Phase-sensitive γ-encoded recoupling of heteronuclear dipolar interactions and 1H chemical shift anisotropy

γ-encoded recoupling sequences are known to produce strong amplitude modulations that lead to sharp doublets when Fourier transformed. These doublets depend very little on the recoupled tensor asymmetry and thus enable for the straightforward determination of dynamic order parameters. It can, howeve...

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Veröffentlicht in:Solid state nuclear magnetic resonance 2021-02, Vol.111, p.101712-101712, Article 101712
Hauptverfasser: Perras, Frédéric A., Paterson, Alexander L., Kobayashi, Takeshi
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Sprache:eng
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Zusammenfassung:γ-encoded recoupling sequences are known to produce strong amplitude modulations that lead to sharp doublets when Fourier transformed. These doublets depend very little on the recoupled tensor asymmetry and thus enable for the straightforward determination of dynamic order parameters. It can, however, be difficult to measure small anisotropies, or small order parameters, using such sequences; the resonances from the doublet may overlap with each other, or with the zero-frequency glitch. This limitation has prevented the widespread use of 1H chemical shift anisotropy (CSA) for the measurement of dynamics, particularly for CH protons which typically have CSAs of only a few ppm when immobile. Here, we introduce a simple modification to the traditional 1H CSA and proton-detected local field pulse sequences that enables the acquisition of a hypercomplex dataset and the removal of the uncorrelated magnetization that results in the zero-frequency glitch. These new sequences then yield a frequency shift in the indirect dimension, rather than a splitting, which is easily identifiable even in cases of weak interactions. [Display omitted] •A phase-alternating recoupling period enables phase-sensitive γ-encoded recoupling.•Hypercomplex data is built from the sum and difference of each experiment.•Half the doublet is eliminated, shifting the center of the recoupled signal.•The new sequences are better suited to the measurement of weak interactions.
ISSN:0926-2040
1527-3326
DOI:10.1016/j.ssnmr.2020.101712