Abstract
AbstractTris(tetramethylaluminate)s of the lanthanoids cerium (1), holmium (2), and erbium (3) were synthesized by treating lanthanoid amide complexes of the type [Ln(NMe2)3(LiCl)3] with an excess amount of AlMe3. These compounds were characterized by single‐crystal X‐ray diffraction, elemental analysis, and NMR spectroscopy. Paramagnetic NMR spectroscopic studies were undertaken to investigate the influence of the compounds on the solvent chemical shifts. NMR parameters for the 1H, 13C, and 27Al nuclei of all the reported lanthanoid tris(tetramethylaluminate)s were measured. The reactions of tris(tetramethylaluminate)s of samarium and holmium with an excess amount of tetrahydrofuran led to [LnMe2(thf)5][AlMe4] {Ln = Ho (4), Sm (5)}. NMR spectroscopic investigations of the paramagnetic holmium and samarium methyl compounds (i.e., 4, 5) as well as the known diamagnetic analogue [YMe2(thf)5][AlMe4] revealed methyl group exchange processes in solution.
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