In this communication, electrochemical and antimicrobial studies of tetraazamacrocyclic complexes [FeC42H32N4Cl2] [1a] and [CoC42H32N4Cl2] [1b] have been carried out. The spectral studies were conformed the octahedral geometry of these macrocyclic complexes. Cyclic voltammetric studies were carried out on Pt dish (0.031 cm2) electrode in DMF. These studies have shown one electron quasirreversible redox processes for these macrocyclic complexes on the basis of their peak separation (ΔE) and peak current ratio (ipa/ipc). Diffusion coefficient (D0) and heterogeneous electron transfer rate constant (K0) were also calculated with the help of Nicholson and Kochi’s method and found in the order K0 [1b] > K0 [1a]. Antimicrobial activity of these macrocyclic complexes was also tested against E. coli, P. aeruginosa, B. cereus, S. aureus and antifungal activity against C. albicans. The observed antimicrobial activity was compared with a standard drug, Gentamycin.