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Mg−Mo−O catalysts have been investigated with different techniques (XRD, XPS, IR, and EPR spectroscopies) in order to explain the difference in catalytic behavior in the oxidative dehydrogenation of propane to propene. The active site would be a coordinatively unsaturated form of Mo5+. The active Mo5+ could be generated on the surface by propane reduction. The slight excess of MoO3 which is necessary for the catalyst to become an active one probably contributes to the formation of Mo5+.