Synthesis and characterisation of alkali metal bis(dimethylsilyl)amides: infinite all-planar laddering in the unsolvated sodinm derivative

被引:50
作者
Eppinger, J
Herdtweck, E
Anwander, R
机构
[1] Univ Stuttgart, Inst Tech Chem 1, D-70569 Stuttgart, Germany
[2] Tech Univ Munich, Inst Anorgan Chem, D-85747 Garching, Germany
关键词
alkali metal; bis(dimethylsilyl) amide; sodium; X-ray structure; laddering;
D O I
10.1016/S0277-5387(97)00506-8
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The synthesis of the bis(dimethylsilyl)amide complexes [MN(SiHMe2)(2)] (M = Li (1), Na (2), K (3)) was accomplished in high yield (>95%) by various standard procedures. Additionally, a novel trans-silylamination reaction has been applied to synthesize the sodium derivative 2. The alkali metal amide complexes which are readily soluble in aliphatic hydrocarbons were characterised by means of IR and H-1, C-13 and Si-29 NMR spectroscopy. A single crystal X-ray diffraction study of the sodium derivative 2 revealed the formation of an infinite, all-planar ladder structure. Compound 2 crystallizes from n-hexane at -35 degrees C in the orthorhombic space group Pnma with a = 5.4439(2) Angstrom, b = 15.7268(9) Angstrom, c = 10.9751(6) Angstrom, V = 939.63(8) Angstrom(3) and Z = 4. Least squares refinement of the model based on 873 reflections converged to a final omega R-2 = 0.1124. (C) 1998 Elsevier Science Ltd. All rights reserved.
引用
收藏
页码:1195 / 1201
页数:7
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