D. Mcelheny et al., Heteronuclear local field NMR spectroscopy under fast magic-angle sample spinning conditions, J MAGN RES, 143(2), 2000, pp. 321-328
The acquisition of bidimensional heteronuclear nuclear magnetic resonance l
ocal field spectra under moderately fast magic-angle spinning (MAS) conditi
ons is discussed. It is shown both experimentally and with the aid of numer
ical 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 H-1-H-1 multiple-pulse homonuc
lear decoupling even for "real" organic solids. The MAS speeds involved are
web within the range of commercially available systems (10-14 kHz) and pro
vide sidebands with sufficient intensity to enable a reliable quantificatio
n of heteronuclear dipolar couplings from methine groups. Simulations and e
xperiments show that useful information can be extracted in this manner eve
n from more tightly coupled -CH2- moieties, although the agreement with the
patterns simulated solely on the basis of heteronuclear interactions is no
t in this case as satisfactory as for methines, Preliminary applications of
this simple approach to the analysis of molecular motions in solids are pr
esented; characteristics and potential extensions of the method are also di
scussed. (C) 2000 Academic Press.