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The homodinuclear cobalt(II) complex [Co2(dipic)2(H2O)5]•2H2O was synthesized with pyridine-2,6-dicarboxylic acid (H2dipic) and cobalt(II) acetate as raw materials by room temperature solid-solid reaction. The complex was characterized by elemental analyses, single crystal X-ray diffraction, X-ray powder diffraction, Fourier transform infrared spectroscopy, UV spectra, and thermogravimetry and differential scanning calorimetry. Its crystal structure belongs to monoclinic system and space group P2(1)/c. There are two types of the Co(II) ions, and they are all six-coordination, one Co(II) is coordinated by four carboxyl O atoms and two pyridine N atoms from two dipic2- anions, and another Co(II) is coordinated by five O atoms from five H2O molecules and one bridged carboxyl O atom from the dipic2- anion. The possible pyrolysis reactions in the thermal decomposition processes of the complex, the experimental and calculated percentage mass loss are also given.