A novel compound, [H(2)bpy][Cu(4,4'-bpy)](2)[HPCuMo11O39] (1), has been prepared under mild hydrothermal conditions and has been structurally characterized by single-crystal X-ray diffraction. Compound 1 exhibits a novel two-dimensional network constructed from the interconnecting of polyoxomolybdate chains, {HPCuMo11O39}(n)(4n-), and transition metal coordination polymer chains, {Cu(4,4'-bpy)}(n)(n+). It is the first example of a two-dimensional structure formed by a polyoxomolybdate chain through the linkage of a transition metal coordination polymer chain.
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