Two coordination polymers (［Co(tib)(mpda)(H2O)2］·H2O, ［Ni(tib)(mpda)(H2O)2］·H2O) were synthesized based on flexible phenyldiacetic acid, and characterized by elemental analysis, infrared spectroscopy, thermogravimetric analysis and X-ray single crystal diffraction. In the structure of ［Ni(tib)(mpda)(H2O)2］·H2O, the tib ligands coordinate as three nodes with Co(II) ions to form a 2D grid plane; cis-mpda ligands are attached to the 2D grid face as end-bases; through the O—H…O interaction between the mpda virgin carboxyl O and the coordinated water molecule (bond length of O1…O3 is 0.262 4 nm, ∠O5—H5A…O2=155.41°), a three-dimensional supramolecular network structure is formed. Two coordination polymers belong to the heterogeneous crystal structure. The specific surface areas of the two coordination polymers are 54 and 58 m2/g, respectively. ［Ni(tib)(mpda)(H2O)2］·H2O has a complete cyclic voltammetric curve (reduction and oxidation potentials are 0.205 and 0.563 V, respectively) and good scanning rate.