1,1'-(四甲基二硅)桥联双(四甲基环戊二烯基)二氯化钛的合成和结构

Synthesis and Structure of 1,1'-(Tetramethyldisilandiyl) Bis(tetramethylcyclopentadienyl) Titanium Dichloride

以1,2-二氯四甲基二硅烷与四甲基环戊二烯基锂反应,生成1,2-二(四甲基环戊二烯基)四甲基二硅烷(1).1经正丁基锂处理后与TiCl_4·2THF作用合成了标题化合物[Me_2Si]_2[η~5-C_5Me_4]_2TiCl_2(2),通过元素分析、UV、MS和~1H NMR谱表征了分子结构,并对其单晶进行了X射线衍射分析.该晶体属于单斜晶系,空间群C_2/c,晶胞参数:a=1.5060(3),b=0.9591(2),C=1.7490(3)nm;β=107.91(2)°,V=2.404(2)nm^3,Z=4,D_e=1.314g/cm^3,μ=6.80cm^(-1),F(000)=1008,R=0.047.

From the reaction of 1,2 - dichlorotetramethyldisilane with tetramethylcyclopenta -dienyl lithium, l,2-bis(tetramethylcyclopentadienyl) tetramethyldisilane(1) was formed. 1 wastreated with n -butyl lithium and followed by reacting with TiCl4 2THF, the title compound 2 was obtained. Its structure was characterized by elemental analysis, UV, MS,1H NMR spectra and determined by X - ray diffraction analysis. The crystal belongs to monoclinic, space groupC2/c. The parameters of the crystal are: a = 1.5060(3), b = 0.9591(2), c = 1.7490(3)nm; β= 107.91(2)°, V = 2.404(2)nm3, Z = 4, Dc = 1.314g/cm3, ,μ= 6.80cm-1 ,F(000)=1008,R = 0.047.