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钛杂环化合物的合成及晶体结构研究

Syntheses and Crystal Structural Studies of Titanacyclic Compounds
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摘要 通过联苯直接锂化,然后与二氯二茂钛反应,合成了5,5—二茂钛芴(Ⅱ),对其进行了晶体结构研究。晶体Ⅱ属单斜晶系,空间群为P2_1/c,晶胞参数:a=16.531(3)A;b=13.223(7)A;c=22.632(5)A;β=87.85(3)°;V=4944.1A^3;Z=12;D_c=1.331g/cm^3;偏离因子R=0.073;结构测定表明:该分子内含有无张力的五园钛环,Ti—C(π键)=2.351~2.389A,Ti—C(σ键)=2.162或2.170A,C(11)—C(17)=79.7°,C_5H_5(质心)—Ti—C_5H_5(质心)=136.2°。另外,直接二锂化二笨醚或二苯砜,再与二氯二茂铁反应,分别得到新化合物的分子式为C_(22)H_(18)OTi·2CH_2Cl_2(Ⅴ)或C_(22)H_(18)SO_2Ti·2CH_2Cl_2(Ⅵ)。 Lithiation of biphenyl with n-butyllithium in the presence of TMEDAleads directly to the 2,2'-dilithio derivative (Ⅰ), in turn, which reactswith Cp_2TiCl_2 also to sythesize 5, 5-dicyclopentadienyl titanofluorene(Ⅱ).The crystal structure of Compound Ⅱ is reported in this paper. Thecrystal is monoclinic, space group P2_1/C. Its unit cell parameters are:a = 16.531(3)?; b = 13.223(7)?; c = 22.632(5)?; β= 87.85(3)°;V = 4944. 1?~3; Z = 12; D_c = 1.331g/cm^3; R = 0.073. The result indicats that themolecule has nontensional five-membered titanacycle, Ti—C(η~5) = 2.351—2.389?, Ti—C(σ) = 2. 161(7) or 2. 169(6)?, angle of C(11)—Ti—C(17) is79.7°, Cp_1 (centroid)—Ti—Cp_2 (centroid) = 136.2°. The directly dimetalationof diphenyl ether or diphenyl sulfone and then reactions with Cp_2 TiCl_2yielded two new titanacyclic compounds, Cp_2TiC_(12)H_8·2CH_2Cl_2(Ⅴ) andCp_2TiC_(12)H_8SO_2·CH_2Cl_2(Ⅵ).
机构地区 兰州大学化学系
出处 《兰州大学学报(自然科学版)》 CAS CSCD 北大核心 1991年第1期59-64,共6页 Journal of Lanzhou University(Natural Sciences)
关键词 钛杂环化合物 晶体结构 二茂钛芴 biphenyl synthesis crystal structure lithiation titanocene dichloride 5, 5-dicyclopentadienyl titanofluorene
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  • 1申华峰,高等学校化学学报,1988年,9卷,11期,1118页
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