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A new infinite three-dimensional framework structure of the title compound [H6MoVI8O27]·3C4N2H10 has been synthesized under mild hydrothermal conditions and charac- terized by elemental analyses, IR, fluorescent spectra and single-crystal X-ray diffraction.C12H36Mo8N6O27 crystallizes in the triclinic system, space group with a = 8.820(3), b = 9.534(3), c = 10.993(4) -, α = 99.985(17), β = 106.65(2), γ = 101.650(14)o, V = 840.6(5) -3, Mr = 1463.99, Z = 1, Dc = 2.892 g/cm3, μ = 2.993 mm-1, F(000) = 702, the final R = 0.0676, wR = 0.1920 and S = 1.074 for 2196 observed reflections with I > 2((I).The title compound exhibits a novel infinite three-dimensional (3D) framework composed of a [H6MoVI8O27] subunit and three dissociated piperazine fragments.The complex exhibits two strong fluorescent emission bands at ca.417 and 440 nm (λex = 378 nm) in the solid state at room temperature.