Improving dipolar recoupling for site-specific structural and dynamics studies in biosolids NMR: windowed RN-symmetry sequences

Physical Chemistry Chemical Physics : PCCP
Xingyu LuTatyana Polenova

Abstract

Experimental characterization of one-bond heteronuclear dipolar couplings is essential for structural and dynamics characterization of molecules by solid-state NMR. Accurate measurement of heteronuclear dipolar tensor parameters in magic-angle spinning NMR requires that the recoupling sequences efficiently reintroduce the desired heteronuclear dipolar coupling term, fully suppress other interactions (such as chemical shift anisotropy and homonuclear dipolar couplings), and be insensitive to experimental imperfections, such as radio frequency (rf) field mismatch. In this study, we demonstrate that the introduction of window delays into the basic elements of a phase-alternating R-symmetry (PARS) sequence results in a greatly improved protocol, termed windowed PARS (wPARS), which yields clean dipolar lineshapes that are unaffected by other spin interactions and are largely insensitive to experimental imperfections. Higher dipolar scaling factors can be attained in this technique with respect to PARS, which is particularly useful for the measurement of relatively small dipolar couplings. The advantages of wPARS are verified experimentally on model molecules N-acetyl-valine (NAV) and a tripeptide Met-Leu-Phe (MLF). The incorporation...Continue Reading

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Citations

Jan 16, 2021·Solid State Nuclear Magnetic Resonance·Frédéric A PerrasTakeshi Kobayashi
Jan 29, 2021·Solid State Nuclear Magnetic Resonance·Yi JiGuangjin Hou
Aug 26, 2017·The Journal of Physical Chemistry. B·Sam Asami, Bernd Reif
Dec 29, 2021·Inorganic Chemistry·Frédéric A PerrasAaron D Sadow

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