The present ternary complexes [Cu(ada)(phen)(H(2)O)]·2H(2)O (1), [Co(2)(ada)(2)(phen)(2)(H(2)O)(2)] (2) and [{Cu(ada)(3)(bipy)}(n)·3nH(2)O] (3) (H(2)ada=adipic acid, phen=1,10-phenanthroline and bipy=2,2'-bipyridine) obtained under varying experimental conditions were characterized by spectral, electrochemical and thermal studies. The bonding modes and the spatial arrangements of the carboxylate dianion around the metal ions have been investigated employing FTIR, EPR and X-ray crystallographic studies. Present data revealed a six coordinate distorted octahedral geometry for 2 with a=8.068, b=9.788, c=11.788Å, α=70.464, β=75.109, γ=72.063° and a five coordinate square pyramidal geometry for 3 with a=9.509, b=9.912, c=12.656Å, α=70.486, β=73.604, γ=75.162°. The superoxide dismutase (SOD) mimic activities of the complexes are in the order 132.