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Synthesis and Crystal Structure of Rare Earth Metal Chlorides Bearing Bridged-lndenyl Ancillary Ligand

Synthesis and Crystal Structure of Rare Earth Metal Chlorides Bearing Bridged-lndenyl Ancillary Ligand
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摘要 Two new rare earth metal chloride complexes supported by a bridged-indenyl ancillary ligand, [C9H6SiMe2- (CH2)2SiMeEC9H6]Ln(u-Cl)2Li(TMEDA) [Ln=Y (1), Lu (2)], were synthesized via salt metathesis reaction. Reaction of C9H7SiMeE(CH2)ESiMeEC9H7 with 2 equiv, of n-butyllithium in hexane at room temperature afforded [C9H6SiMe2- (CHE)2SiMeEC9H6]Li2 as white powder in 95% isolated yield. Further treatment of [C9H6SiMe2(CHE)2SiMeE- C9H6]Li2 with anhydrous LnCl3 in 1 : 1 molar ratio in THF/TMEDA at room temperature provided the bridged-indenyl rare earth metal chlorides 1 and 2 in 86%--89% isolated yields. Both complexes were characterized by FT-IR spectroscopy, NMR spectroscopy, elemental analysis, and X-ray single crystal structure analysis. The central metals in both complexes are eight-coordinated by two indenyl ligands in η^5-fashion, and two chlorine atoms to adopt a distorted tetrahedral geometry. Two new rare earth metal chloride complexes supported by a bridged-indenyl ancillary ligand, [C9H6SiMe2- (CH2)2SiMeEC9H6]Ln(u-Cl)2Li(TMEDA) [Ln=Y (1), Lu (2)], were synthesized via salt metathesis reaction. Reaction of C9H7SiMeE(CH2)ESiMeEC9H7 with 2 equiv, of n-butyllithium in hexane at room temperature afforded [C9H6SiMe2- (CHE)2SiMeEC9H6]Li2 as white powder in 95% isolated yield. Further treatment of [C9H6SiMe2(CHE)2SiMeE- C9H6]Li2 with anhydrous LnCl3 in 1 : 1 molar ratio in THF/TMEDA at room temperature provided the bridged-indenyl rare earth metal chlorides 1 and 2 in 86%--89% isolated yields. Both complexes were characterized by FT-IR spectroscopy, NMR spectroscopy, elemental analysis, and X-ray single crystal structure analysis. The central metals in both complexes are eight-coordinated by two indenyl ligands in η^5-fashion, and two chlorine atoms to adopt a distorted tetrahedral geometry.
出处 《Chinese Journal of Chemistry》 SCIE CAS CSCD 2011年第2期273-277,共5页 中国化学(英文版)
基金 Project supported by Zhejiang Provincial Natural Science Foundation (No. Y4090617), State Key Laboratory of Polymer Physics and Chemistry (No. 200902) and Key Laboratory of Organic Synthesis of Jiangsu Province (No. KJS0907).
关键词 rare earths bridging ligands SYNTHESIS crystal structure rare earths, bridging ligands, synthesis, crystal structure
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