The defect scheelite-type lanthanum(III) ortho-oxidomolybdate(VI) La0.667[MoO4]

Schustereit, T.; Schleid, T.; Hartenbach, I.

doi:10.1107/S1600536813000731

Volume 69
Part 2
Page i7
February 2013

Received 17 December 2012
Accepted 8 January 2013
Online 16 January 2013

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (Mo-O) = 0.001 Å
Disorder in main residue
R = 0.016
wR = 0.032
Data-to-parameter ratio = 16.2
Details

The defect scheelite-type lanthanum(III) ortho-oxidomolybdate(VI) La_0.667[MoO₄]

Tanja Schustereit,^a Thomas Schleid ^a and Ingo Hartenbach ^a ^*

^aInstitut für Anorganische Chemie, Universität Stuttgart, Pfaffenwaldring 55, 70569 Stuttgart, Germany
Correspondence e-mail: hartenbach@iac.uni-stuttgart.de

In scheelite-type La_0.667[MoO₄], one crystallographically unique position with site symmetry -4.. and an occupancy of 2/3 is found for the La³⁺ cation. The cation is surrounded by eight O atoms in the shape of a trigonal dodecahedron. The structure also contains one [MoO₄]^2- anion (site symmetry -4..), which is surrounded by eight vertex-attached La³⁺ cations. The polyhedra around the La³⁺ cations are interconnected via common edges, building up a three-dimensional network, in the tetrahedral voids of which the Mo⁶⁺ cations reside.

Related literature

For isotypic Ln_0.667[MoO₄] structures with Ln = Ce, Pr, Nd and Sm, see: Schustereit et al. (2011). For synthetic details, see: Liu et al. (2012).

Experimental

Crystal data

La_0.667[MoO₄]
M_r = 252.59
Tetragonal, I 4₁ /a
a = 5.3599 (3) Å
c = 11.9425 (7) Å
V = 343.09 (3) Å³
Z = 4
Mo K radiation
= 11.74 mm^-1
T = 293 K
0.11 × 0.08 × 0.06 mm

Data collection

Nonius KappaCCD diffractometer
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1995) T_min = 0.291, T_max = 0.480
2577 measured reflections
260 independent reflections
174 reflections with I > 2(I)
R_int = 0.046

Refinement

R[F² > 2(F²)] = 0.016
wR(F²) = 0.032
S = 0.98
260 reflections
16 parameters
_max = 0.41 e Å^-3
_min = -0.37 e Å^-3

Table 1
Selected bond lengths (Å)

La-Oⁱ	2.5728 (14)
La-Oⁱⁱ	2.5766 (14)
Mo-O	1.7606 (14)
Symmetry codes: (i) $[y+{\script{1\over 4}}, -x+{\script{1\over 4}}, z+{\script{1\over 4}}]$ ; (ii) $[-x+{\script{1\over 2}}, -y, z+{\script{1\over 2}}]$ .

Data collection: COLLECT (Nonius, 1998); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXL97.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2715 ).

Acknowledgements

This work was supported by the State of Baden-Württemberg (Stuttgart) and the Deutsche Forschungsgemeinschaft (DFG, Frankfurt/Main) within the funding program Open Access Publishing.

References

Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Liu, J., Wang, J., Zhang, Z., Chen, H., Yang, X., Li, R. & Zhao, J. (2012). J. Lumin. 137, 2874-2878.
Nonius (1998). COLLECT. Nonius BV, Delft, The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.
Schustereit, T., Müller, S. L., Schleid, Th. & Hartenbach, I. (2011). Crystals, 1, 244-253.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Stoe & Cie (1995). X-SHAPE. Stoe & Cie, Darmstadt, Germany.

inorganic compounds