中华医学超声杂志

应用化学 ›› 1993, Vol. 0 ›› Issue (3): 80-82.

• 研究简报 • 上一篇    下一篇

[(t-BuCp)2GdCl]2的合成及晶体结构

宋社平, 金松春, 林永华, 沈琪   

  1. 中国科学院长春应用化学研究所稀土化学与物理开放实验室 130022 长春
  • 收稿日期:1992-04-20 修回日期:1992-06-24 出版日期:1993-06-10 发布日期:1993-06-10

SYNTHESIS AND CRYSTAL STRUCTURE OF [(t-BuCp)2GdCl]2

Song Shepin, Jin Songchun, Lin Yonghua, Shen Qi   

  1. Laboratory of Rare Earth Chemistry and Physics, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, 130022 Changchun
  • Received:1992-04-20 Revised:1992-06-24 Published:1993-06-10 Online:1993-06-10

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摘要： Wayda最近报道,无水氯化稀土LnCl3和叔丁基环戊二烯钠(t-BuCp)Na进行交换反应时,由于歧化反应得不到单取代或双取代的轻稀土氯化物衍生物,只能得到中稀土和重稀土氯化物衍生物,并且没有测得这些配合物的晶体结构。我们采用提高反应温度和延长反应时间,使交换反应进行完全,有效地避免了歧化反应的发生,成功地分离到了单取代或双取代的叔丁基环戊二烯基轻稀土氯化物。并测得(t-BuCp)2LnCl·nTHF(Ln=Pr,n=2;Ln=Yb,n=1)的分子结构。

关键词: 叔丁基环戊二烯, 钆有机配合物, 合成, 晶体结构

Abstract: The title complex [(t-BuCp)2GdCl]2 was synthesizedby reacting anhydrous GdCl3 with sodium tert-butylcyclopentadienide in THF. The complex was characterized by elemental analysis,infrared and 1H NMR spectroscopy. The crystal of the complex as determined by an X-ray diffraetometry belongs to orthorhombic with space group Cmca,unit cell parameters a=2.3397(3),b=0.9460 (5),c=1.6473(5)nm. V=3.646(2)nm2,Dc=1.58g/cm3,Z=4. The structure was refined by least-square technique to R=0.051 for 1027 observed reflections. The molecules exist as a chlorinebridged dimer,Gd-C1 0.2771 (3)nm with tert-butylcyclopentadienyl groups being bonded in a pentahepto-fashion.

Key words: tert-butylcyclopentadienyl, organogadolinium complex, synthesis, crystal structure

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