Experimental aspects of multidimensional solid-state NMR correlation spectroscopy.
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 (1)H chemical shift, (1)H-(15)N dipolar coupling, and (15)N chemical shift frequencies. The broadening effects of the homonuclear (1)H-(1)H dipolar couplings are suppressed using flip-flop (phase- and frequency-switched) Lee-Goldburg irradiations in both the (1)H chemical shift and the (1)H-(15)N dipolar coupling dimensions. The experiments are illustrated using the (1)H and (15)N chemical shift and dipolar couplings in a single crystal of (15)N-acetylleucine.
Ramamoorthy
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Department of Chemistry, University of Pennsylvania, Philadelphia, Pennsylvania 19104, USA.
Wu
C H
CH
Opella
S J
SJ
D006860:Hydrogen Bonding; D007930:Leucine / Q000031:analogs & derivatives / Q000737:chemistry; D009587:Nitrogen Isotopes; D019906:Nuclear Magnetic Resonance, Biomolecular / Q000379:methods*
D009587:Nitrogen Isotopes; D007930:Leucine; C088117:acetylleucine