The addition of excess glycine ethyl ester to Co{(H2NCH2CH2)3N}(OSMe2)23+ in Me2SO leads to the symmetrical dimeric peroxo ion p,p - [Co( tren )(NH2CH2CO2Et)]2O24+ under mild conditions. The single-crystal X- ray structure of the perchlorate salt is described, and the mechanism for the dimer formation is considered.