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The structural transition and atomic ordering of a new series of ordered double perovskite oxides Sr2FexMo2-xO6 (0.8 less than or equal to x less than or equal to 1.5) have been studied by X-ray powder diffraction (XRD). Rietveld refinement of the powder diffraction profiles indicates that the crystal structure of the compounds Sr2FexMo2-xO6 changes from a tetragonal I4/mmm lattice to a cubic Fm(3)over-bar-m lattice around x = 1.2 and the lattice parameters decrease slightly as Fe content increases. The degree of ordering in Sr2FexMo2-xO6 exhibits a maximal at x = 0.95 and decreases as x deviates from 0.95. (C) 2002 Elsevier Science B.V. All rights reserved.