摘要
在 THF中 ,通过三甲硅基环戊二烯基锂与四氯化锆反应合成了标题化合物 ,经元素分析 ,IR和 1 H NMR谱表征了其结构 ,并用 X-射线衍射测定了晶体结构 ,该晶体属于三斜晶系 ,空间群为 P1 ,晶体学参数 :a=0 .6787(6) ,b=1 .2 92 4 (2 ) ,c=1 .30 34(2 ) nm,α=67.83(1 ) ,β=82 .50 (3) ,γ=75.64 (3)°,V=1 .0 2 5nm3 ,Z=2 ,Dx=1 .41 5 g· cm-3 ,μ=8.989cm-1 ,F (0 0 0 ) =448,R=0 .0 32。质谱研究表明 ,化合物在质谱过程中发生二聚 C*p2 ZrClZr C*P2Cl(C*P=C5H4Si Me3 )。
The title compound was synthesized by the reaction of the lithium trimethylsi- lylcyclopentadienide with zirconium tetrachloride in THF.The structure was characterized by elemental analysis,IR and1 H NMR spectra.Furthermore,the crystal structure was de- termined by X- ray diffraction. The crystal belongs to space group P1of triclinic system. The cell parameters are a=0 .6 787(6 ) ,b=1.2 92 4 (2 ) ,c=1.30 34(2 ) nm,α=6 7.83(1) ,β= 82 .5 0 (3) ,γ=75 .6 4 (3)°,V=1.0 2 5 nm3 ,Z=2 ,Dx=1.4 15 g· cm-3 ,μ=8.989cm-1 ,F (0 0 0 ) =4 4 8,final R=0 .0 32 for 370 6 unique reflections [I≥ 3σ(I) ]. Molecular ion of the complex thatindicates a dimeric structure C* p2 Zr Cl Zr C* P 2 Cl (C*P=C5H4Si Me3 ) was found in the mass spectrum.
出处
《无机化学学报》
SCIE
CAS
CSCD
北大核心
1996年第1期55-60,共6页
Chinese Journal of Inorganic Chemistry
关键词
三甲硅基环戊二烯
锆
晶体结构
trimethylsilylcyclopentadiene zirconium crystal structure
