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Three metal molybdate hydrates,Fe(H2O)2(MoO4)2·H3O(FeMo),NaCo2(MoO4)2(H3O2)(CoMo)and Mn2(MoO4)3·2H3O(MnMo),were synthesized by the mixed-solvent-thermal methods and characterized by singlecrystal X-ray diffraction.X-Ray photoelectron spectroscopy and bond-valence sums were applied to confirming the valance of Fe,Co,Mn and Mo.Thermo-gravimetric analysis and X-ray powder diffraction measurements indicate that the samples were converted to different structural compounds upon heating in air at 600 ℃ for 1 h.The magnetic properties of these compounds were studied.The dominant magnetic interactions are antiferromagnetic in nature.However,different synthesis conditions led to the diversity of magnetic properties of compound CoMo.