The preparation of high active hydrodesulfurization catalysts is described. The procedure is based on the synthesis of labile bimetallic Co-Mo complexes in aqueous solution followed by the deposition on alumina surface at the conditions providing the structure of precursor remains unaltered after the drying. The prepared oxide surface compounds contain cobalt in the immediate vicinity of molybdenum that provides the selective formation of bimetallic sulfide compounds during the sulfidation. These compounds reveal the high activity in hydrotreatment of diesel fuels. (C) 2009 Elsevier B.V. All rights reserved.