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

Jörg Eppinger; Eberhardt Herdtweck; Reiner Anwander

doi:10.1016/S0277-5387(97)00506-8

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

Jörg Eppinger, Eberhardt Herdtweck, Reiner Anwander^*

^*Corresponding author for this work

Research output: Contribution to journal › Article › peer-review

50 Scopus citations

Abstract

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 ¹H, ¹³C and ²⁹Si 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°C in the orthorhombic space group Pnma with a = 5.4439(2) Å, b = 15.7268(9) Å, c = 10.9751(6) Å, V = 939.63(8) Å₃ and Z = 4. Least squares refinement of the model based on 873 reflections converged to a final ωR₂ = 0.1124.

Original language	English (US)
Pages (from-to)	1195-1201
Number of pages	7
Journal	Polyhedron
Volume	17
Issue number	7
DOIs	https://doi.org/10.1016/S0277-5387(97)00506-8
State	Published - 1998
Externally published	Yes

Keywords

Alkali metal
Bis(dimethylsilyl) amide
Laddering
Sodium
X-ray structure

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry
Materials Chemistry

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10.1016/S0277-5387(97)00506-8

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title = "Synthesis and characterisation of alkali metal bis(dimethylsilyl) amides: Infinite all-planar laddering in the unsolvated sodium derivative",

abstract = "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 1H, 13C and 29Si 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°C in the orthorhombic space group Pnma with a = 5.4439(2) {\AA}, b = 15.7268(9) {\AA}, c = 10.9751(6) {\AA}, V = 939.63(8) {\AA}3 and Z = 4. Least squares refinement of the model based on 873 reflections converged to a final ωR2 = 0.1124.",

keywords = "Alkali metal, Bis(dimethylsilyl) amide, Laddering, Sodium, X-ray structure",

author = "J{\"o}rg Eppinger and Eberhardt Herdtweck and Reiner Anwander",

year = "1998",

doi = "10.1016/S0277-5387(97)00506-8",

language = "English (US)",

volume = "17",

pages = "1195--1201",

journal = "Polyhedron",

issn = "0277-5387",

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TY - JOUR

T1 - Synthesis and characterisation of alkali metal bis(dimethylsilyl) amides

T2 - Infinite all-planar laddering in the unsolvated sodium derivative

AU - Eppinger, Jörg

AU - Herdtweck, Eberhardt

AU - Anwander, Reiner

PY - 1998

Y1 - 1998

N2 - 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 1H, 13C and 29Si 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°C in the orthorhombic space group Pnma with a = 5.4439(2) Å, b = 15.7268(9) Å, c = 10.9751(6) Å, V = 939.63(8) Å3 and Z = 4. Least squares refinement of the model based on 873 reflections converged to a final ωR2 = 0.1124.

AB - 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 1H, 13C and 29Si 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°C in the orthorhombic space group Pnma with a = 5.4439(2) Å, b = 15.7268(9) Å, c = 10.9751(6) Å, V = 939.63(8) Å3 and Z = 4. Least squares refinement of the model based on 873 reflections converged to a final ωR2 = 0.1124.

KW - Alkali metal

KW - Bis(dimethylsilyl) amide

KW - Laddering

KW - Sodium

KW - X-ray structure

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DO - 10.1016/S0277-5387(97)00506-8

M3 - Article

AN - SCOPUS:0000689305

SN - 0277-5387

VL - 17

SP - 1195

EP - 1201

JO - Polyhedron

JF - Polyhedron

IS - 7

ER -

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

Abstract

Keywords

ASJC Scopus subject areas

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