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Volume 68 
Part 12 
Page i88  
December 2012  

Received 14 August 2012
Accepted 24 October 2012
Online 3 November 2012

Key indicators
Single-crystal X-ray study
T = 298 K
Mean [sigma](Mo-O) = 0.005 Å
Disorder in main residue
R = 0.037
wR = 0.095
Data-to-parameter ratio = 12.7
Details
Open access

Li0.17Na5.83Mo11O36

aLaboratoire de Matériaux et Cristallochimie, Faculté des Sciences de Tunis, Université de Tunis ElManar, 2092 Manar II Tunis, Tunisia
Correspondence e-mail: faouzi.zid@fst.rnu.tn

The title mixed-alkali-metal molybdenium oxide, hexakis(lithium/sodium) undecamolybdate, was synthesized by solid-state reaction at 793 K. Its [Mo11O36]6- framework is built up from MoO6 octahedra and MoO5 pyramids linked together by edges and vertices. The framework delimits two types of intersecting tunnels running along [100] and [001], where the sodium and lithium ions are located. Two of the sodium ions and the lithium ion have fractional site occupancies. One of the Mo atoms has site symmetry 2, one sodium ion has site symmetry 2 and one has site symmetry -1, and the Li+ ion has site symmetry 2. Structural relationships between the title compound and the anatase and Na6Mo11O36 structures are discussed.

Related literature

For complex oxides containing lithium ions, see: Daidouh et al. (1997[Daidouh, A., Veiga, M. L. & Pico, C. (1997). J. Solid State Chem. 130, 28-34.]); Whittingham & Silbernagel (1976[Whittingham, M. S. & Silbernagel, B. G. (1976). Mater. Res. Bull. 11, 29-36.]); Mizushima et al. (1980[Mizushima, K., Jones, P. C., Wiseman, P. J. & Goodenough, J. B. (1980). Mater. Res. Bull. 15, 783-789.]); Kanno et al. (1994[Kanno, R., Kubo, H., Kawamoto, Y., Kamiyama, T., Izumi, F., Takeda, Y. & Takano, M. (1994). J. Solid State Chem. 110, 216-225.]); Guilmard et al. (2003[Guilmard, M., Croguennec, L. & Delmas, C. (2003). Chem. Mater. 15, 4484-4493.]); Lin et al. (2005[Lin, Y. K., Lu, C. H., Wu, H. C. & Yang, M. H. (2005). J. Power Sources, B146, 594-597.]); Yuh et al. (1995[Yuh, C., Johnsen, R., Farooque, M. & Maru, H. (1995). J. Power Sources, B56, 1-10.]); Koyama et al. (2004[Koyama, Y., Yabuuchi, N., Tanaka, I., Adachi, H. & Ohzuku, T. (2004). J. Electrochem. Soc. 151, A1545-A1551.]). For details of structurally related compounds, see: Bramnik & Ehrenberg (2004[Bramnik, K. G. & Ehrenberg, H. (2004). Z. Anorg. Allg. Chem. 630, 1336-1341.]); Caillet (1967[Caillet, P. (1967). Bull. Soc. Chem. Fr. pp. 4750-4757.]); Seleborg (1967[Seleborg, M. (1967). Acta Chem. Scand. 21, 499-504.]). For further synthetic details, see: Bramnik & Ehrenberg (2004[Bramnik, K. G. & Ehrenberg, H. (2004). Z. Anorg. Allg. Chem. 630, 1336-1341.]). For bond-valence sums, see: Brown & Altermatt (1985[Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.]). For related literature, see: Koyama et al. (2004[Koyama, Y., Yabuuchi, N., Tanaka, I., Adachi, H. & Ohzuku, T. (2004). J. Electrochem. Soc. 151, A1545-A1551.]).

