A　novel　compound,　(Himi)(H3O)　[Cu(imi)2]　2[P2Mo5O23]·H2O　1　(imi　=　imidazole),　was　synthesized　by　hydrothermal　method　and　characterized　by　X-ray　single　analysis,　ESR　spectrum,　one-dimensional　(1D)　infrared　spectroscopy　and　two-dimensional　(2D)　correlation　infrared　spectroscopy　under　thermal　and　magnetism　perturbation.　Crystal　data　for　the　compound　1:　orthorhombic　system,　space　group　Pnma,　a　=　14.580(3)　Å,　b　=　21.073(4)　Å,　c　=　16.664(3)　Å,　Z　=　4.　It　consists　of　the　Mo-Cu　building-blocks　[Cu(imi)　4]2[P2Mo5O23]　2-,　protonated　imidazole　cations　and　water　molecules.　In　the　Mo-Cu　building-blocks,　[Mo5P2O23]6-　clusters　are　linked　by　{Cu(imi)4}2+　group　to　form　a　two-dimension　parallelogram　griddling　structure.　From　the　2D　IR　correlation　spectroscopy　analyses,　it　is　discovered　that　the　intensity　changes　of　MoO　and　P-O　band　are　sensitive　to　the　temperature　variation,　whereas　the　Mo-O　bond　linking　to　Cu2+　can　be　remarkably　affected　by　the　magnetism　variation.　Furthermore,　the　intensity　changes　of　P-O　bands　occur　prior　to　that　of　the　MoO　band　during　the　temperature　elevation.　©　2005　Elsevier　B.V.　All　rights　reserved.