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. ...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.展开更多
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）.
文摘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.
