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Issue 32, 2009
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Measurements of relative chemical shift tensor orientations in solid-state NMR: new slow magic angle spinning dipolar recoupling experiments

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Abstract

Solid-state NMR experiments can be used to determine conformational parameters, such as interatomic distances and torsion angles. The latter can be obtained from measurements of the relative orientation of two chemical shift tensors, if the orientation of these with respect to the surrounding bonds is known. In this paper, a new rotor-synchronized magic angle spinning (MAS) dipolar correlation experiment is described which can be used in this way. Because the experiment requires slow MAS rates, a novel recoupling sequence, designed using symmetry principles, is incorporated into the mixing period. This recoupling sequence is based in turn on a new composite cyclic pulse referred to as COAST (for combined offset and anisotropy stabilization). The new COAST-C721 sequence is shown to give good theoretical and experimental recoupling efficiency, even when the CSA far exceeds the MAS rate. In this regime, previous recoupling sequences, such as POST-C721, exhibit poor recoupling performance. The effectiveness of the new method has been explored by a study of the dipeptideL-phenylalanyl-L-phenylalanine.

Graphical abstract: Measurements of relative chemical shift tensor orientations in solid-state NMR: new slow magic angle spinning dipolar recoupling experiments

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Article information


Submitted
03 Apr 2009
Accepted
06 Jul 2009
First published
15 Jul 2009

Phys. Chem. Chem. Phys., 2009,11, 6999-7007
Article type
Paper

Measurements of relative chemical shift tensor orientations in solid-state NMR: new slow magic angle spinning dipolar recoupling experiments

A. P. S. Jurd and J. J. Titman, Phys. Chem. Chem. Phys., 2009, 11, 6999
DOI: 10.1039/B906814G

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