Three new Zn(Ⅱ)/Cd(Ⅱ) coordination polymers based on 2-mercaptonicotinic acid (H2mna) with 1,2-di(4-pyridyl)ethylene (dpe) introduced as a bridging ligand have been synthesized via hydrothermal method and structurally characterized by single-crystal X-ray diffraction as well as elemental analysis and IR. As reported in this paper, [Zn2(dpe)0.5(mna)2] (1) can be classified as a two-dimensional layer structure in which the 1D chain composed of Zn(Ⅱ) and mna ligands is bridged by dpe ligands, while the complex named [Zn4(dpe)4(mna)4] (2) is a tetra-nuclear cluster compound. These two compounds are further extended to three-dimensional structures by hydrogen bonds along with C-H…π and π…π interactions. Compound 3 with general formular [Cd2(dpe)0.5(mna)2]·H2O belongs to a three-dimensional porous structure in which the 2D metal layers formed by the coordination of Cd(Ⅱ) and mna ligands are connected with the bridging of dpe ligands. Three new Zn (Ⅱ) / Cd (Ⅱ) coordination polymers based on 2-mercaptonicotinic acid (H2mna) with 1,2-di (4-pyridyl) ethylene (dpe) introduced as a bridging ligand have been synthesized via hydrothermal method and structurally characterized by single-crystal X-ray diffraction as well as elemental analysis and IR. As reported in this paper, [Zn2 (dpe) 0.5 (mna) 2] can be classified as a two-dimensional layer structure in which the 1D chain composed of Zn (II) and mna ligands is bridged by dpe ligands, while the complex named [Zn4 (dpe) 4 (mna) 4] (2) is a tetra-nuclear cluster compound. These two two compounds are further extended to Three-dimensional structures by hydrogen bonds along with CH ... π and π ... π interactions. Compound 3 with general formular [Cd2 (dpe) 0.5 (mna) 2] · H2O belongs to a three-dimensional porous structure in which the 2D metal layers formed by the coordination of Cd (II) and mna ligands are connected with the bridging of dpe ligands.