Publication year: 2011 Source: Journal of Magnetic Resonance, Available online 22 September 2011
Bingwu*Yu, Hugo*van Ingen, Subramanian*Vivekanandan, Christoph*Rademacher, Scott E.*Norris, ...
Jcouplings are essential for measuring RDCs (residual dipolar couplings), now routinely used to deduce molecular structure and dynamics of glycans and proteins. Accurate measurement ofJCHis critical for RDCs to reflect the true structure and dynamics in the molecule of interest. We report noticeable discrepancies betweenJCHvalues measured with HSQC type pulse sequences in theH dimension from those measured in theC dimension for seventeen sugars and show that these discrepancies arise from strong scalar coupling. In order to determine how to minimize errors in measuringJCH, we analyze the strong coupling effects in detail using the product operator-formalism and spectral simulations based on the solution of the Liouville equation (not considering relaxation effects) in the presence of strong coupling. We report that the apparentJCHmeasured with 2D HSQC-based sequences in either dimension can be in error by up to 4 Hz and that the values measured in theH dimension can disagree with those in theC dimension by up to 7 Hz. We demonstrate that spectral simulations can reproduce the errors induced by strong coupling and that these can be used to extract trueJCHvalues. We find that theJCHvalues measured using a modified Z-filtered coupled HSQC are still affected by strong coupling. We conclude that spectral simulation yields accurateJCHwith errors as low as 1% in the presence of strong coupling. Graphical abstract
Highlights
? One-bond heteronuclear C-H couplings and RDCs may contain systematic ? errors.HH strong coupling causes these errors, which distort peak position. ? The errors are found in both 1H and 13C dimensions of a 2D HSQC. ? The errors are not due to digital resolution. ? Accurate coupling constants and RDCs should be obtained from simulations.
Identifying Guanosine Self Assembly at Natural Isotopic Abundance by High-Resolution 1H and 13C Solid-State NMR Spectroscopy
Identifying Guanosine Self Assembly at Natural Isotopic Abundance by High-Resolution 1H and 13C Solid-State NMR Spectroscopy
Amy L. Webber, Stefano Masiero, Silvia Pieraccini, Jonathan C. Burley, Andrew S. Tatton, Dinu Iuga, Tran N. Pham, Gian Piero Spada and Steven P. Brown
http://pubs.acs.org/appl/literatum/publisher/achs/journals/content/jacsat/0/jacsat.ahead-of-print/ja206516u/aop/images/medium/ja-2011-06516u_0007.gif
Journal of the American Chemical Society
DOI: 10.1021/ja206516u
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More AccurateJCHCoupling Measurement in the Presence ofJHHStrong Coupling in Natural Abundance
Linear Mode
