Applicability of EXAFS spectroscopy for determination of the molecular stru
cture of heterometallic chalcogenide clusters in the crystalline state and
in solution was examined. The spatial structure of the metal core of the Fe
MoW(mu(3)-Se)(CO)(7)(eta(5)-C5H5) cluster was deter mined using EXAFS data
obtained at the K absorption edge for Fe, Mo, and Se and at the L-III-edge
for W. The geometric parameters (the bond lengths and bond angles) obtained
from EXAFS data are close to those determined by X-ray analysis. The Mo K-
edge EXAFS study of the structurally similar FeMo2Te(CO)(7)(eta(5)-C5H5) cl
uster both in the crystalline state and in o-xylene solution confirmed that
the geometry of the metal core of the cluster is retained in solution.