Crystalline metal-organic framework cobalt （II） benzenetricarboxylate C%（BTC）2·12H2O （MOF-Co） has been prepared using solvothermal method. The reaction of cobalt （II） nitrate and 1,3,5-benzenetriearboxylic （BTC） acid in a mixed solution of N,N-dimethylformarnide （DMF）/C2H5OH/H2O （1：1：1, v/v） at low temperature for short reaction times produced this crystalline compound. Compared with traditional hydrothermal method, a mixed solution method for the synthesis of crystalline metal complex was found to be highly efficient. After water molecules were removed from this metal complex, its exposed nodes served as active sites. When this MOF-Co was employed in the oxidation of CO, it showed good catalytic properties causing 100% conversion of CO to CO2 at low temperature of 160 ℃.
Proton-conductive crystalline metal-organic framework nickel（Ⅱ） benzenetricar- boxylate Ni3（BTC）2A12H2O（MOF-Ni） was prepared by the reaction of nickel（Ⅱ） nitrate and 1,3,5- benzenetricarboxylic（BTC） acid in a mixed solvent of N,N-dimethylformamide（DMF）/C2H5OH/ H2O （1：1：1, ν/ν） at low temperature and short reaction time. It was characterized by thermo- gravimetric analyses （TG）, FT-IR and N2 adsorption-desorption. Single-crystal X-ray diffraction analysis indicated that the complex belongs to monoclinic system, space group C2 with α = 17.407（6）, b = 12.878（5）, c = 6.542（2） A, β = 112.07°, V = 1359.0（8） A^3, Dc = 1.971 g/cm3, μ = 2.166 mm^-1 and Z = 2. Linear polarization resistance （LPR） analysis showed that the complex possesses semiconducting properties.