Experimental

Crystal data
  • Li0.17Na5.83Mo11O36

  • Mr = 1766.55

  • Monoclinic, C 2/c

  • a = 7.2250 (9) Å

  • b = 17.863 (2) Å

  • c = 22.086 (3) Å

  • [beta] = 90.162 (8)°

  • V = 2850.5 (6) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 4.89 mm-1

  • T = 298 K

  • 0.30 × 0.24 × 0.14 mm

Data collection
  • Enraf-Nonius CAD-4 diffractometer

  • Absorption correction: [psi] scan (North et al., 1968[North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359.]) Tmin = 0.25, Tmax = 0.50

  • 6662 measured reflections

  • 3138 independent reflections

  • 3065 reflections with I > 2[sigma](I)

  • Rint = 0.032

  • 2 standard reflections every 120 min intensity decay: 2.3%

Refinement
  • R[F2 > 2[sigma](F2)] = 0.037

  • wR(F2) = 0.095

  • S = 1.33

  • 3138 reflections

  • 247 parameters

  • 1 restraint

  • [Delta][rho]max = 1.39 e Å-3

  • [Delta][rho]min = -1.85 e Å-3

Data collection: CAD-4 EXPRESS (Duisenberg, 1992[Duisenberg, A. J. M. (1992). J. Appl. Cryst. 25, 92-96.]; Macícek & Yordanov, 1992[Macícek, J. & Yordanov, A. (1992). J. Appl. Cryst. 25, 73-80.]); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995[Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marberg, Germany.]); 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, 1998[Brandenburg, K. (1998). DIAMOND. University of Bonn, Germany.]); software used to prepare material for publication: WinGX (Farrugia, 1999[Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HB6937 ).


References

Bramnik, K. G. & Ehrenberg, H. (2004). Z. Anorg. Allg. Chem. 630, 1336-1341.  [CrossRef] [ChemPort]
Brandenburg, K. (1998). DIAMOND. University of Bonn, Germany.
Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.  [CrossRef] [ISI] [details]
Caillet, P. (1967). Bull. Soc. Chem. Fr. pp. 4750-4757.
Daidouh, A., Veiga, M. L. & Pico, C. (1997). J. Solid State Chem. 130, 28-34.  [CrossRef] [ChemPort] [ISI]
Duisenberg, A. J. M. (1992). J. Appl. Cryst. 25, 92-96.  [CrossRef] [ChemPort] [ISI] [details]
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.  [CrossRef] [ChemPort] [details]
Guilmard, M., Croguennec, L. & Delmas, C. (2003). Chem. Mater. 15, 4484-4493.  [ISI] [CrossRef] [ChemPort]
Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marberg, Germany.
Kanno, R., Kubo, H., Kawamoto, Y., Kamiyama, T., Izumi, F., Takeda, Y. & Takano, M. (1994). J. Solid State Chem. 110, 216-225.  [CrossRef] [ChemPort] [ISI]
Koyama, Y., Yabuuchi, N., Tanaka, I., Adachi, H. & Ohzuku, T. (2004). J. Electrochem. Soc. 151, A1545-A1551.  [ISI] [CrossRef] [ChemPort]
Lin, Y. K., Lu, C. H., Wu, H. C. & Yang, M. H. (2005). J. Power Sources, B146, 594-597.  [ISI] [CrossRef]
Macícek, J. & Yordanov, A. (1992). J. Appl. Cryst. 25, 73-80.  [CrossRef] [ISI] [details]
Mizushima, K., Jones, P. C., Wiseman, P. J. & Goodenough, J. B. (1980). Mater. Res. Bull. 15, 783-789.  [CrossRef] [ChemPort] [ISI]
North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359.  [CrossRef] [details]
Seleborg, M. (1967). Acta Chem. Scand. 21, 499-504.  [CrossRef] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Whittingham, M. S. & Silbernagel, B. G. (1976). Mater. Res. Bull. 11, 29-36.
Yuh, C., Johnsen, R., Farooque, M. & Maru, H. (1995). J. Power Sources, B56, 1-10.  [CrossRef] [ISI]


Acta Cryst (2012). E68, i88  [ doi:10.1107/S1600536812044224 ]

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