Three　Strandberg　type　molybdophenylphosphonate　complexes　with　the　formular　{[Cu(2,2＇-bpy)(2)](2)　[(C6H5P)(2)Mo5O21]}center　dot　H2O　(1),　[Ni(2,2＇-bpy)(3)](2)[(C6H5P)(2)Mo5O21]center　dot　2H(2)O　(2)　and　{[Ni(2,2＇-bpy)(2)](2)[(C6H5P)(2)　Mo5O21]center　dot　H2O}center　dot　2H(2)O　(3)　(bpy　=　bipyridine)　have　been　synthesized　under　hydrothermal　condition　and　structurally　determined　by　single-crystal　X-ray　diffraction.　The　cations　and　the　anionic　clusters　in　three　compounds　are　linked　via　strong　covalent　bonds　or　the　hydrogen　bonds.　Intermolecular　interaction　makes　the　building　blocks　construct　supramolecular　structure　and　assembles　a　spiral　chain　in　compound　2.　The　interaction　also　plays　an　important　role　in　the　stabilization　of　the　molecular　aggregate.　The　obtained　compounds　were　characterized　by　various　means　containing　elemental　analysis,　PXRD,　IR,　TGA　and　thermal　infrared　spectra.　In　order　to　investigated　the　structural　characteristics　of　intermolecular　interaction　and　thermal　stability　or　magnetic　sensitivity　of　the　compounds,　2D-IR　correlation　spectra　(2D-IR　COS)　under　thermal/magnetic　perturbation　were　carried　out.　And　the　magnetic　property　was　studied　as　well.　(C)　2014　Elsevier　B.V.　All　rights　reserved.