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X-ray standing wave (XSW) analysis and X-ray photoelectron spectroscopy are used to trace the electronic and atomic-scale structural changes of a supported vanadium oxide system at different stages of its oxidationreduction cycle. Both the oxidation state and adsorption geometry of the vanadium oxide and its R-Fe 2 O 3 -(0001) single crystal support show reversible changes through the oxidation-reduction cycle characteristic of catalytic behavior. The 3D V atomic distribution maps, derived from the summation of the XSW measured Fourier components, reveal that the V undergoes adsorption site exchange during the oxidation and reduction cycle.

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