Monometallic zinc(II) and nickel(II) complexes, [Zn(H 2 nsh)(H 2 O)] (1) and [Ni(H 2 nsh)(H 2 O) 2 ](2), have been synthesized in methanol by template method from bis(2-hydroxy-1-naphthaldehyde)succinoyldihydrazone (H 4 nsh). Reaction of monometallic complexes with alternate metal(II) acetates as a transmetallator in 1 : 3 molar ratio resulted in the formation of heterobimetallic complexes [NiZn(nsh)(A) 3 ] and [ZnNi(nsh)(A 0 ) 2 ] (A ¼ H 2 O (3), py (4), 2-pic (5), 3-pic (6), 4-pic (7)), (A 0 ¼ H 2 O (8), py (9), 2-pic (10), 3-pic (11), and 4-pic (12)). The complexes have been characterized by elemental analyzes, mass spectra, molar conductance, magnetic moments, electronic, EPR, and IR spectroscopies. All of the complexes are non-electrolytes. Monometallic zinc(II) is diamagnetic while monometallic nickel(II) complex and all heterobimetallic complexes are paramagnetic. The metal centers in heterobimetallic complexes are tethered by dihydrazone and naphthoxo bridging. Zinc(II) is square pyramidal; nickel(II) is six-coordinate distorted octahedral except [ZnNi(nsh)(A) 2 ], in which nickel(II) has square-pyramidal geometry. The displacement of metal center in monometallic complexes by metal ion has been observed in the resulting heterobimetallic complexes.