Proton to carbon-13 INEPT in solid-state NMR spectroscopy.
A refocused INEPT through-bond coherence transfer technique is demonstrated for NMR of rigid organic solids and is shown to provide a valuable building block for the development of NMR correlation experiments in biological solids. The use of efficient proton homonuclear dipolar decoupling in combination with a direct spectral optimization procedure provides minimization of the transverse dephasing of coherences and leads to very efficient through-bond (1)H-(13)C INEPT transfer for crystalline organic compounds. Application of this technique to 2D heteronuclear correlation spectroscopy leads to up to a factor of 3 increase in sensitivity for a carbon-13 enriched sample in comparison to standard through-bond experiments and provides excellent selectivity for one-bond transfer. The method is demonstrated on a microcrystalline sample of the protein Crh (2 x 10.4 kDa).
Elena
Bénédicte
B
Laboratoire de Chimie (UMR 5182 CNRS/ENS), Ecole Normale Supérieure de Lyon, 69364 Lyon, France.
Lesage
Anne
A
Steuernagel
Stefan
S
Böckmann
Anja
A
Emsley
Lyndon
L