One three-dimensional coordination polymer [Co(AIP)(BPY)(0.5)center dot H2O](n)center dot 2nH(2)O (AIP, 5-aminoisophthalic; BPY, 4,4'-bipyridine) has been synthesized solvothermally and characterized by powder X-ray diffraction, FT-IR spectra. The molar heat capacities of [Co(AIP)(BPY)(0.5)center dot H2O](n)center dot 2nH(2)O were measured by temperature modulated differential scanning calorimetry (TMDSC) over the temperature range of 188-3001K for the first time, and no phase transition or thermal anomaly was detected in the experimental temperature range. The thermodynamic parameters relative to the standard reference temperature 298.15K were derived based on the above molar heat capacities data. Besides, a two-step sequential thermal decomposition mechanism for the material was investigated through the thermogravimetry (TG-DTG) from 300 to 1073 K. (C) 2013 Elsevier B.V. All rights reserved.