Utilizing mononuclear complex Ni（2-mpac）2（H2O）2 as the molecular building block,a novel coordination polymer [Ni2（2-mpac）4（4,4＇-bpy）·2H2O]n（1,2-mpac = 5-methyl-2-pyrazinecar-boxylic acid,4,4＇-bpy = 4,4＇-bipyridine） was successfully synthesized and structurally characterized by X-ray single-crystal diffraction method.Crystal data：monoclinic,space group C2/c,a = 23.870（1）,b = 9.887（4）,c = 18.929（9） ,β = 126.840（5）°,V = 3575（3） 3,Z = 4,S = 1.046,μ = 1.594 mm-1,F（000） = 1768 and Dc = 1.127 g·cm-3.The final R = 0.0351 and wR = 0.0792 for 2372 observed reflections with Ⅰ 〉 2σ（Ⅰ） and R = 0.0564 and wR = 0.0938 for all reflections.
A new coordination polymer with the formula of [Co（2-mpac）2（py）·4H2O）]n （1, 2-mpac = 5-methyl-2-pyrazinecarboxylic acid, py = pyrazine） has been synthesized through hydrothermal synthesis and structurally characterized by X-ray single-crystal diffraction method. 1 exhibits a 3D supramolecular network. Crystal data： monoclinic, space group C2/m, a = 15.907（9）, b = 7.104（3）, c = 9.793（5）, β = 95.232（8）o, V = 1102.0（10）3, Z = 2, S = 0.995, the final R = 0.0509, wR = 0.1626 for 1002 observed reflections with （I 〉 2σ（I）） and R = 0.0530, wR = 0.1667 for all data. In addition, elemental analysis, IR and thermalgravimetric analysis are presented.
