Journal of the American Chemical Society, Vol.119, No.23, 5390-5397, 1997
A Li-6-C-13 Redor Study of the Tmeda Complex of Solid Fluorenyllithium
The solid-state structure of the TMEDA complex of fluorenyllithium is investigated by the Li-6-C-13 REDOR NMR experiment. The REDOR experiment was performed on Li-6-enriched samples with detection of the natural abundance C-13-signal. This simplifies the interpretation of the data and also the sample preparation. The dipole-dipole couplings between the Li-6 cation and the C-13 nuclei, determined with the REDOR sequence, yields direct structural information. The distance information is also helpful when assigning the solid-state C-13 NMR spectrum. The position of the Li cation is determined to within +/-0.2 Angstrom (with respect to the fluorenyl framework).
Keywords:NUCLEAR-MAGNETIC-RESONANCE;ORGANO-LITHIUM COMPOUNDS;NMR-SPECTROSCOPY;ROTATING SOLIDS;STATE NMR;C-13;TEMPERATURE;COUPLINGS