Mononuclear complexes of Zn(II) N,N’ coordinated with phendione and phendioxime andrnpolynuclear of Ni(II), Cu(II) and Zn(II) complexes of the phendioxime were synthesized andrncharacterized by direct method. The Ni(II), Cu(II) and Zn(II) species coordinated by N,N’ of thernoximate and phen groups. The Ni(II) complex of the oximate has square-planar geometry andrnthe phen has octahedral goemetry. And the Cu(II) and Zn(II) complexes of the oximate and thernphen have octahedral geometry. Mononuclear complex of Zn(II) with phendione N,N’rncoordinated was the precursor for mononuclear complex of Zn(II) with phedioxime N,N’rnoctahedral coordinated by the phen group and the hetronuclear complex of Ni(II) with thernmononuclear Zn-phendioxime complex was synthesized and characterized by template method.rnThe Zn(II) and Ni(II) species coordinated by N,N’ of the phen and oximate groups, respectively.rnThe Zn(II) moiety coordinated through N,N’ of the phen has octahedral geometry and the Ni(II)rnmoiety coordinated through N,N’ of the oximate has tetrahedral geometry. Structures of thernligand and its complex is proposed and formulated according to the elemental analysis, 1H, 13CrnNMR, UV-Vis and AAS, molar conductivity and magnetic susceptibility..rnKey words: phendione, phendioxime, phen and oximate.