The hydrothermal reaction of MoO3, CuSO4·5H2O, 1,2,4-triazole and H2O produces a 50% yield of [{Cu2-(triazolate)2(H2O)2}Mo4O13], a material constructed from {Mo4O13}n2n– chains entrained within the three dimensional framework provided by the {Cu2(triazolate)2(H2O)2}n2n+ polymeric complex.