A　novel　compound,　(4,4＇-HbpY)(2)(K2Mo8O26)　1　(bpy　=　bipydine),　was　synthesized　by　hydrothermal　method　and　characterized　by　X-ray　single　analysis,　thermal　gravimetric　analysis,　one-dimensional　(ID)　infrared　spectroscopy　and　two-dimensional　(2D)　correlation　infrared　spectroscopy　under　thermal　perturbation.　In　the　compound　1,　the　[Mo8O26]　units　link　to　potassium　ions　to　form　layer　structure,　and　the　protonated　4,4＇-bpy　are　linked　to　chains　by　hydrogen　bonds.　The　2D　IR　correlation　spectroscopy　study　indicates　that　the　intensity　changes　of　Mo=O,　N-H　and　C-C　stretching　vibration　are　sensitive　to　the　temperature　variation,　and　the　intensity　changes　of　asymmetry　stretching　vibration　of　the　terminal　Mo=O　occur　prior　to　that　of　terminal　Mo=O　linked　by　K　atom.　At　the　same　time,　the　peaks　of　asymmetry　stretching　vibrations　of　the　terminal　Mo=O　and　the　stretching　vibrations　of　N-H　split　into　two　peaks　respectively　in　2D　IR　correlation　spectroscopy.　(c)　2005　Elsevier　B.V.　All　rights　reserved.