Homoleptic Trigonal Planar Lanthanide Complexes Stabilized by Superbulky Silylamide Ligands
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The lithium silylamides [Li(μ3-NHSiMe2But)]6 (1) and [Li(μ-NHSiPri3)(THF)]2 (2) were reacted with ClSiMe3, ClSiMe2But, or ClSiPri3 to prepare a series of secondary silylamines by salt metathesis reactions. These were deprotonated with KH to afford the group 1 transfer agents [K{μ-N(SiMe2But)(SiMe3)}(C7H8)]2 (3), [{K[μ-N(SiPri3)(SiMe3)]}2]∞ (4), [{K[μ-N(SiMe2But)2]}2(C7H8)]∞ (5), [K{N(SiPri3)(SiMe2But)}]∞ (6), [K{N(SiPri3)2}]∞ (7), and [K{N(SiPri3)2}(THF)3] (8). The synthetic utility of these group 1 transfer agents has been demonstrated by their reactions with [Ln(I)3(THF)4] (Ln = La, Ce) in various stoichiometries to yield heteroleptic [La{N(SiMe2But)(SiMe3)}2(μ-I)]2 (9) and homoleptic [Ln{N(SiMe2But)(SiMe3)}3] (Ln = La 10, Ce 11) and [La{N(SiMe2But)2}3] (12). The very bulky silylamide ligands described herein can impart unusual geometries to their lanthanide complexes. Complexes 10–12 remarkably exhibit approximate planarity in the solid state rather than the more common trigonal pyramidal shapes observed in previously reported neutral homoleptic lanthanide silylamide complexes. Complexes 1–12 have been variously characterized by X-ray crystallography, NMR spectroscopy, FTIR spectroscopy, and CHN microanalysis.
创建时间：
2015-12-17
