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Synthesis and Crystal Structure of Rare Earth Metal Chlorides Bearing Bridged-Indenyl Ancillary Ligand
Authors:Wang Yibin  Feng Xiaoying  Luo Yunjie  Zhang Yong  Liang Hongze
Institution:1. Faculty of Materials Science & Chemical Engineering, Ningbo University, Ningbo, Zhejiang 315211, China;2. Organometallic Chemistry Laboratory, Ningbo Institute of Technology, Zhejiang University, Ningbo, Zhejiang 315100, China;3. School of Chemistry and Chemical Engineering, Suzhou University, Suzhou, Jiangsu 215123, China
Abstract:Two new rare earth metal chloride complexes supported by a bridged‐indenyl ancillary ligand, C9H6SiMe2‐ (CH2)2SiMe2C9H6]Ln(µ‐Cl)2Li(TMEDA) Ln=Y ( 1 ), Lu ( 2 )], were synthesized via salt metathesis reaction. Reaction of C9H7SiMe2(CH2)2SiMe2C9H7 with 2 equiv. of n‐butyllithium in hexane at room temperature afforded C9H6SiMe2‐ (CH2)2SiMe2C9H6]Li2 as white powder in 95% isolated yield. Further treatment of C9H6SiMe2(CH2)2SiMe2‐ 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 η5‐fashion, and two chlorine atoms to adopt a distorted tetrahedral geometry.
Keywords:rare earths  bridging ligands  synthesis  crystal structure
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