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Volume 68 
Part 11 
Pages i80-i81  
November 2012  

Received 25 September 2012
Accepted 6 October 2012
Online 13 October 2012

Key indicators
Single-crystal X-ray study
T = 298 K
Mean [sigma](Mo-O) = 0.007 Å
R = 0.035
wR = 0.096
Data-to-parameter ratio = 12.9
Details
Open access

LiNa5Mo9O30

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 tite compound, lithium pentasodium nonamolybdate, LiNa5Mo9O30, was synthesized by solid-state reaction. The three-dimensional [Mo9O30]6- framework is built up from MoO6 octahedra and MoO5 bipyramids, linked together by edges and corners. The framework delimits two types of intersecting tunnels running along [100] and [010] in which the Na+ and Li+ ions are located. The asymmetric unit contains one Mo, one Na and one Li site located on a twofold rotation axis. The crystal studied was a racemic twin with site a twin ratio of 0.51 (10):0.49 (10). Relationships between the structures of K2Mo3O10, K2Mo4O13, Cs2Mo7O22, Na6Mo10O33 and Na6Mo11O36 compounds are discussed.

Related literature

For background to the physico-chemical properties of related compounds, see: Mizushima et al. (1980[Mizushima, K., Jones, P. C., Wiseman, P. J. & Goodenough, J. B. (1980). Mater. Res. Bull. 15, 783-789.]); Thackeray et al. (1984[Thackeray, M. M., Johnson, P. J., De Picciotto, L. A., Bruce, P. G. & Goodenough, J. B. (1984). Mater. Res. Bull. 19, 179-187.]); Dahn et al. (1991[Dahn, J. R., von Sacken, U., Juzkow, M. W. & Al-Janaby, H. (1991). J. Electrochem. Soc. 138, 2207-2211.]); Tarascon et al. (1991[Tarascon, J. M., Wang, E., Shokoohi, F. K., McKinnon, W. R. & Colson, S. (1991). J. Electrochem. Soc. 138, 2859-2864.]); 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.]); Yuh et al. (1995[Yuh, C., Johnsen, R., Farooque, M. & Maru, H. (1995). J. Power Sources, B56, 1-10.]); Broussely et al. (1995[Broussely, M., Perton, F., Biensan, P., Bodet, J. M., Labat, J., Lecerf, A., Delmas, C., Rougier, A. & Pérès, J. P. (1995). J. Power Sources, 54, 109-114.]); Capitaine et al. (1996[Capitaine, F., Graverau, P. & Delmas, C. (1996). Solid State Ionics, 89, 197-202.]); Delmas et al. (1999[Delmas, C., Ménétrier, M., Croguennec, L., Saadoune, I., Rougier, A., Pouillerie, C., Prado, G., Grüne, M. & Fournès, L. (1999). Electrochim. Acta, 45, 243-253.]); Bruce et al. (1999[Bruce, P. G., Armstrong, A. R. & Gitzendanner, R. L. (1999). J. Mater. Chem. 9, 193-198.]); Guilmard et al. (2003[Guilmard, M., Croguennec, L. & Delmas, C. (2003). Chem. Mater. 15, 4484-4493.]). For similar structure types, see: Caillet (1967[Caillet, P. (1967). Bull. Soc. Chim. Fr. pp. 4750-4757.]); Seleborg (1967[Seleborg, M. (1967). Acta Chem. Scand. 21, 499-504.]); Gatehouse et al. (1983[Gatehouse, B. M., Jenkins, C. E. & Miskin, B. K. (1983). J. Solid State Chem. 46, 269-274.]). For background to their electronic properties, see: Aranda et al. (1992[Aranda, M. A. G., Attfield, J. P., Bruque, S. & Martinez-Lara, M. (1992). Inorg. Chem. 31, 1045-1049.]); Nguyen & Sleight, (1996[Nguyen, P. T. & Sleight, A. W. (1996). J. Solid State Chem. 122, 259-265.]); Daidouh et al. (1997[Daidouh, A., Veiga, M. L. & Pico, C. (1997). J. Solid State Chem. 130, 28-34.]); Ouerfelli et al. (2007[Ouerfelli, N., Guesmi, A., Molinié, P., Mazza, D., Zid, M. F. & Driss, A. (2007). J. Solid State Chem. 180, 2942-2949.]). For details of structural relationships between these compounds, see: Gatehouse & Leverett (1968[Gatehouse, B. M. & Leverett, P. (1968). J. Chem. Soc. A, pp. 1293-1298.]); Gatehouse & Miskin (1975[Gatehouse, B. M. & Miskin, B. K. (1975). Acta Cryst. B31, 1293-1299.]); Eda et al. (2004[Eda, K., Chin, K., Sotani, N. & Witlingham, M. S. (2004). J. Solid State Chem. 177, 916-921.]). For the preparation, 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.]).

