Tris(trimethylsilyl)stannyl alkali derivatives: Syntheses and NMR spectroscopic properties

被引：30

作者：

Fischer, R ^{[1
]}

Baumgartner, J ^{[1
]}

Marschner, C ^{[1
]}

Uhlig, F ^{[1
]}

机构：

[1] Graz Tech Univ, Inst Anorgan Chem, A-8010 Graz, Austria

来源：

INORGANICA CHIMICA ACTA | 2005年 / 358卷 / 11期

基金：

奥地利科学基金会;

关键词：

X-ray crystal structures; NMR spectroscopy; alkali stannides; preparation;

D O I：

10.1016/j.ica.2005.04.006

中图分类号：

O61 [无机化学];

学科分类号：

070301 ; 081704 ;

摘要：

Starting from tetrakis(trimethylsilyl)stannane, the tris(trimethylsilyl)stannyl alkali derivatives (Me3Si)(3)SnM, (M = Li, Na, K, Rb, Cs) were prepared in excellent yields. Reaction with MgBr2 (.) Et2O afforded bis[tris(trimethylsilyl)stannyl]magnesium. Reaction products were investigated by means of multinuclear NMR spectroscopy. At low temperatures, coupling of Li-7 and Sn-119 between [(Me3Si)(3)Sn](-) and [Li (.) 3THF](+) (337 Hz) or [Li (.) 12Cr4](+) (275 Hz), was observed. NMR chemical shifts and coupling constants of the stannyl anions exhibit a strong dependency on the nature of the cation, solvent system, concentration and temperature. In addition, the molecular structure of tris(trimethylsilyl)stannyl sodium (.) 15Cr5 was determined by X-ray crystallography. The [Na (.) 15Cr5](+) and [(Me3Si)(3)Sn](-) units are joined by a direct Sn-Na contact, 3.0775(18) angstrom in length. (c) 2005 Elsevier B.V. All rights reserved.

引用

页码：3174 / 3182

页数：9

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