Li0.17Na5.83Mo11O36

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

doi:10.1107/S1600536812044224

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 (Mo-O) = 0.005 Å
Disorder in main residue
R = 0.037
wR = 0.095
Data-to-parameter ratio = 12.7
Details

Li_0.17Na_5.83Mo₁₁O₃₆

Ines Ennajeh,^a Hamadi Hamza,^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 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); Whittingham & Silbernagel (1976); Mizushima et al. (1980); Kanno et al. (1994); Guilmard et al. (2003); Lin et al. (2005); Yuh et al. (1995); Koyama et al. (2004). For details of structurally related compounds, see: Bramnik & Ehrenberg (2004); Caillet (1967); Seleborg (1967). For further synthetic details, see: Bramnik & Ehrenberg (2004). For bond-valence sums, see: Brown & Altermatt (1985). For related literature, see: Koyama et al. (2004).

Experimental

Crystal data

Li_0.17Na_5.83Mo₁₁O₃₆
M_r = 1766.55
Monoclinic, C 2/c
a = 7.2250 (9) Å
b = 17.863 (2) Å
c = 22.086 (3) Å
= 90.162 (8)°
V = 2850.5 (6) Å³
Z = 4
Mo K radiation
= 4.89 mm^-1
T = 298 K
0.30 × 0.24 × 0.14 mm

Data collection

Enraf-Nonius CAD-4 diffractometer
Absorption correction: scan (North et al., 1968) T_min = 0.25, T_max = 0.50
6662 measured reflections
3138 independent reflections
3065 reflections with I > 2(I)
R_int = 0.032
2 standard reflections every 120 min intensity decay: 2.3%

Refinement

R[F² > 2(F²)] = 0.037
wR(F²) = 0.095
S = 1.33
3138 reflections
247 parameters
1 restraint
_max = 1.39 e Å^-3
_min = -1.85 e Å^-3

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 (Farrugia, 1999).

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

References

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inorganic compounds