高等学校化学学报 ›› 2003, Vol. 24 ›› Issue (6): 973.

• 论文 • 上一篇    下一篇

二(四氢糠基茚)稀土氯化物的合成及晶体结构

程建华1, 崔冬梅1,2, 陈文启1, 胡宁海1, 唐涛1, 黄葆同1   

  1. 1. 中国科学院长春应用化学研究所高分子物理与化学国家重点实验室, 长春 130022;
    2. 长春工业大学化工系, 长春 130012
  • 收稿日期:2002-04-16 出版日期:2003-06-24 发布日期:2003-06-24
  • 通讯作者: 唐涛(1963年出生),男,博士,研究员,主要从事多相聚合物材料、烯烃聚合与催化剂及纳米材料的研究.E-mail:ttang@ns.ciac.jl.cn E-mail:ttang@ns.ciac.jl.cn
  • 基金资助:

    国家科技部“九七三”项目(批准号:1999064801)资助

Synthesis and Crystal Structure of Bis(tetrahydrofurfurylindenyl) Lanthanide Chlorides

CHENG Jian-Hua1, CUI Dong-Mei1,2, CHEN Wen-Qi1, HU Ning-Hai1, TANG Tao1, HUANG Bao-Tong1   

  1. 1. State Key Laboratory of Polymer Physics and Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022, China;
    2. Department of Chemical Engineering, Changchun University of Technology, Changchun 130012, China
  • Received:2002-04-16 Online:2003-06-24 Published:2003-06-24

摘要: 将四氢糠基茚锂分别与无水三氯化钇和无水三氯化钆以摩尔比2;1反应,除去不溶物和溶剂后,将产物在甲苯/THF中冷冻得到晶体(C4H7OCH2C9H6)2LnCl[Ln=Y(1);Ln=Gd(2)].这两种配合物都是单分子无溶剂化合物,在空气中稳定.配合物1和2的晶体结构都属于正交晶系,P212121空间群,晶胞参数分别为a=1.04252(9)nm,b=1.47455(12)nm,c=1.49799(13)nm,Z=4,Dc=1.508g/cm3;a=1.03701(10)nm,b=1.47233(12)nm,c=1.51354(14)nm,Z=4,Dc=1.699g/cm3.它们的结构相似,但空间构象不同.稀土中心离子分别与两个茚中的五元环和两个氧原子及氯原子成键,形成九配位结构.

关键词: 四氢糠基茚, 稀土配合物, 晶体结构, 合成

Abstract: Lanthanocene chlorides (C4H7OCH2C9H6)2 LnCl[Ln=Y(1); Ln=Gd(2)] were synthesized by the reaction of tetrahydrofurfurylindenyl lithium(in situ) with corresponding anhydrous lanthanide chorides in THF. The crystal structures of these two complexes were determined by X-ray diffraction and they were unsolvated monomeric complexes. They were stable in the air for several hours. Complexes 1 and 2 belong to the same crystal system(orthorhombic) and space group(P212121). The unit cell dimensions of complex 1 were a=1.042 52(9) nm, b=1.474 55(12) nm, c=1.497 99(13) nm, Z=4, D c=1.508g/cm3; The unit cell dimensions of complex 2 were a=1.037 01(10) nm, b= 1.472 33(12) nm, c=1.513 54(14) nm, Z=4, D c=1.699 g/cm3. They have the same structure and different space configurations. The central metal atom is coordinated by two indenyl, two oxygen of the tetrahydrofurfuryl and one chlorine atom to form a distorted trigonal bipyramid.

Key words: Tetrahydrofurfurylindenyl, Rare earth complex, Crystal structure, Synthesis

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