A novel heterodinucleating macrocyclic Zn(II)-Ni(II) complex was prepared by stepwise procedure. The prepared mono- and dinuclear macrocyclic complexes were characterized by elemental analysis, IR, NMR spectroscopies, and molar conductance measurements. Characterization results confirm the expected C2 symmetry geometry for mononuclear macrocyclic zinc complex with trans disposed pyridyl ligands. In contrast, the X-ray crystal structure of the macrocyclic Zn(II)-Ni(II) complex reveals a C1 symmetry geometry so that, Zn(II) ion is located in six coordination site with cis disposed pyridyl ligands and the penta-dantate compartment is occupied by the Ni(II) ion in a square pyramidal geometry. The thermogravimetric analysis (DTA/TG) of binuclear complex is also investigated.