Department of Chemistry, Zakir Husain College (University of Delhi), 1 .L.N. Marg. New Delhi- 110 002. India E-mail : schandra_00@yahoo.com Manuscript received 9 December 2002, revised 22 September 2003, accepted 3 May 2004 Complexes of transition metal ions with an azamacrocyclic ligand viz. 2,16-dimethyl-3,6,9,12,15,21-hexaaza-bicyclo[15.3.1]henicosa-1(21),2,15,17,19-pentacne (L1) have been prepared. All the complexes were found to have the composition ML1Cl2 (where M = MnII , CoII , NiII and CuII or M'L1Cl3 (where M' = Crlll and FeIII ). Molar conductance measurements of MnII , CoII and NiII complexes in DMSO correspond to 1 : 1 electrolytes, whereas ML1Cl3 and CuL1Cl2 are 1 : 2 electrolytes. Therefore complexes may be formulated as [ML1CI]CI, [ML1CI]Cl2 and [CuL1]Cl2. All the complexes wet·e characterized through elemental analyses, molar conductance and magnetic susceptibility measurements, IR, electronic and EPR spectral studies.