Two new macrocyclic complexes, [ML](ClO4)(2)center dot 4,4'-bpy [M = Cu (1) and Ni (2), L = 1,3,6,9,11,14-hexaazatricyclo [12.2.1.1(6,9)]octadecane, 4,4'-bpy = 4,4'-bipyridine], have been synthesized and structurally characterized by X-ray crystallography analyses. Complex 1 crystallizes in the triclinic crystalline system of space group P-1, while complex 2 crystallizes in the monoclinic crystalline system of space group P2(1)/n. In the both complexes, M(II) [M = Cu (1) and Ni (2)] centers are located in a distorted square plane environment. The weakly interactions raised the structure unit to a 3D network.