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Bis[citrato(3−)-O1,O3,O6]silicate: A Dianionic Complex with Hexacoordinate Silicon(IV) and Two Tridentate Dioato(2−)olato(1−) Ligands

2002; Wiley; Volume: 2002; Issue: 5 Linguagem: Inglês

10.1002/1099-0682(200205)2002

1099-0682

Reinhold Tacke, M. Penka, Friedrich Popp, Ingo Richter,

Synthetic Organic Chemistry Methods

Simple preparative methods for the synthesis of a hexacoordinate silicate dianion with two tridentate citrato(3−) ligands have been developed. Thus, treatment of tetramethoxysilane with two molar equivalents of citric acid and two molar equivalents of tri(n-butyl)amine in tetrahydrofuran yielded tri(n-butyl)ammonium bis[citrato(3−)-O1,O3,O6]silicate (10). Alternatively, 10 was prepared by treatment of tetrachlorosilane with two molar equivalents of citric acid and six molar equivalents of tri(n-butyl)amine in acetonitrile. Compound 10 was characterized by elemental analyses (C,H,N), solid-state 29Si VACP/MAS NMR studies, solution NMR experiments (1H, 13C; CD3CN), and a crystal structure analysis. (© Wiley-VCH Verlag GmbH, 69451 Weinheim, Germany, 2002)