Two isomers of the dinuclear complex with beta-alanyl-L-aspartate (beta-ad), glycinate (gly), and ethylenediamine (en), [Co(beta-ad)Co(gly)(en)(mu-OH)(2)](+), were prepared by treating an aqueous solution containing [Co(beta-ad)(OH2)(2)] and [Co(gly)(en)(OH2)(2)](2+) under basic conditions. The geometrical structures and absolute configurations of these isomers were assigned on the basis of the NMR, UV, and CD spectral data; the assignments were confirmed on the basis of the spectral data of the mononuclear species that were obtained by the acid hydrolysis of the isomers. The faster eluted isomer (eluted with H2O on an SP-Sephadex (K+ form) column) consists of [Co(beta-ad)(mu-OH)(2)] (beta-ad coordinates to cobalt(III) as a tetradentate) and Delta-fac(O)-[Co(gly)(en)(mu-OH)(2)] moieties, and the later consists of [Co(beta-ad)(mu-OH)(2)] and Lambda-fac(O)-[Co(gly)(en)(mu-OH)(2)]. Another di-mu-hydroxo-dicobalt(III) complex containing beta-alanyl-L-histidinate (car), [Co-2(car)(2)(mu-OH)(2)], was also prepared by treating an aqueous solution containing [Co(car)(OH2)(2)](+) under basic conditions. The dinuclear structures of these complexes are stable for several days in the neutral aqueous solutions.