This work describes the physico-chemical studies of metal complexes with N and S donor ligands. Emphasis has been given to the synthesis and characterization of polyazamacrocycles and dithiocarbamato complexes of transition metal ions and Sn(IV). They have been characterized by FT-IR, NMR (1H, 13C and 119Sn), mass spectrometry and X-ray crystallography. The synthesis of 14-membered hexaaza macrocyclic complexes of the type CuL]X2, CuL1]X2, CuL(N3)(ClO4).3/2O]n, CuL(N3)2] and CuL1(N3)(ClO4)]n was reported. The effect of anions on the gross geometry and chemical properties of the Cu(II)...