A　novel　molybdophosphate　supermolecular　compound　(bipyH2)2(H2P2Mo5O　23)　·　H2O　has　been　synthesized　by　hydrothermal　method　and　characterized　by　crystal　X-ray　structure　analysis,　IR　spectrum,　Raman　spectrum,　UV-Vis　DRIS　spectrum,　fluorescence　spectrum　and　CV.　The　crystal　belongs　to　monoclinic　system　with　a　space　group　P21/c,　a=1.679　51(7)　nm,　b=1.151　93(4)　nm,　c=1.889　08(8)　nm,　β=108.335(1)°,　V=3.469　2(2)　nm3,　Z=4,　Dc=2.382　g/cm3,　F(000)=2　408,　μ=1.951　mm-1,　R=0.024　4,　Rw=0.072　1.　The　heteropoly　anion[H2P2Mo5O23]4-　and　protonated　4,4′-bipy　are　connected　to　a　supermolecular　compound　by　hydrogen　bonds;　and　the　anions　contain　five　MoO6　octahedra　and　two　PO4　tetrahedron;　Mo,　P　atoms　show　a　distorted　pentagonal　bipyramidal　configuration,　and　the　heteropoly　anions　are　connected　to　a　infinite　planar　structure　with　the　protonated　4,4′-bipy.