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Synthesis and Crystal Structure of Rare Earth Metal Chlorides Bearing Bridged‐Indenyl Ancillary Ligand
Author(s) -
Wang Yibin,
Feng Xiaoying,
Luo Yunjie,
Zhang Yong,
Liang Hongze
Publication year - 2011
Publication title -
chinese journal of chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.28
H-Index - 41
eISSN - 1614-7065
pISSN - 1001-604X
DOI - 10.1002/cjoc.201190077
Subject(s) - chemistry , ligand (biochemistry) , metal , crystal structure , salt metathesis reaction , yield (engineering) , nuclear magnetic resonance spectroscopy , molar ratio , medicinal chemistry , crystallography , stereochemistry , metathesis , polymerization , organic chemistry , catalysis , biochemistry , materials science , receptor , metallurgy , polymer
Two new rare earth metal chloride complexes supported by a bridged‐indenyl ancillary ligand, [C 9 H 6 SiMe 2 ‐ (CH 2 ) 2 SiMe 2 C 9 H 6 ]Ln(µ‐Cl) 2 Li(TMEDA) [Ln=Y ( 1 ), Lu ( 2 )], were synthesized via salt metathesis reaction. Reaction of C 9 H 7 SiMe 2 (CH 2 ) 2 SiMe 2 C 9 H 7 with 2 equiv. of n ‐butyllithium in hexane at room temperature afforded [C 9 H 6 SiMe 2 ‐ (CH 2 ) 2 SiMe 2 C 9 H 6 ]Li 2 as white powder in 95% isolated yield. Further treatment of [C 9 H 6 SiMe 2 (CH 2 ) 2 SiMe 2 ‐ C 9 H 6 ]Li 2 with anhydrous LnCl 3 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.