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Synthesis and superstructural characterization of Fe1.89Mo4.11O7

Published online by Cambridge University Press:  03 March 2011

George L. Schimek
Affiliation:
Ames Laboratory, United States Department of Energy and Department of Chemistry, Iowa State University, Ames, Iowa 50011
Robert E. McCarley
Affiliation:
Ames Laboratory, United States Department of Energy and Department of Chemistry, Iowa State University, Ames, Iowa 50011
L. Scott Chumbley
Affiliation:
Ames Laboratory, United States Department of Energy and Department of Materials Science and Engineering, Iowa State University, Ames, Iowa 50011
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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.

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Articles
Copyright
Copyright © Materials Research Society 1994

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References

REFERENCES

1(a) van de Berg, J.M., Inorg. Chim. Acta 2, 216 (1968); (b) Anzenhofer, K. and de Boer, J., Acta Crystallogi. B25, 1419 (1969); (c) Guillevic, J., LeMarouille, J. Y., and Grandjean, D., Acta Crystallogr. B30, 111 (1974); (d) Chevrel, R., Sergent, M., Meury, J. L., Quan, D. T., and Collin, Y., J. Solid State Chem. 10, 260 (1974); (e) Chevrel, R., Thise d'Etat, University of Rennes (1974); (f) Wada, H., Onoda, M., Nozaki, H., and Kawada, I., J. Solid State Chem. 63, 369 (1986); (g) Perrin, C., Chevrel, R., and Sergent, M., C.R. Acad. Ser. C 230, 949 (1975); (h) Perrin, C., Chevrel, R., and Sergent, M., C.R. Acad. Ser. C 181, 23 (1975); (i) Le Beuze, A., Zerrouki, M. C., Loirat, H., and Lissillour, R., J. Alloys and Compounds 190, 1 (1992).CrossRefGoogle Scholar
2Torardi, C. C. and McCarley, R. E., J. Am. Chem. Soc. 101, 3963 (1979).CrossRefGoogle Scholar
3Carlson, C. D., Brough, L. F., Edwards, P. A., and McCarley, R. E., J. Less-Comm. Met. 156, 325 (1989).CrossRefGoogle Scholar
4Lii, K. H., McCarley, R. E., Kim, S., and Jacobson, R. A., J. Solid State Chem. 64, 347 (1986).CrossRefGoogle Scholar
5Gall, P., Gougeon, P., and McCarley, R. E., Acta Crystallogr. C47, 1585 (1991).Google Scholar
6Gall, P., Gougeon, P., and McCarley, R. E., Acta Crystallogr. C47, 2026 (1991).Google Scholar
7Schimek, G. L., Lii, K. H., Brough, L. F., Carlin, R. T., McCarley, R.E., and Reiff, W., unpublished research.Google Scholar
8(a) McCarley, R.E., ACS Symp. Ser. 211, 273 (1983); (b) McCarley, R.E., Philos. Trans. R. Soc. London A 308, 141 (1982); (c) Lii, K. H., Ph.D. Dissertation, Iowa State University, Ames, Iowa (1985); (d) McCarley, R. E. and Brough, L. F., unpublished results.CrossRefGoogle Scholar
9Johnson, C. K., Report ORNL-5138, Oak Ridge, TN (1962).Google Scholar