Experimental

Crystal data
  • LiMo9Na5O30

  • Mr = 1465.35

  • Orthorhombic, F d d 2

  • a = 7.1927 (8) Å

  • b = 37.159 (4) Å

  • c = 17.925 (2) Å

  • V = 4791.0 (9) Å3

  • Z = 8

  • Mo K[alpha] radiation

  • [mu] = 4.77 mm-1

  • T = 298 K

  • 0.30 × 0.20 × 0.10 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 = 0.31, Tmax = 0.61

  • 3006 measured reflections

  • 2605 independent reflections

  • 2579 reflections with I > 2[sigma](I)

  • Rint = 0.035

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

Refinement
  • R[F2 > 2[sigma](F2)] = 0.035

  • wR(F2) = 0.096

  • S = 1.13

  • 2605 reflections

  • 202 parameters

  • 1 restraint

  • [Delta][rho]max = 1.55 e Å-3

  • [Delta][rho]min = -1.65 e Å-3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 1259 Fridel pairs

  • Flack parameter: 0.51 (10)

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 Marburg, 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 publication routines (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: VN2054 ).


References

Aranda, M. A. G., Attfield, J. P., Bruque, S. & Martinez-Lara, M. (1992). Inorg. Chem. 31, 1045-1049.  [CrossRef] [ChemPort] [ISI]
Bramnik, K. G. & Ehrenberg, H. (2004). Z. Anorg. Allg. Chem. 630, 1336-1341.  [CrossRef] [ChemPort]
Brandenburg, K. (1998). DIAMOND. University of Bonn, Germany.
Broussely, M., Perton, F., Biensan, P., Bodet, J. M., Labat, J., Lecerf, A., Delmas, C., Rougier, A. & Pérès, J. P. (1995). J. Power Sources, 54, 109-114.  [CrossRef] [ChemPort] [ISI]
Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.  [CrossRef] [ISI] [details]
Bruce, P. G., Armstrong, A. R. & Gitzendanner, R. L. (1999). J. Mater. Chem. 9, 193-198.  [ISI] [CrossRef] [ChemPort]
Caillet, P. (1967). Bull. Soc. Chim. Fr. pp. 4750-4757.
Capitaine, F., Graverau, P. & Delmas, C. (1996). Solid State Ionics, 89, 197-202.  [CrossRef] [ChemPort] [ISI]
Dahn, J. R., von Sacken, U., Juzkow, M. W. & Al-Janaby, H. (1991). J. Electrochem. Soc. 138, 2207-2211.  [CrossRef] [ChemPort] [ISI]
Daidouh, A., Veiga, M. L. & Pico, C. (1997). J. Solid State Chem. 130, 28-34.  [CrossRef] [ChemPort] [ISI]
Delmas, C., Ménétrier, M., Croguennec, L., Saadoune, I., Rougier, A., Pouillerie, C., Prado, G., Grüne, M. & Fournès, L. (1999). Electrochim. Acta, 45, 243-253.  [ISI] [CrossRef] [ChemPort]
Duisenberg, A. J. M. (1992). J. Appl. Cryst. 25, 92-96.  [CrossRef] [ChemPort] [ISI] [details]
Eda, K., Chin, K., Sotani, N. & Witlingham, M. S. (2004). J. Solid State Chem. 177, 916-921.  [ISI] [CrossRef] [ChemPort]
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.  [CrossRef] [ChemPort] [details]
Flack, H. D. (1983). Acta Cryst. A39, 876-881.  [CrossRef] [details]
Gatehouse, B. M., Jenkins, C. E. & Miskin, B. K. (1983). J. Solid State Chem. 46, 269-274.  [CrossRef] [ChemPort] [ISI]
Gatehouse, B. M. & Leverett, P. (1968). J. Chem. Soc. A, pp. 1293-1298.
Gatehouse, B. M. & Miskin, B. K. (1975). Acta Cryst. B31, 1293-1299.  [CrossRef] [details] [ISI]
Guilmard, M., Croguennec, L. & Delmas, C. (2003). Chem. Mater. 15, 4484-4493.  [ISI] [CrossRef] [ChemPort]
Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, 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]
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]
Nguyen, P. T. & Sleight, A. W. (1996). J. Solid State Chem. 122, 259-265.  [CrossRef] [ChemPort] [ISI]
North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359.  [CrossRef] [details]
Ouerfelli, N., Guesmi, A., Molinié, P., Mazza, D., Zid, M. F. & Driss, A. (2007). J. Solid State Chem. 180, 2942-2949.  [ISI] [CrossRef] [ChemPort]
Seleborg, M. (1967). Acta Chem. Scand. 21, 499-504.  [CrossRef] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Tarascon, J. M., Wang, E., Shokoohi, F. K., McKinnon, W. R. & Colson, S. (1991). J. Electrochem. Soc. 138, 2859-2864.  [CrossRef] [ChemPort] [ISI]
Thackeray, M. M., Johnson, P. J., De Picciotto, L. A., Bruce, P. G. & Goodenough, J. B. (1984). Mater. Res. Bull. 19, 179-187.  [CrossRef] [ChemPort] [ISI]
Yuh, C., Johnsen, R., Farooque, M. & Maru, H. (1995). J. Power Sources, B56, 1-10.  [CrossRef] [ISI]


Acta Cryst (2012). E68, i80-i81   [ doi:10.1107/S1600536812041876 ]

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