Two meso-dichlorophenyl substituted metallocorroles were synthesized and characterized as to their electrochemical and spectroelectrochemical properties in dichloromethane, benzonitrile, and pyridine containing 0.1 M tetra-n -butylammonium perchlorate (TBAP) as supporting electrolyte. The examined compounds are represented as (Cl 2 Ph) 3 CorFe IV Cl and (Cl 2 Ph) 3 CorMn IV Cl where (Cl 2 Ph) 3 Cor is the trianion of 5,10,15-tri(2,4-dichlorophenyl)corrole. Each metallocorrole was examined as to its catalytic activity for the electoreduction of dioxygen when coated on an edge-plane pyrolytic graphite electrode in 1.0 M HClO 4 . Cyclic voltammetry combined with linear sweep voltammetry at a rotating disk electrode (RDE) and a rotating ring disk electrode (RRDE) was utilized to evaluate the catalytic activity for the electroreduction of O 2 . The main O 2 reduction product is hydrogen peroxide under the given experimental conditions.