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Due to the steric demands of the ligands they display distorted trigonal\u2010bipyramidal structures in the solid state, as shown by X\u2010ray crystallography, with the O<jats:sup>\u2212<\/jats:sup> moiety binding to the Lewis acidic Re atom and the Re\u2010bound methyl group being located either in <jats:italic>cis<\/jats:italic> or <jats:italic>trans<\/jats:italic> position to the Schiff base. In solution, however, the steric differences seem not to be maintained, as can be deduced from <jats:sup>17<\/jats:sup>O NMR spectroscopy. Furthermore, the Schiff\u2010base ligands exchange with donor ligands. Nevertheless, the catalytic behaviour is influenced significantly by the Schiff bases coordinated to the MTO moiety, which lead either to high selectivities and good activities or to catalyst decomposition. 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