[Journal logo]

Volume 69 
Part 6 
Page i34  
June 2013  

Received 1 March 2013
Accepted 7 May 2013
Online 11 May 2013

Key indicators
Powder Synchrotron study
T = 298 K
Mean [sigma](P-N) = 0.007 Å
R = 0.091
wR = 0.119
Data-to-parameter ratio = 8.2
Details
Open access

Synchrotron powder study of Na3V(PO3)3N

aDepartment of Chemistry, Division of Energy Systems Research, Ajou University, Suwon 443-749, Republic of Korea
Correspondence e-mail: sjookim@ajou.ac.kr

Polycrystalline trisodium vanadium(III) nitridotriphosphate, Na3V(PO3)3N, was prepared by thermal nitridation of a mixture of NaPO3 and V2O5. The title compound is isotypic with Na3Al(PO3)3N. In the crystal, the P-atom and the three O-atom sites are on general positions, whereas the Na-, V- and N-atom sites are located on threefold rotation axes. The P atom is coordinated by three O atoms and one N atom in form of a slightly distorted tetrahedron. Three PO3N tetrahedra build up a nitridotriphosphate group, (PO3)3N, by sharing a common N atom. The V atom is coordinated by six O atoms in form of a slightly distorted octahedron. The Na+ ions occupy three crystallographically distinct sites. One Na+ ion is situated in an irregular polyhedral coordination environment composed of six O atoms and one N atom, while the other two Na+ cations are surrounded by six and nine O atoms, respectively.

Related literature

For structure determination of the isotypic Na3Al(PO3)3N, see: Conanec et al. (1994[Conanec, R., L'Haridon, P., Feldmann, W., Marchand, R. & Laurent, Y. (1994). Eur. J. Solid State Inorg. Chem. 31, 13-24.]). For the preparation of various related materials, A3B(PO3)3N (A = Na, K; B = Al, Ga, Cr, Mn, Fe) and A2B2(PO3)3N (A = Na; B = Mg, Mn, Fe, Co), see: Conanec et al. (1996[Conanec, R., Feldmann, W., Marchand, R. & Laurent, Y. (1996). J. Solid State Chem. 121, 418-422.]); Feldmann (1987a[Feldmann, W. (1987a). Z. Chem. 27, 100-101.],b[Feldmann, W. (1987b). Z. Chem. 27, 182-183.]). For studies focused on the ionic conductivity of Na2Mg2(PO3)3N, see: Lee et al. (2012[Lee, M. S., Kang, J. K. & Kim, S. J. (2012). Bull. Korean Chem. Soc. 33, 2083-2086.]). For a review of structural features of metal nitridophosphate compounds, see: Marchand & Laurent (1991[Marchand, R. & Laurent, Y. (1991). Eur. J. Solid State Inorg. Chem. 28, 57-76.]); Marchand et al. (2000[Marchand, R., Schnick, W. & Stock, N. (2000). Adv. Inorg. Chem. 50, 193-233.]). For bond-valence-sum calculations, see: Brese & O'Keeffe (1991[Brese, N. E. & O'Keeffe, M. (1991). Acta Cryst. B47, 192-197.]). For comparison of bond lengths in related structures, see: Conanec et al. (1994[Conanec, R., L'Haridon, P., Feldmann, W., Marchand, R. & Laurent, Y. (1994). Eur. J. Solid State Inorg. Chem. 31, 13-24.]); Jacobs & Nymwegen (1997[Jacobs, H. & Nymwegen, R. Z. (1997). Z. Anorg. Allg. Chem. 623, 429-433.]); Lee et al. (2012[Lee, M. S., Kang, J. K. & Kim, S. J. (2012). Bull. Korean Chem. Soc. 33, 2083-2086.]); Shannon (1976[Shannon, R. D. (1976). Acta Cryst. A32, 751-767.]); Zatovsky (2010[Zatovsky, I. V. (2010). Acta Cryst. E66, i12.]).

Experimental

Crystal data
  • Na3V(PO3)3N

  • Mr = 370.83

  • Cubic, P 21 3

  • a = 9.44783 (5) Å

  • V = 843.33 (1) Å3

  • Z = 4

  • Synchrotron radiation, [lambda] = 1.547400 Å

  • T = 298 K

  • Flat sheet, 20 × 20 mm

Data collection
  • Pohang Light Source 9B HRPD Beamline diffractometer

  • Specimen mounting: packed powder pellet

  • Data collection mode: reflection

  • Scan method: step

  • 2[theta]min = 10.060°, 2[theta]max = 130.500°, 2[theta]step = 0.010°

Refinement
  • Rp = 0.091

  • Rwp = 0.119

  • Rexp = 0.075

  • RBragg = 0.056

  • [chi]2 = 2.519

  • 12045 data points

  • 288 parameters

Data collection: local software at 9B HRPD beamline; cell refinement: DICVOL (Boultif & Louër, 2004[Boultif, A. & Louër, D. (2004). J. Appl. Cryst. 37, 724-731.]); data reduction: local software at 9B HRPD beamline; method used to solve structure: coordinates taken from an isotypic compound; program(s) used to refine structure: FULLPROF (Rodriguez-Carvajal, 2001[Rodriguez-Carvajal, J. (2001). FULLPROF. http://www.ill.eu/sites/fullprof/]); molecular graphics: DIAMOND (Brandenburg, 1999[Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: FULLPROF.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2731 ).


Acknowledgements

This work was supported by the National Research Foundation of Korea (grant Nos. 2009-0094046 and 2010-0013089). The authors thank Dr Do-Cheon Ahn for his help in performing the sXRD experiment at the Pohang light source.

References

Boultif, A. & Louër, D. (2004). J. Appl. Cryst. 37, 724-731.  [ISI] [CrossRef] [ChemPort] [details]
Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Brese, N. E. & O'Keeffe, M. (1991). Acta Cryst. B47, 192-197.  [CrossRef] [ISI] [details]
Conanec, R., Feldmann, W., Marchand, R. & Laurent, Y. (1996). J. Solid State Chem. 121, 418-422.  [CrossRef] [ChemPort] [ISI]
Conanec, R., L'Haridon, P., Feldmann, W., Marchand, R. & Laurent, Y. (1994). Eur. J. Solid State Inorg. Chem. 31, 13-24.  [ChemPort]
Feldmann, W. (1987a). Z. Chem. 27, 100-101.  [CrossRef]
Feldmann, W. (1987b). Z. Chem. 27, 182-183.  [CrossRef] [ChemPort]
Jacobs, H. & Nymwegen, R. Z. (1997). Z. Anorg. Allg. Chem. 623, 429-433.  [CrossRef] [ChemPort]
Lee, M. S., Kang, J. K. & Kim, S. J. (2012). Bull. Korean Chem. Soc. 33, 2083-2086.  [ChemPort]
Marchand, R. & Laurent, Y. (1991). Eur. J. Solid State Inorg. Chem. 28, 57-76.  [ChemPort]
Marchand, R., Schnick, W. & Stock, N. (2000). Adv. Inorg. Chem. 50, 193-233.  [ISI] [CrossRef] [ChemPort]
Rodriguez-Carvajal, J. (2001). FULLPROF. http://www.ill.eu/sites/fullprof/
Shannon, R. D. (1976). Acta Cryst. A32, 751-767.  [CrossRef] [details]
Zatovsky, I. V. (2010). Acta Cryst. E66, i12.  [CrossRef] [details]


Acta Cryst (2013). E69, i34  [ doi:10.1107/S1600536813012427 ]

This is an open-access article distributed under the terms of the Creative Commons Attribution Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.