChemPort] [details]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]

Acta Cryst (2013). E69, i10  [ doi:10.1107/S1600536813001372 ]

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