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Synthesis and Characterization of the First Bisand Tris[1‐(ω‐alken‐1‐yl)indenyl]lanthanide Complexes
Author(s) -
Schumann Herbert,
Karasiak Dirk F.,
Mühle Stefan H.
Publication year - 2000
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/(sici)1521-3749(200006)626:6<1434::aid-zaac1434>3.0.co;2-f
Subject(s) - chemistry , lanthanide , indene , medicinal chemistry , lutetium , lithium (medication) , lanthanum , tris , gadolinium , samarium , chloride , inorganic chemistry , yttrium , ion , organic chemistry , biochemistry , medicine , endocrinology , oxide
Abstract 1‐Allyl‐2,4,7‐trimethyl‐1 H‐indene ( 1 ) and 1‐(3‐buten‐1‐yl)‐4,7‐dimethyl‐1 H‐indene ( 2 ), which are to prepare from (2,4,7‐trimethylindenyl)lithium and allyl chloride or from (4,7‐dimethylindenyl)lithium and 4‐bromo‐1‐butene, react with n ‐butyllithium yielding (1‐allyl‐2,4,7‐trimethylindenyl)lithium [LiL ( 1 a )] or [1‐(3‐buten‐1‐yl)‐4,7‐dimethylindenyl]lithium [LiL′ ( 2 a )], respectively. The reactions of the trichlorides of gadolinium, erbium, yttrium, lutetium, and ytterbium with 1 a or 2 a (mole ratio 1 : 2) in THF produce the bis(indenyl)lanthanide chloride complexes L 2 LnCl(THF) [Ln = Gd ( 1 b ), Er ( 1 c )], L 2 ′ LnCl(THF) [Y ( 2 d ), Lu ( 2 e )], or L 2 ′ Yb(μ‐Cl) 2 Li(THF) 2 ( 2 f ), whereas the trichlorides of the comparatively large samarium and lanthanum ions react with different molar amounts of 2 a in THF exclusively with formation of the tris(indenyl) complexes L 3 ′ Sm ( 2 g ) or L 3 ′ La(μ‐Cl)Li(Et 2 O) 3 ( 2 h ), respectively. All new compounds were characterized by elemental analyses, mass spectrometry, and the diamagnetic compounds 2 d , 2 e and 2 h also by 1 H and 13 C{ 1 H}‐NMR spectroscopy. The single crystal X‐ray structural analyses of 1 c , 2 f , 2 g and 2 h demonstrate that the alkenyl groups of the indenyl side chains are not coordinated to the lanthanide atoms.