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化学学报
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化学学报 ›› 1992, Vol. 50 ›› Issue (10): 1024-1032. 上一篇    下一篇

研究论文

镧系金属有机配合物的研究,XL.双(2-甲氧乙基环戊二烯基)钇和镱的硼氢配合物的合成及晶体结构

邓道利;郑晓帆;钱长涛;金松春;林永华   

  1. 中国科学院上海有机化学研究所;中国科学院长春应用化学研究所
  • 发布日期:1992-10-15

Studies organolanthanide.XL.synthesis and X-ray structure of bis(2-methoxyethylcy-clopentadienyl) yttrium and ytterbium tetrahydroborates

DENG DAOLI;ZHENG XIAOFAN;QIAN CHANGTAO;JIN SONGCHUN;LIN YONGHUA   

  • Published:1992-10-15

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双(2-甲氧乙基环戊二烯基)氯化钇和镱, 在THF中, 室温与硼氢化钠发生置换反应, 生成双(2-甲氧乙基环戊二烯基)硼氢化钇(1)和镱(2), 产率分别为70和59%。它们都经红外光谱, 质谱, ^1HNMR和元素分析鉴定。将1和2在THF-己烷中重结晶,得到适用于X射线衍射分析的单品。1的空间群为Pna2~1, 晶胞参数:a=1.2390(3),b=1.1339(2), c=1.1919(2)nm, 晶胞体积,1.6745(6)nm^3,D~c=1.39g.cm^-3, z=4, R=0.061;2的空间群为Pna2~1, 晶胞参数:a=1.2399(6),b=1.1371(5),c=1.1897(2)nm, 晶胞体积, 1.6773(1)nm^3,Dc=1.72g.cm^-3, z=4, R=0.038, 1与2都是含有两个配位键(Ln-O)的双型的单体结构。

关键词: 晶体结构测定, 红外分光光度法, Ｘ射线衍射分析, 环戊二烯 P, 质子磁共振谱法, 钇络合物, 镱络合物, 硼烷类

Bis(2-methoxyethylcyclopentadienyl)yttrium and -ytterbium tetrahydroborates have been synthesized in good yields by the reaction of bis(2-methoxyethylcyclopentadienyl)lanthanide chlorides with sodium borohydride in THF at room temperature The title complexes were characterized by elemental analyses, MS, 1H NMR and IR spectra. The crystal structures of the title compounds have been determine by x-ray diffraction. The x-ray structures and IR reveal the bidentate yttrium and ytterbium tetrahydroborate complexes with the intramol. coordination bonds between lanthanide metal and ligand oxygen atoms.

Key words: CRYSTAL STRUCTURE DETERMINATION, INFRARED SPECTROPHOTOMETRY, X-RAY DIFFRACTION ANALYSIS, CYCLOPENTADIENE P, PROTON MAGNETIC RESONANCE SPECTROMETRY, YTTRIUM COMPLEX, YTTERBIUM COMPLEX, BORANES

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