Three new complexes have been prepared based on the transition metals and zwitterionic dicarboxylate ligand 1,1'-(1,4-phenylene-bis(methylene))-bis(pyridine-3-carboxylic acid) (L), whose formulas are {[Cd 4 (L)(SO 4 )]• (Cl) 6 } n (1), [Zn(L)Cl 2 ] n (2), and [Co(L)Cl 2 ] n (3), respectively. Complexes 1-3 have been characterized by elemental analyses, IR spectroscopy, XRD, thermal analyses and single crystal X-ray (powder) diffraction. 1 crystallizes in monoclinic space group C2/m, displaying a 2-D layer structure with three unique Cd 2+ centers. 2 and 3 are isomorphic structures with the orthorhombic Cmca space group. They exhibit a 1-D zigzag chain, which can be linked to generate a 2-D layer via hydrogen bonding interactions (C-H…O). Moreover, electrochemical behavior reveals that the redox reaction of 3-CPE is a surface-controlled reaction. And the luminescent properties of the title complexes have been investigated at room temperature.