Heteronuclear local field NMR spectroscopy under fast magic-angle sample spinning conditions
The acquisition of bidimensional heteronuclear nuclear magnetic resonance local field spectra under moderately fast magic-angle spinning (MAS) conditions is discussed. It is shown both experimentally and with the aid of numerical simulations on multispin systems that when sufficiently fast MAS rates are employed, quantitative dipolar sideband patterns from directly bonded spin pairs can be acquired in the absence of (1)H-(1)H multiple-pulse homonuclear decoupling even for "real" organic solids. The MAS speeds involved are well within the range of commercially available systems (10-14 kHz) and provide sidebands with sufficient intensity to enable a reliable quantification of heteronuclear dipolar couplings from methine groups. Simulations and experiments show that useful information can be extracted in this manner even from more tightly coupled -CH(2)- moieties, although the agreement with the patterns simulated solely on the basis of heteronuclear interactions is not in this case as satisfactory as for methines. Preliminary applications of this simple approach to the analysis of molecular motions in solids are presented; characteristics and potential extensions of the method are also discussed. Copyright 2000 Academic Press.
McElheny
D
Department of Chemistry (M/C 111), University of Illinois at Chicago, 845 West Taylor Street, Chicago, Illinois, 60607-7061, USA.
DeVita
E
Frydman
L