| Summary: | An intriguing but rare silicon-centered spirocyclic compound, spiro[5.5]octaferrocenylpentasiloxane (<b>4</b>) featuring silicon fused six-membered ferrocenyl-functionalized siloxane rings, has been obtained during the thermally induced transformation of triferrocenylsilane Fc<sub>3</sub>Si–H (<b>1</b>) into triferrocenylsilanol Fc<sub>3</sub>Si–OH (<b>2</b>), when N,N-dimethylformamide (DMF) was used as a solvent in the presence of the metal carbonyl Mo(CO)<sub>6</sub>. The unexpected formation of the maximally ferrocenyl substituted silicon centered spirocyclic <b>4</b> involves the obtention, and subsequent condensation, of different ferrocenylsilanol intermediates. Spirocyclic silicate <b>4</b> has been characterized using a combination of MALDI-TOF mass spectrometry, elemental analysis, and single crystal X-ray diffraction analysis.
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