12-membered and 14-membered pyridine based transition metal macrocyclic complexes [MIIL1Cl2], [MIIIL1Cl2]Cl, and [MIIL2Cl2], [MIIIL2Cl2]Cl, have been synthesized where L1= 5,6, 11,12-tetraphenyl-dipyrido[b, h]1,4,7,10- tetraazacyclododecane and L2 = 5,7,12,14-tetramethyl-dipyrido[b, i] 1,4,8,11-tetraazacyclotetradecane. MII= Ni (II), MIII = Fe (III). These complexes were characterized by UV-Vis, IR, Mass, TGA/DTA, microanalysis (C, H, and N). These complexes have been assigned saddle-shape nonplanar octahedral configurations on the basis of electronic spectral data. Redox behavior of these macrocyclic complexes were studied by cyclic voltammetric technique. The results suggest quasirreversible behavior of most of the redox processes. .