The dioxomolybdenum(VI) fragment MoO2X2 has been confined within the ordere
d mesopores of pure siliceous hexagonal MCM-41 and cubic MCM-48 molecular s
ieves either by direct grafting (solvent impregnation) with MoO2X2(THF)(2)
or by using a spacer ligand [L = NC(CH2)(2)Si-(OEt)(3)]. The materials have
been characterised by elemental analysis, powder X-ray diffraction, N-2 ad
sorption, IR spectroscopy, and magic-angle spinning NMR spectroscopy (C-13,
Si-29). All catalysts, homogeneous and heterogenised, are active in the ep
oxidation of cyclooctene with tert-butyl hydroperoxide.