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Volume 64 
Part 3 
Page i17  
March 2008  

Received 22 November 2007
Accepted 29 January 2008
Online 6 February 2008


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© International Union of Crystallography 2008

Key indicators
Single-crystal X-ray study
T = 298 K
Mean [sigma](Ge-O) = 0.013 Å
R = 0.058
wR = 0.133
Data-to-parameter ratio = 10.3
Details

A quaternary germanium(II) phosphate, Na[Ge4(PO4)3]

Chi-Shen Leea* and Sheng-Feng Wenga

aDepartment of Applied Chemistry and Institute of Molecular Science, National Chiao Tung University, 1001 Ta-Hsueh Rd, Hsinchu 30010, Taiwan
Correspondence e-mail: chishen@mail.nctu.edu.tw

A new germanium(II) phosphate, sodium tetragermanium tris(phosphate), Na[Ge4(PO4)3], has been synthesized by a solid-state reaction. The compound is isotypic with A[Sn4(PO4)3] (A = Na, K, NH4). It features a [Ge4(PO4)3]- framework made up of GeO3 pyramids and PO4 tetrahedra, which are linked by shared corners, yielding a three-dimensional structure. The crystal studied showed partial inversion twinning.

Related literature

Open-framework series of isotypic tin(II) phosphates with general formula A[Sn4(PO4)3] (A = Na, K, NH4) were synthesized by hydrothermal methods (Ayyappan et al., 2000[Ayyappan, S., Chang, J. S., Stock, N., Hatfield, R., Rao, C. N. R. & Cheetham, A. K. (2000). Int. J. Inorg. Mater. 2, 21-27.]; Bontchev & Moore, 2004[Bontchev, R. P. & Moore, R. C. (2004). Solid State Sci. 6, 867-873.]; Deng et al., 2004[Deng, J.-F., Kang, Y.-J., Mi, J.-X., Li, M.-R., Zhao, J.-T. & Mao, S.-Y. (2004). Acta Cryst. E60, i116-i117.]; Mao et al., 2004[Mao, S. Y., Deng, J. F., Li, M. R., Mi, J. X., Chen, H. H. & Zhao, J. T. (2004). Z. Kristallogr. 219, 205-206.]). For related literature, see: Brown & Altermatt (1985[Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.]); Cheetham et al. (1999[Cheetham, A. K., Férey, G. & Loiseau, T. (1999). Angew. Chem. Int. Ed. 38, 3268-3292.]); Weakley & Watt (1979[Weakley, T. J. R. & Watt, W. W. L. (1979). Acta Cryst. B35, 3023-3024.]).

Experimental

Crystal data

  • Na[Ge4(PO4)3]

  • Mr = 598.26

  • Trigonal, R 3c

  • a = 9.377 (8) Å

  • c = 23.48 (3) Å

  • V = 1788 (3) Å3

  • Z = 6

  • Mo K[alpha] radiation

  • [mu] = 10.49 mm-1

  • T = 298 (2) K

  • 0.2 × 0.13 × 0.1 mm
Data collection

  • Bruker SMART CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2000[Bruker (2000). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.488, Tmax = 1 (expected range = 0.171-0.350)

  • 2164 measured reflections

  • 639 independent reflections

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

  • Rint = 0.068
Refinement

  • R[F2 > 2[sigma](F2)] = 0.058

  • wR(F2) = 0.133

  • S = 1.09

  • 639 reflections

  • 62 parameters

  • 1 restraint

  • [Delta][rho]max = 1.71 e Å-3

  • [Delta][rho]min = -1.06 e Å-3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 146 Friedel pairs

  • Flack parameter: 0.23 (8)

Data collection: SMART (Bruker, 2000[Bruker (2000). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2000[Bruker (2000). SMART, 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: ATOMS (Dowty, 2005[Dowty, E. (2005). ATOMS. Shape Software, Kingsport, TN, USA.]); 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: FI2055 ).

Acknowledgements

This work was supported by the National Science Council (NSC94-2113-M-009-012, 94-2120-M-009-014) and the Institute of Nuclear Energy Research, Atomic Energy Council, Taiwan (NL940251).

References

Ayyappan, S., Chang, J. S., Stock, N., Hatfield, R., Rao, C. N. R. & Cheetham, A. K. (2000). Int. J. Inorg. Mater. 2, 21-27.  [CrossRef] [ChemPort]
Bontchev, R. P. & Moore, R. C. (2004). Solid State Sci. 6, 867-873.  [CrossRef] [ChemPort]
Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.  [CrossRef] [details]
Bruker (2000). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Cheetham, A. K., Férey, G. & Loiseau, T. (1999). Angew. Chem. Int. Ed. 38, 3268-3292.  [CrossRef] [ChemPort]
Deng, J.-F., Kang, Y.-J., Mi, J.-X., Li, M.-R., Zhao, J.-T. & Mao, S.-Y. (2004). Acta Cryst. E60, i116-i117.  [CrossRef] [details]
Dowty, E. (2005). ATOMS. Shape Software, Kingsport, TN, USA.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.  [CrossRef] [ChemPort] [details]
Mao, S. Y., Deng, J. F., Li, M. R., Mi, J. X., Chen, H. H. & Zhao, J. T. (2004). Z. Kristallogr. 219, 205-206.  [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Weakley, T. J. R. & Watt, W. W. L. (1979). Acta Cryst. B35, 3023-3024.  [CrossRef] [details]

Acta Cryst (2008). E64, i17  [ doi:10.1107/S1600536808003231 ]