Two new one-dimension copper(II) coordination polymers [CuL 2(NCS) 2] n ( 1) and [CuL 2(NO 3) 2] n ( 2) (L = (C 5H 4N)C(CH 3) N–N (CH 3)C(C 5H 4N)) have been synthesized and characterized by IR, elemental analysis, TG technique and X-ray crystallography. Each Cu(II) atom has a distorted octahedral N 6 ( 1) or N 4O 2 ( 2) environment with four pyridyl N atoms from four ligands and two N atoms from two NCS − anions for polymer 1 or two O atoms from two NO 3 − anions for polymer 2, respectively. A pair of bis-monodentate bridging ligands links two Cu(II) centers to form one dimension chain structure containing bimetallic 22-membered macrometallacyclic rings. 1D chain is held together with its neighboring ones via C–H⋯S hydrogen bonds for 1 and C–H⋯O hydrogen bonds, C–H⋯π interactions for 2 to form a 3D supramolecular structure, respectively. The luminescent properties of the polymers 1 and 2 were investigated in the solid state at room temperature.