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Synthesis and Structures of Bis(tetramethylipiperidino)aluminum Halides‐X‐ray Crystal Structures of tmp 2 AlX (X = Cl, Br, I) and [tmp 2 A1(μ‐F)l 2
Author(s) -
Krossing Ingo,
Nöth Heinrich,
Tacke Christiane,
Schmidt Martin,
Schwenk Holger
Publication year - 1997
Publication title -
chemische berichte
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 0009-2940
DOI - 10.1002/cber.19971300805
Subject(s) - chemistry , crystal structure , dimer , hexane , halide , ether , nuclear magnetic resonance spectroscopy , crystallography , diethyl ether , x ray crystallography , yield (engineering) , medicinal chemistry , stereochemistry , inorganic chemistry , organic chemistry , physics , materials science , diffraction , optics , metallurgy
N‐Lithio‐2,2,6,6‐tetramethylpiperidine [Li(tmp)] reacts with AlX 3 (X = Cl, Br) in diethyl ether/ n‐hexane solution to generate the products of substitution and ether cleavage, [tmpAl(X)(μ‐OEt)], ( la , X = Cl; 1b , X = Br). However, when the reaction is allowed to proceed in n‐hexane alone, an almost quantitative yield of compounds tmp 2 AlX ( 2a , X = Cl; 2b , X = Br; 2c , X = I) is obtained. According to 27 AI‐NMR spectroscopy, mass spectroscopy, cryoscopy, and X‐ray crystal structure determinations, these compounds are monomeric in the solid state, in solution, and in the gas phase. 2b reacts with AgBF 4 yielding the fluoride‐bridged dimer (tmp 2 AlF), 2d , as shown by X‐ray crystal structure determination.