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Compensated second-order recoupling : application to third spin assisted recoupling
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Giffard, Mathilde, Hediger, Sabine, Lewandowski, Józef R., Bardet, Michel, Simorre, Jean-Pierre, Griffin, Robert G. and De Paëpe, Gaël (2012) Compensated second-order recoupling : application to third spin assisted recoupling. Physical Chemistry Chemical Physics, Vol.14 (No.20). pp. 7246-7255. doi:10.1039/c2cp40406k ISSN 1463-9076.
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Official URL: http://dx.doi.org/10.1039/c2cp40406k
Abstract
We consider the effect of phase shifts in the context of second-order recoupling techniques in solid-state NMR. Notably we highlight conditions leading to significant improvements for the Third Spin Assisted Recoupling (TSAR) mechanism and demonstrate the benefits of resulting techniques for detecting long-distance transfer in biomolecular systems. The modified pulse sequences of PAR and PAIN-CP, Phase-Shifted Proton Assisted Recoupling (AH-PS-PAR) and Phase-Shifted Proton-Assisted Insensitive Nuclei Cross Polarization (ABH-PS-PAIN-CP), still rely on cross terms between heteronuclear dipolar couplings involving assisting protons that mediate zero-quantum polarization transfer between low-γ nuclei ( 13C- 13C, 15N- 15N, 15N- 13C polarization transfer). Using Average Hamiltonian Theory we show that phase inversion compensates off-resonance contributions and yields improved polarization transfer as well as substantial broadening of the matching conditions. PS-TSAR greatly improves on the standard TSAR based methods because it alleviates their sensitivity to precise RF settings which significantly enhances robustness of the experiments. We demonstrate these new methods on a 19.6 kDa protein (U-[ 15N, 13C]-YajG) at high magnetic fields (up to 900 MHz 1H frequency) and fast sample spinning (up to 65 kHz MAS frequency). © 2012 the Owner Societies.
| Item Type: | Journal Article | ||||
|---|---|---|---|---|---|
| Divisions: | Faculty of Science, Engineering and Medicine > Science > Chemistry | ||||
| Journal or Publication Title: | Physical Chemistry Chemical Physics | ||||
| Publisher: | Royal Society of Chemistry | ||||
| ISSN: | 1463-9076 | ||||
| Official Date: | 28 May 2012 | ||||
| Dates: |
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| Volume: | Vol.14 | ||||
| Number: | No.20 | ||||
| Page Range: | pp. 7246-7255 | ||||
| DOI: | 10.1039/c2cp40406k | ||||
| Status: | Peer Reviewed | ||||
| Publication Status: | Published | ||||
| Access rights to Published version: | Restricted or Subscription Access |
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