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A compound {[Co(azpy)2(NCS)2]·1/4EtOH·1/2H2O}n(1), where azpy=4,4'- azo-bispyridine, was synthesized and characterized by means of IR, TGA-DTA, magnetic susceptibility and X-ray single crystal diffraction. It consists of two independent sets of fully interlocked two-dimensional networks with the dihedral angle 61. 7°, organized in parallel stacks of the sheets which are made of edge-shared [Co(Ⅱ)]4 squares separated by 0. 906 2 nm, and defined size rhombic channels. The thermal gravimetric analysis indicates that the framework is stable up to 198 C. The variable-temperature magnetic susceptibility measurements indicated that there is a weak antiferromagnetic interaction between the cobalt(Ⅱ) ions in the complex (1).