Reaktion von Bis(trimethylsilylamino)dichlorsilan mit Titantetrachlorid - Synthese und Kristallstruktur von [μ-ClTiCl2N(SiMe3)SiCl2NH2]2
作者:Stefan Rannabauer、Regina Bettenhausen、Wolfgang Schnick
DOI:10.1002/1521-3749(200202)628:2<373::aid-zaac373>3.0.co;2-2
日期:2002.2
TiCl4 reacts quantitatively with Cl2Si(NHSiMe3)2 in n-pentane under evolution of Me3SiCl yielding [μ-ClTiCl2N(SiMe3)-SiCl2NH2]2 (1), which is obtained as a yellow, crystalline solid forming small intergrown needles, that rapidly hydrolyse. The product 1 shows a thermal stability up to 80?C. The molecular structure of 1 has been solved by X-ray powder diffraction methods and it could be confirmed by
TiCl4 与正戊烷中的 Cl2Si(NHSiMe3)2 在 Me3SiCl 的演化下发生定量反应,生成 [μ-ClTiCl2N(SiMe3)-SiCl2NH2]2 (1),其为黄色结晶固体,形成小的共生针状体,可快速水解. 产品 1 显示出高达 80℃的热稳定性。1 的分子结构已经通过 X 射线粉末衍射法解析出来,并且可以通过在 -70 ℃下进行单晶 X 射线结构测定来证实。因此,在固体 1 中是二聚体 ([μ-ClTiCl2N(SiMe3)SiCl2NH2]2, P21/n (no. 14), Z = 2, a = 1504.89(6), b = 1296.33(6), c = 710.90(4) pm,β = 91.276(2)?)。