摘要
以1,3-二氯六甲基三硅烷相继与环戊二烯基钠、正丁基锂和四氯化钛作用合成了1,1′-(六甲基三硅撑)双环戊二烯基二氯化钛(1),1在氨基钠的存在下与对氯苯酚作用制得题目化合物(2).通过元素分析、~1H NMR 和 MS 鉴定了1与2的结构,并对2进行 X 射线结构分析确证了其结构.2的晶体属单斜晶系的 P2_1/c 空间群.晶胞参数:a=1.0746(3),b=2.4865(7),c=1.2568(2)nm;β=113.42(2)°;V=3.08137nm^3;Z=4,D_σ(?)=1.305g·cm^(-3).化合物中三个硅原子的桥链发生明显扭曲.通过氧原子中心原子钛与苯环发生共轭,使整个分子形成共轭体系.
1.1’-[Hexamethyltrisilandiyl]-dicyclopentadienyl titanium dichloride(1)wasobtained from the reaction of 1,3-dichlorohexamethyl trisilane with cyclopentadienylsodium,n-butyl lithium and titanium tetrachloride in series in one pot.In the presenceof sodium amide 1 reacts with p-chlorophonol to yield the title compound 2.The structureof 2 was characterized by elemental analysis,~1H NMR,MS and confirmed by X-raydiffraction method.The crystal is monoclinic,space group P2_1/c.The parameters ofcrystal cell are:a=1.0746(3),b=2.4865(7),c=1.2568(2)nm;β=113.42(2)°;V=3.08137nm^3,Z=4,D_c=1.305 g·cm^(-3).The final R factor is 0.062.The dihedral angle oftwo Cp rings is 47.97°.The bridge silicone chain was twisted to accomondate thecondition for coordination.In the molecule of 2 titanium conjugates with benzene ringvia oxygen.
出处
《化学学报》
SCIE
CAS
CSCD
北大核心
1991年第8期751-756,共6页
Acta Chimica Sinica
