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Ammonium dodecamolybdoantimonate, with a body-centred cubic symmetry, has been synthesized from antimony( 111) oxide and ammonium heptamolybdate in aqueous acidic solution. The corresponding potassium, rubidium and caesium salts were prepared by ion exchange. They were characterized by elemental analysis, X-ray diffraction, X-ray fluorescence, i.r., X-ray photoelectron spectroscopy, thermogravimetry, and differential thermal analysis.