The synthesis of MCM-41 analogue mesoporous metallosilicates with high specific surfaces, containing the redox active metals Ti, V, Cr, Mn, Fe, or Co, from an aqueous gel, under reflux is described. Their X-ray diffractograms reveal a highly ordered array of the mesopores. A strong host-guest interaction between the incorporated template molecules and the pore walls, observed by C-13 n.m.r., indicates the incorporation of the metals, which is further evidenced by u.v.-vis and Si-29 n.m.r. spectroscopy. These mesoporous metallosilicates are active as catalysts for the liquid phase oxidation of cyclohexane with aqueous H2O2 or tert-butyl hydroperoxide. (C) Elsevier Science Inc. 1997.1841795408416