A　novel　compound,　(4,4′-Hbpy)2(K2Mo　8O26)　1　(bpy　=　bipydine),　was　synthesized　by　hydrothermal　method　and　characterized　by　X-ray　single　analysis,　thermalgravimetric　analysis,　one-dimensional　(1D)　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　MoO,　NH　and　CC　stretching　vibration　are　sensitive　to　the　temperature　variation,　and　the　intensity　changes　of　asymmetry　stretching　vibration　of　the　terminal　MoO　occur　prior　to　that　of　terminal　MoO　linked　by　K　atom.　At　the　same　time,　the　peaks　of　asymmetry　stretching　vibrations　of　the　terminal　MoO　and　the　stretching　vibrations　of　NH　split　into　two　peaks　respectively　in　2D　IR　correlation　spectroscopy.　©　2005　Elsevier　B.V.　All　rights　reserved.