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Cross-correlated spin relaxation effects in methyl 1H CPMG-based relaxation dispersion experiments: Complications and a simple solution
Authors:Dmitry?M.?Korzhnev,Anthony?K.?Mittermaier,Lewis?E.?Kay  mailto:kay@pound.med.utoronto.ca"   title="  kay@pound.med.utoronto.ca"   itemprop="  email"   data-track="  click"   data-track-action="  Email author"   data-track-label="  "  >Email author
Affiliation:(1) Contribution from the Protein Engineering Network Centers of Excellence and the Departments of Medical Genetics, Biochemistry and Chemistry, The University of Toronto, Toronto, Ontario, Canada,, M5S 1A8
Abstract:
Artifacts associated with the measurement of methyl 1H single quantum CPMG-based relaxation dispersion profiles are described. These artifacts arise due to the combination of cross-correlated spin relaxation effects involving intra-methyl 1H–1H dipolar interactions and imperfections in 1H refocusing pulses that are applied during CPMG intervals that quantify the effects of chemical exchange on measured transverse relaxation rates. As a result substantial errors in extracted exchange parameters can be obtained. A simple lsquowork-aroundrsquo is presented where the 1H chemical shift difference between the exchanging states is extracted from a combination of 13C single quantum and 13C–1H multiple quantum dispersion profiles. The approach is demonstrated with an application to a folding/unfolding reaction involving a G48M mutant Fyn SH3 domain.
Keywords:cross-correlated spin relaxation  methyl groups  1H CPMG relaxation dispersion  1H–  13C multiple quantum coherence.
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