Bis(dichlorosilyl)methylamine-Synthesis, Crystal Structure, and Conformational Analysis in the Gas Phase

Holger Fleischer; Donald C. McKean; Simon Parsons; Michael Buhl

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Bis(dichlorosilyl)methylamine-Synthesis, Crystal Structure, and Conformational Analysis in the Gas Phase

机译：双（二氯甲硅烷基）甲胺的合成，晶体结构及气相构象分析

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A straightforward preparation has been found for bis(dichlorosilyl)methylamine, (SiHCl_2)_2NMe (1), involving reaction between H_2NMe and an excess of SiHCl_3, dissolved either in pentane or THF at 253 K. 1 and a side-product, 1,3.5-trichloro-2,4,6-trimethylcyclotrisilazane, (-SiHCl_NMe-)_3 (2), were identified by elemental analysis, mass spectrometry and ~1H-NMR-spectroscopy. Some physical, NMR- and IR spectroscopical properties of 1 were determined. The molecular and crystal structure of 1 was investigated by single crystal X-ray diffraction. Selected structural parameters: r(Si-N) 169.7(5), r(Si-Cl) 203.1(2)-204.4(2), r(C-N) 150.0(8) pm; a(SiNSi) 123.6(3), a(SiNC) 118.3(4)/118.0(4) deg. Ab initio force field data and infrared intensities were calculated for four conformers of 1. Comparison of the observed and calculated IR spectra favours the two structures found ab initio provided that their actual abundancies are different from those calculated.

机译：发现了一种简单的双（二氯甲硅烷基）甲胺（SiHCl_2）_2NMe（1）的制备方法，涉及H_2NMe与过量的HCl（3H）在253 K下溶于戊烷或THF的反应。1和副产物1，通过元素分析，质谱和〜1H-NMR光谱鉴定了3.5-三氯-2,4,6-三甲基环三硅氮烷（-SiHCl_NMe-）_ 3（2）。确定了1的一些物理，NMR和IR光谱性质。通过单晶X射线衍射研究了1的分子和晶体结构。选定的结构参数：r（Si-N）169.7（5），r（Si-Cl）203.1（2）-204.4（2），r（C-N）150.0（8）pm; a（SiNSi）123.6（3），a（SiNC）118.3（4）/118.0（4）度计算了四个构象数为1的从头算力场数据和红外强度。比较观察到的和计算出的红外光谱，从头开始发现的两个结构都对它们有利，条件是它们的实际丰度与所计算的不同。

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《Zeitschrift fur Anorganische und Allgemeine Chemie》 |1999年第2期|共8页
作者
Holger Fleischer; Donald C. McKean; Simon Parsons; Michael Buhl;
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中图分类化学;
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bis(dichlorosilyl)methylamine; crystal structure; infrared spectrum; force field-calculations;

机译：双（二氯甲硅烷基）甲胺;晶体结构;红外光谱;力场计算;

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1. Bis(dichlorosilyl)methylamine-Synthesis, Crystal Structure, and Conformational Analysis in the Gas Phase [J] . Holger Fleischer, Donald C. McKean, Simon Parsons, Zeitschrift fur Anorganische und Allgemeine Chemie . 1999,第2期

机译：双（二氯甲硅烷基）甲胺的合成，晶体结构及气相构象分析
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Bis(dichlorosilyl)methylamine-Synthesis, Crystal Structure, and Conformational Analysis in the Gas Phase

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