Four coordination polymers based on two bis-pyridyl-bis-amide ligands and three aromatic dicarboxylates with different substituent groups, namely, [Co(3-bpcb) 1.5 (NPH)(H2O)]·4H2O (1), [Co(3-bpcb)(NIPH)] (2), [Co(3-bpcb)0.5 (5-H2 AIP)]·2H2O (3), [Co(3-bpcd) 0.5 (5-H2 AIP)(H2O)]·2H2O (4) [3-bpcb = N,N′-bis(3-pyridinecarboxamide)-1,4-benzene, 3-bpcd = N,N′-bis(3- pyridine)cyclohexane-1,4-dicarboxamide, H2 NPH = 3-nitrophthalic acid, H2 NIPH = 5-nitroisophthalic acid, 5-H4 AIP = 5-aminoisophthalic acid] have been synthetized under hydrothermal conditions. Complex 1 displays a one dimensional (1D) chain based on the binuclear [Co2 (NPH)2 ] units and 3-bpcb ligands, which is extended into a three dimensional (3D) supramolecular framework through hydrogen bonding and - stacking interactions. In complex 2, the (3,5)-connected two dimensional (2D) layers are constructed from 1D Co-NIPH chains and bidentate-bridging 3-bpcb ligands. Complex 3 is a 2D double layer based on Co-5-H2 AIP 2D layers and 3-bpcb pillars. Complex 4 also displays a 2D network, which is constructed from the Co-5-H2AIP 1D double chains and 3-bpcd ligands. Finally, complexes 2-4 are extended into 3D supramolecular frameworks by hydrogen bonding or - stacking interactions. The substituent groups of dicarboxylates play an important role in the assembly and structures of the title complexes. In addition, the fluorescent properties of complexes 1-4 and the electrochemical behaviors of 3 and 4 at room temperature have been investigated. Four coordination polymers based on two bis-pyridyl-bis-amide ligands and three aromatic dicarboxylates with different substituent groups, namely, [Co (3-bpcb) 1.5 (NPH) (3-bpcb) 0.5 (5-H2 AIP)] 2H2O (3) [Co (3-bpcd) 0.5 (5-H2 AIP) · 2H2O (4) [3-bpcb = N, N’-bis (3-pyridinecarboxamide) -1,4- benzene, 3-bpcd = N, N’-bis H2 NPH = 3-nitrophthalic acid, H2 NIPH = 5-nitroisophthalic acid, 5-H4 AIP = 5-aminoisophthalic acid] have been synthetized under hydrothermal conditions. Complex 1 displays a one dimensional (1D) chain based on the binuclear [Co2 (NPH) 2] units and 3-bpcb ligands, which is extended into a three dimensional (3D) supramolecular framework through hydrogen bonding and - stacking interactions. In complex 2, the are constructed from 1D Co-NIPH chains and bidentate-bridging 3-bpcb ligands. Complex 3 is a 2D double layer based on Co-5-H2 AIP 2D l Complex 4 also displays a 2D network, which is constructed from the Co-5-H2AIP 1D double chains and 3-bpcd ligands. Finally, complexes 2-4 are extended into 3D supramolecular frameworks by hydrogen bonding or - stacking interactions. The substituent groups of dicarboxylates play an important role in the assembly and structures of the title complexes. In addition, the fluorescent properties of complexes 1-4 and the electrochemical behaviors of 3 and 4 at room temperature have been investigated.