New mononuclear iron(III), cobalt(II) and nickel(II) macrocyclic complexes of the general formulae [M(L)X 2 ] [where M=Co(II) and Ni(II)] and [Fe(L)X 2 ]X [L=5,9-dioxo-3,4,7,10,11,17-hexaaza-2,11,13,15,1(17)-N-pentadienebicyclo[3,11,1 1,13 ]heptadecane; X=Cl, NO 3 , OAc or 0.5 SO 4 ] were synthesized. The complexes were characterized on the basis of elemental analyses, atomic absorption, magnetic moment measurements, UV -Vis and infrared spectral studies. All the complexes were found to have octahedral geometry.