Infrared (IR) spectra have been measured for a supramolecular assembly based on intermolecular hydrogen bonding between sebacic acid (SEA) molecule as a proton donor and azopyridine (AZP) molecules as a proton acceptor ([SEA·AZP]) over a temperature range from 29 to 155°C in order to explore the involved hydrogen-bonding species and heat-induced structural variations. The temperature-dependent IR spectra have shown that the intermolecular hydrogen bondings are formed and stable enough in the supramolecular assembly but they become slightly decoupled when temperature is higher than the clearing point of supramolecular assembly. Two-dimensional (2D) correlation spectra in 1780–1660cm
−1 region have provided information about the structural variations of intermolecular hydrogen bonding concerning with C
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O group. While, 2D correlation spectra in 880–820cm
−1 region have revealed hydrogen bonding changes concerning with proton in the adjacent position of pyridyl ring. Three different hydrogen-bonded species in the supramolecular assembly have been clarified by the 2D correlation analysis. The specific order of the temperature-induced structural changes in the involved intermolecular hydrogen-bonded species in supramolecular assembly has also been elucidated in the present study.