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Structural Diversity of Lithium Neopentoxide Compounds

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posted on 13.10.2001, 00:00 by Timothy J. Boyle, Todd M. Alam, Kelly P. Peters, Mark A. Rodriguez
The reaction of LiN(SiMe3)2 with 1 equiv of HOCH2CMe3 (HONep) in toluene led to the formation of [Li(μ3-ONep)]8 (1). The complex adopts a novel dual-edge fused hexagon−square prismatic structure with a C2v axis of rotation that relates the top and bottom eight-membered rings. Substituting the noncoordinating solvent toluene for a Lewis basic solvent (THF or py) led to the isolation of compounds of the general formula [Li(μ3-ONep)]4(solv)3, where solv = THF (2) or py (3). The cube structures of 2 and 3 have one Li which is not solvated because of steric crowding of the ONep ligands. Multinuclear solid-state (6Li, 7Li, and 13C) MAS and solution-state (1H, 7Li, and 13C) NMR studies were undertaken to verify the identity of the bulk powder and to determine the solution behavior of these compounds.