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Volume 69 
Part 8 
Page i44  
August 2013  

Received 4 June 2013
Accepted 1 July 2013
Online 6 July 2013

Key indicators
Single-crystal X-ray study
T = 100 K
Mean [sigma](P-O) = 0.002 Å
R = 0.020
wR = 0.058
Data-to-parameter ratio = 23.5
Details
Open access

Calcium hexakis(dihydrogenphosphito)stannate(IV), Ca[Sn(H2PO2)6], with some remarks on the so-called Ge2(H2PO2)6 structure type

aInstitut für Chemie neuer Materialien, Strukturchemie, Universität Osnabrück, Barbarastr. 7, D-49069 Osnabrück, Germany
Correspondence e-mail: hreuter@uos.de

The title compound, Ca[Sn(H2PO2)6], was formed after a few days when tin(II) fluoride was allowed to react with phosphinic acid at ambient conditions. The structure consists of chains of Ca2+ and Sn4+ cations in octahedral sites with -3 symmetry bridged by bidentate hypophosphite anions. The chains are hexagonally close packed along [001]. The discovery of the compound and the successful structure refinement provides strong evidence that an isostructural compound, originally described as the mixed-valence compound, Ge2[H2PO2]6 [Weakley (1983[Weakley, T. J. R. (1983). J. Chem. Soc. Pak. 5, 279-281.]). J. Chem. Soc. Pak. 5, 279-281], must be reformulated as Ca[Ge(H2PO2)6].

Related literature

For the reaction of SnF2 with H3PO2, see: Everest (1951[Everest, D. A. (1951). J. Chem. Soc. pp. 2903-2905.]). For the structures of Ge2(H2PO2)6, see: Weakley (1983[Weakley, T. J. R. (1983). J. Chem. Soc. Pak. 5, 279-281.]), and Fe2(H2PO2)6, see: Kuratieva & Naumov (2006[Kuratieva, N. V. & Naumov, D. Yu. (2006). Acta Cryst. C62, i9-i10.]). For the so-called Ge2(H2PO2)6 structure type, see: Bergerhoff et al. (1999[Bergerhoff, G., Berndt, M., Brandenburg, K. & Degen, T. (1999). Acta Cryst. B55, 147-156.]); Villars et al. (2010[Villars, P., Cenzual, K., Daams, J., Gladyshevskii, R., Shcherban, O., Dubenskyy, V., Kuprysyuk, V. & Savysyuk, I. (2010). Ge2(H2PO2)6 in The Landolt-Bornstein Database, edited by P. Villars & K. Cenzual. Heidelberg: Springer-Verlag Berlin.]). For Ca-O bond lengths, see: Smith & Leider (1968[Smith, D. K. & Leider, H. R. (1968). J. Appl. Cryst. 1, 246-249.]) and for Sn-O bond lengths, see: Yamanaka et al. (2000[Yamanaka, T., Kurashima, R. & Mimaki, J. (2000). Z. Kristallogr. 215, 424-428.]). Bond-valence sums were calculated using Valist (Wills, 2010[Wills, A. S. (2010). VaList. Program available from www.CCP14.ac.uk.])

Experimental

Crystal data
  • Ca[Sn(H2PO2)6]

  • Mr = 548.69

  • Hexagonal, [R \overline 3]

  • a = 11.8619 (4) Å

  • c = 9.8668 (4) Å

  • V = 1202.31 (8) Å3

  • Z = 3

  • Mo K[alpha] radiation

  • [mu] = 2.56 mm-1

  • T = 100 K

  • 0.36 × 0.11 × 0.05 mm

Data collection
  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2009[Bruker (2009). APEX2, SADABS and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.459, Tmax = 0.887

  • 18525 measured reflections

  • 777 independent reflections

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

  • Rint = 0.054

Refinement
  • R[F2 > 2[sigma](F2)] = 0.020

  • wR(F2) = 0.058

  • S = 1.21

  • 777 reflections

  • 33 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 1.02 e Å-3

  • [Delta][rho]min = -0.42 e Å-3

Table 1
Selected bond lengths (Å)

Sn1-O1 2.0266 (15)
Ca1-O2 2.3303 (19)
P1-O2 1.4768 (18)
P1-O1 1.5397 (16)

Data collection: APEX2 (Bruker, 2009[Bruker (2009). APEX2, SADABS and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2009[Bruker (2009). APEX2, SADABS and SAINT. 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: CQ2005 ).


Acknowledgements

We thanks the Deutsche Forschungsgemeinschaft and the Government of Lower Saxony for funding the diffractometer.

References

Bergerhoff, G., Berndt, M., Brandenburg, K. & Degen, T. (1999). Acta Cryst. B55, 147-156.  [CrossRef] [IUCr Journals]
Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Bruker (2009). APEX2, SADABS and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Everest, D. A. (1951). J. Chem. Soc. pp. 2903-2905.  [CrossRef]
Kuratieva, N. V. & Naumov, D. Yu. (2006). Acta Cryst. C62, i9-i10.  [CrossRef] [IUCr Journals]
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.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]
Smith, D. K. & Leider, H. R. (1968). J. Appl. Cryst. 1, 246-249.  [CrossRef] [ChemPort] [IUCr Journals] [Web of Science]
Villars, P., Cenzual, K., Daams, J., Gladyshevskii, R., Shcherban, O., Dubenskyy, V., Kuprysyuk, V. & Savysyuk, I. (2010). Ge2(H2PO2)6 in The Landolt-Bornstein Database, edited by P. Villars & K. Cenzual. Heidelberg: Springer-Verlag Berlin.
Weakley, T. J. R. (1983). J. Chem. Soc. Pak. 5, 279-281.  [ChemPort]
Wills, A. S. (2010). VaList. Program available from www.CCP14.ac.uk.
Yamanaka, T., Kurashima, R. & Mimaki, J. (2000). Z. Kristallogr. 215, 424-428.  [CrossRef] [ChemPort]


Acta Cryst (2013). E69, i44  [ doi:10.1107/S1600536813018205 ]

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