Chiral bis-alkoxysilanes are used as building blocks for the synthesis of new periodically ordered mesoporous organosilica materials (see figure). A bis-alkoxysilane molecule with a chiral group as a bridging organic ligand is prepared via enantioselective organometallic catalysis using a ruthenium catalyst with 2,2'-bis(diphenylphosphino)-1,1'-binaphthalene as a ligand. The synergistic co-assembly is then used to prepare a high-surface-area mesoporous material with an average pore size of about 3 nm.