1H-detected 1H-1H correlation spectroscopy of a stereo-array isotope labeled amino acid under fast magic-angle spinning

The combined use of selective deuteration, stereo-array isotope labeling (SAIL), and fast magic-angle spinning effectively suppresses the H-1-H-1 dipolar couplings in organic solids. This method provided the high-field H-1 NMR linewidths comparable to those achieved by combined rotation and multiple-pulse spectroscopy. This technique was applied to two-dimensional H-1-detected H-1-H-1 polarization transfer CHH experiments of valine. The signal sensitivity for the H-1-detected CHH experiments was greater than that for the C-13-detected H-1-H-1 polarization transfer experiments by a factor of 2-4. We obtained the H-1-H-1 distances in SAIL valine by CHH experiments with an accuracy of about 0.2 angstrom by using a theory developed for H-1-H-1 polarization transfer in C-13-labeled organic compounds. (C) 2010 Elsevier Inc. All rights reserved.