Experimental Aspects of Multidimensional Solid-State NMR Correlation Spectroscopy

Abstract

The experimental parameters critical for the implementation of multidimensional solid-state NMR experiments that incorporate heteronuclear spin exchange at the magic angle are discussed. This family of experiments is exemplified by the three-dimensional experiment that correlates the 1H chemical shift, 1H-15N dipolar coupling, and 15N chemical shift frequencies. The broadening effects of the homonuclear 1H-1H dipolar couplings are suppressed using flip-flop (phase- and frequency-switched) Lee-Goldburg irradiations in both the 1H chemical shift and the 1H-15N dipolar coupling dimensions. The experiments are illustrated using the 1H and 15N chemical shift and dipolar couplings in a single crystal of 15N-acetylleucine. © 1999 Academic Press.