Add time:08/01/2019         Source:sciencedirect.com

The reactions of (THF)3LiSi(SiMe3)3 with Me3GeCl, Ph3GeCl and GeCl4 give R3GeSi(SiMe3)3, RMe (75%), Ph (79%) and Cl (20%), respectively. The products, colorless, crystalline solids, unreactive toward air except for Cl3GeSi(SiMe3)3 which is hygroscopic and rapidly hydrolyzed, were characterized by elemental analyses, GC-MS and their 1H, 13C and 29Si NMR spectra. An X-ray structure determination established that crystals of Ph3GeSi(SiMe3)3 are monoclinic, C2/c, with a=17.102(6), b=9.997(3), c=37.368(9) Å, β=91.61(2)o, V=6386 Å3 and Z=8. Examination of the structural parameters revealed the presence of twisting distortions among the phenyl and trimethylsilyl substituents evidently relieving steric strain along the GeSi vector. Bond distances and angles predicted from force field calculations closely matched those determined by diffraction for the phenyl derivative. Calculations on Me3GeSi(SiMe3)3 and Cl3GeSi(SiMe3)3 confirmed the expectation that steric strain is minimal in those molecules. The reactions of (Me3Si)3SiSnCl3·THF and ((Me3Si)3Si)2SnCl2 with LiAlH4 in ether were investigated as a possible means to prepare silyltin(IV) hydrides. Despite use of a variety of conditions following those in published preparations of alkyltin(IV) hydrides, no silyltin hydrides were isolated. MNDO calculations indicated that decomposition of ((Me3)3Si)3SiSnH3 to ((Me3)3Si)SiH, Sn and H2 is thermodynamically favored.

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