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Preparation and structural study from neutron diffraction data of Pr5Mo3O16
Authors:MJ Martínez-Lope  D Sheptyakov
Institution:a Instituto de Ciencia de Materiales de Madrid, C.S.I.C., Cantoblanco, E-28049 Madrid, Spain.
b Laboratory for Neutron Scattering, Paul Scherrer Institut, CH-5232 Villigen PSI, Switzerland
Abstract:The title compound has been prepared as polycrystalline powder by thermal treatments of mixtures of Pr6O11 and MoO2 in air. In the literature, an oxide with a composition Pr2MoO6 has been formerly described to present interesting catalytic properties, but its true stoichiometry and crystal structure are reported here for the first time. It is cubic, isostructural with CdTm4Mo3O16 (space group Pn-3n, Z=8), with a=11.0897(1) Å. The structure contains MoO4 tetrahedral units, with Mo-O distances of 1.788(2) Å, fully long-range ordered with PrO8 polyhedra; in fact it can be considered as a superstructure of fluorite (M8O16), containing 32 MO2 fluorite formulae per unit cell, with a lattice parameter related to that of cubic fluorite (af=5.5 Å) as a≈2af. A bond valence study indicates that Mo exhibits a mixed oxidation state between 5+ and 6+ (perhaps accounting for the excellent catalytic properties). One kind of Pr atoms is trivalent whereas the second presents a mixed Pr3+-Pr4+ oxidation state. The similarity of the XRD pattern with that published for Ce2MoO6 suggests that this compound also belongs to the same structural type, with an actual stoichiometry Ce5Mo3O16.
Keywords:R2MoO6  Rare-earth molybdenum oxides  Fluorite superstructure  Mixed valence compound  Ce2MoO6  Ce5Mo3O16
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