The first inorg/organic hybrid complex incorporating the macrocyclic oxamide, of formula [(NiL) 2 Cu 2 (l-NSC) 2 (NSC) 2 ] (1), (NiL, H 2 L = 2, 3-dioxo-5,6,14,15-dibenzo-1,4,8,12-tetraazacyclo-pentadeca-7,13-dien), have been synthesized and structurally characterized. The crystals crystallize in the triclinic system, space group P-1, for (1) a = 8.319 (3) Å , b = 10.434(4) Å , c = 14.166(5) Å , a = 107.030(5)°, b = 91.257(5)°, c = 107.623(5)°. The complex involved both bridging N, S-ligand, and oxamide ligand, C-HÁ Á ÁS interactions and NCS fi Ni weak coordination interactions making the complex superamolecular.