Some new complexes of [NiL(PR3)] (where L = (E)-3-[(2-amino-5-nitrophenylimino) methyl)benzene-1,2-)diol) (L 1 ), (E)-4-((2-amino-5-nitrophenylimino)methyl)benzene-1,3-) diol) (L 2 ), R = Ph and Bu) containing tridentate NNO were synthesized and characterized by 1 H NMR, UV-Vis, FT-IR spectroscopic methods and elemental analysis. The geometry of [Ni(L 2 )(PBu 3 )] complex was determined by X-ray crystallography. It was indicated that the complex have a square planar structure and four coordinates in the solid state.