Synthesis and superstructural characterization of Fe1.89Mo4.11O7
Chumbley, L. Scott
Superstructuring in the new compound Fe1.89Mo4.11O7 has been elucidated by transmission electron microscopy. This compound is a member of the family M2MO4O7 and has both iron and molybdenum atoms occupying octahedrally coordinated sites in the structure, represented by Fet(Fe0.89M0.11)0Mo4O7. The superstructuring, detected only by electron diffraction, involved tripling of all three lattice parameters of the subcell. The subcell was structured by single crystal x-ray diffraction [Imma, no. 74, a = 5.9793(5) Å, b = 5.7704(4) Å, and c = 17.036(1) Å]. This structure type contains a close-packed arrangement of Mo4O7 units, which are infinite chains of trans edge-shared molybdenum octahedra running parallel to b*. Two different coordination environments are observed for the cations. Parallel to the a* direction, infinite edge-sharing MO6 (M = 89% Fe or 11% Mo) octahedra are observed. The second cation site, with nearly tetrahedral coordination by oxygen, is filled solely by iron. The superstructure can be rationalized by a regular arrangement of iron and molybdenum atoms in the octahedrally coordinated cation sites.
This article is from Journal of Materials Research 9 (1994): 891-897, doi: 10.1557/JMR.1994.0891. Posted with permission.