Abstract: A new supramolecular Co(Ⅲ)-based complex with N, N'-bis-5-nitro-salicylidene)-1,2 -diaminoethane was synthesized by hydrothermal method. The structure of complex was characterized by elemental analysis, IR and single-crystal X-ray diffraction. X-ray structural analysis showed that the ligand employs chelate mode to link with Co(Ⅲ) ion. The three-dimensional network of complex was formed from hydrogen bonding interaction. The result of thermal analysis demonstrated that the title complex had superior thermo stability. In addition, the synthetic conditions of the complex was discussed.