LiNa5Mo9O30

Hamza, H.; Ennajeh, I.; Zid, M.F.; Driss, A.

doi:10.1107/S1600536812041876

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 (Mo-O) = 0.007 Å
R = 0.035
wR = 0.096
Data-to-parameter ratio = 12.9
Details

LiNa₅Mo₉O₃₀

Hamadi Hamza,^a Ines Ennajeh,^a Mohamed Faouzi Zid ^a ^* and Ahmed Driss ^a

^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); Thackeray et al. (1984); Dahn et al. (1991); Tarascon et al. (1991); Kanno et al. (1994); Yuh et al. (1995); Broussely et al. (1995); Capitaine et al. (1996); Delmas et al. (1999); Bruce et al. (1999); Guilmard et al. (2003). For similar structure types, see: Caillet (1967); Seleborg (1967); Gatehouse et al. (1983). For background to their electronic properties, see: Aranda et al. (1992); Nguyen & Sleight, (1996); Daidouh et al. (1997); Ouerfelli et al. (2007). For details of structural relationships between these compounds, see: Gatehouse & Leverett (1968); Gatehouse & Miskin (1975); Eda et al. (2004). For the preparation, see: Bramnik & Ehrenberg (2004). For bond-valence sums, see: Brown & Altermatt (1985).

Experimental

Crystal data

LiMo₉Na₅O₃₀
M_r = 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 radiation
= 4.77 mm^-1
T = 298 K
0.30 × 0.20 × 0.10 mm

Data collection

Enraf-Nonius CAD-4 diffractometer
Absorption correction: scan (North et al., 1968) T_min = 0.31, T_max = 0.61
3006 measured reflections
2605 independent reflections
2579 reflections with I > 2(I)
R_int = 0.035
2 standard reflections every 120 min intensity decay: 2.3%

Refinement

R[F² > 2(F²)] = 0.035
wR(F²) = 0.096
S = 1.13
2605 reflections
202 parameters
1 restraint
_max = 1.55 e Å^-3
_min = -1.65 e Å^-3
Absolute structure: Flack (1983), 1259 Fridel pairs
Flack parameter: 0.51 (10)

Data collection: CAD-4 EXPRESS (Duisenberg, 1992; Macícek & Yordanov, 1992); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1998); software used to prepare material for publication: WinGX publication routines (Farrugia, 1999).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: VN2054 ).

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inorganic compounds