ansa-Metallocenes with a Ph2Si bridge: molecular structures of HfCl2[Ph2Si(η5-C13H8)(η5-C5H4)] and HfCl2[Ph2Si(C13H9)(η5-C5H4)]2†
作者:Vyacheslav V. Izmer、Anton Y. Agarkov、Valentina M. Nosova、Lyudmila G. Kuz’mina、Judith A. K. Howard、Irina P. Beletskaya、Alexander Z. Voskoboynikov
DOI:10.1039/b009280k
日期:——
A mixture of rac- and meso-HfCl2[Ph2Si(η5-C9H6)2] was synthesized by treatment of HfCl4 with the dilithium salt of di(1H-inden-1-yl)diphenylsilane. These complexes were isolated after fractional crystallization in 15.5 and 8.5% yields, respectively. A sterically strained ansa complex HfCl2[Ph2Si(η5-C13H8)(η5-C5H4)] was synthesized in 62% yield by treatment of HfCl4 with the dilithium salt of cyclopentadienyl(fluoren-9-yl)diphenylsilane. Both this compound, and the by-product of reaction, HfCl2[Ph2Si(C13H9)(η5-C5H4)]2, were characterized by crystal structure analysis.
通过将HfCl4与二(1H-茚-1-基)二苯基硅烷的双锂盐反应,合成了rac-和meso-HfCl2[Ph2Si(η5-C9H6)2]的混合物。这些络合物经过分级结晶分别以15.5%和8.5%的产率被分离出来。通过将HfCl4与环戊二烯(氟烯-9-基)二苯基硅烷的双锂盐反应,合成了一种立体受压的ansa络合物HfCl2[Ph2Si(η5-C13H8)(η5-C5H4)],产率为62%。该化合物及其反应副产物HfCl2[Ph2Si(C13H9)(η5-C5H4)]2通过晶体结构分析进行了表征。