A detailed study of the chemical structure of mesoporous silica catalysts containing rhodium ligands and nanoparticles (RhP-MSN) was carried out by multi-dimensional solid-state NMR techniques. The degree of functionalization of the rhodium-phosphinosilyl complex to the surface of the RhP-MSN channels was determined by (29)Si NMR experiments. The structural assignments of the rhodium-phosphinosilyl complex were unambiguously determined by employing the novel, indirectly detected heteronuclear correlation ((13)C-(1)H and (31)P-(1)H idHETCOR) techniques, which indicated that oxidation of the attached phosphinosilyl groups and detachment of Rh was enhanced upon syngas conversion.
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