Paper
Synthesen und Kristallstrukturen von Bis(N-lithiumtrimethylsilylamino)-bis(dimethylamino)silan und 1,1-Dichloro-2,4-bis(trimethylsilylamino)-3,3-bis(dimethylamino)siladiazatitanac yclobutan
Published 2002 · Josef Engering, E. Peters, M. Jansen
Zeitschrift für Naturforschung. B, A journal of chemical sciences
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Abstract
Bis(N-lithio-trimethylsilylamino)bis(dimethylamino)silane (1) is formed in the reaction of silicon tetrachloride with excess hexamethyldisilazane, followed by halogen substitution using two equivalents of LiN(CH 3 ) 2 , andtreatment with two equivalents of n-butyllithium in hexane. 1, found to be dimeric in the solid state, was characterised by single crystal X-ray diffraction (monoclinic, C2/c, a = 1925.2(4), b = 1501.7(2), c = 1389.7(3) pm, β = 101.98(2), Z = 4, C 2 0 H 6 0 Lι 4 N 8 Si 6 ), and by solid state and solution NMR spectroscopy and mass spectrometry. Further reaction with titanium tetrachloride (molar ratio 1:1) yields orange crystals of the dimer [TiCl{(μ 2 -NSi(CH 3 ) 3 ) 2 Si(N(CH 3 ) 2 ) 2 }μ 2 -Cl] 2 (2) characterised by single crystal X-ray diffraction (triclinic, P1, a = 942.1(4), b = 991.7(4), c = 1222.6(5) pm, a = 90.12(1), β = 94.42(2), γ = 107.64(1)°, Z= 1, C 2 0 H 6 0 Cl 4 N 8 Si 6 Ti 2 ).
Bis(N-lithio-trimethylsilylamino)-bis(dimethylamino)silane (1) is a dimeric solid state compound with a strong reactivity towards n-butyllithium, and its crystal structure suggests that it may serve as a catalyst for the
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