Comparison of methods for the NMR measurement of motionally averaged dipolar couplings

Southern, Scott A.; Perras, Frédéric A.

doi:10.1016/j.jmr.2024.107710

Comparison of methods for the NMR measurement of motionally averaged dipolar couplings

Journal Article · Sun Jun 09 00:00:00 EDT 2024 · Journal of Magnetic Resonance

DOI:https://doi.org/10.1016/j.jmr.2024.107710· OSTI ID:2376183

Southern, Scott A. ^[1]; Perras, Frédéric A. ^[2]

Ames Laboratory (AMES), Ames, IA (United States)
Ames Lab., and Iowa State Univ., Ames, IA (United States)

Motionally averaged dipolar couplings are an important tool for understanding the complex dynamics of catalysts, polymers, and biomolecules. While there is a plethora of solid-state NMR pulse sequences available for their measurement, in can be difficult to gauge the methods’ strengths and weaknesses. In particular, there has not been a comprehensive comparison of their performance in natural abundance samples, where 1H homonuclear dipolar couplings are important and the use of large MAS rotors may be required for sensitivity reasons. In this work, we directly compared some of the more common methods for measuring C–H dipolar couplings in natural abundance samples using L-alanine (L-Ala) and the N-formyl-L-methionyl-L-leucyl-L-phenylalanine (fMLF) tripeptide as model systems. Here, we evaluated their performance in terms of accuracy, resolution, sensitivity, and ease of implementation. We found that, despite the presence of 1H homonuclear dipolar interactions, all methods, with the exception of REDOR, were able to yield the reasonable dipolar coupling strengths for both mobile and static moieties. Of these methods, PDLF provides the most convenient workflow and precision at the expense of low sensitivity. In low-sensitivity cases, MAS-PISEMA and DIPSHIFT appear to be the better options.

View Accepted Manuscript (DOE)

Research Organization:: Ames Laboratory (AMES), Ames, IA (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES). Chemical Sciences, Geosciences & Biosciences Division (CSGB)

Grant/Contract Number:: AC02-07CH11358

OSTI ID:: 2376183

Report Number(s):: IS-J--11,356

Journal Information:: Journal of Magnetic Resonance, Journal Name: Journal of Magnetic Resonance Vol. 364; ISSN 1090-7807

Publisher:: ElsevierCopyright Statement

Country of Publication:: United States

Language:: English

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