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A novel three-dimensional inorganic bimetallic compound Cu[Mo3O10]·H2O 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in the orthorhombic system, space group Pnma, a=8.6085(17) A˚, b=7.5822(15) A˚, c=13.690(3) A˚, V=893.6(3) A˚3, Z=4, λ(MoKα) = 0.71073 A˚ (R(F)=0.0357 for 1101 reflections). The structure of compound 1 is based on [{Mo3O10}2−]∞ isopolyoxomolybdate chains bonded together with CuO4 tetrahedra into a three-dimensional inorganic open framework. Three types of Mo–Cu layers and one-dimensional tunnels are observed in the title compound. [Copyright &y& Elsevier]