Synthesis and Derivatives of Pentakis[(trimethylsilyl)oxy]antimony

Michael Baier, Peter Bissinger, Hubert Schmidbaur

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6 Scopus citations

Abstract

Pentakis[(trimethylsilyl)oxy]antimony(V) [Sb(OSiMe3)5; 1] is prepared from SbCl5 and 5 equiv of NaOSiMe3 in benzene or hexane solution. According to mass spectrometric and NMR spectroscopic data, 1 appears to be a monomer. It forms a pyridine adduct pyr·Sb(OSiMe3)5 (2), the crystal structure of which has been determined. The mononuclear complex has octahedrally coordinated antimony atoms. With an additional equivalent of NaOSiMe3, the antimonate complex Na[Sb(OSiMe3)6] (3) is formed, which crystallizes as a monoglyme adduct [Na(MeOCH2CH2OMe)] [Sb(OSiMe3)6] (3a). Partial hydrolysis of 3, or a direct synthesis using NaOSiMe3 and NaOH as reagents for SbCl5, leads to the crystalline dinuclear complex Na2-[Sb2(OH)2(OSiMe3)10], the structure of which has also been determined. It features two cubes with a common Na2O2 face and tetracoordinated sodium and hexacoordinated antimony atoms. The hydroxy groups are in bridgehead positions. NMR data suggest that the dimers dissociate in solution to give octahedral mononuclear complexes with the silyloxy groups in fixed eis and trans positions (4:1) relative to the OH groups.

Original languageEnglish
Pages (from-to)2208-2212
Number of pages5
JournalOrganometallics
Volume12
Issue number6
DOIs
StatePublished - 1993
Externally publishedYes

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