Transition metal complexes of the type ML.nH 2 O [Where M= Co(II),Ni(II),Cu(II) and Zn(II), L= Schiff base of 5 nitro salicylaldehyde and anthranalic acid , n= 0,1 …..] were characterized by using 1 H NMR ,TGA, Diffused refluctance and ESR spectroscopy. On the basis of above studies Co(II), Ni(II) shows tetrahedral structure, Cu(II) shows binuclear structure and Zn(II) shows square planar structure.