Determination of the relative orientation between 15N-1H dipolar coupling and 1H chemical shift anisotropy tensors under fast MAS solid-state NMR

Sehrawat, Neelam; Nehra, Ekta; Kumar Rohilla, Ketan; Kobayashi, Takeshi; Nishiyama, Yusuke; Kumar Pandey, Manoj

doi:10.1016/j.jmr.2023.107428

Determination of the relative orientation between ¹⁵N-¹H dipolar coupling and ¹H chemical shift anisotropy tensors under fast MAS solid-state NMR

Journal Article · Wed Mar 29 00:00:00 EDT 2023 · Journal of Magnetic Resonance

DOI:https://doi.org/10.1016/j.jmr.2023.107428· OSTI ID:1969481

Sehrawat, Neelam ^[1]; Nehra, Ekta ^[1]; Kumar Rohilla, Ketan ^[1]; Kobayashi, Takeshi ^[2]; Nishiyama, Yusuke ^[3]; Kumar Pandey, Manoj ^[1]

Indian Inst. of Technology (IIT) (India)
Ames Lab., and Iowa State Univ., Ames, IA (United States)
RIKEN, Saitama (Japan); JEOL Ltd., Tokyo (Japan)

Here, in this work, we have proposed a proton-detected three-dimensional (3D) ¹⁵N-¹H dipolar coupling (DIP)/¹H chemical shift anisotropy (CSA)/¹H chemical shift (CS) correlation experiment to measure the relative orientation between the ¹⁵N-¹H dipolar coupling and the ¹H CSA tensors under fast magic angle spinning (MAS) solid-state NMR. In the 3D correlation experiment, the ¹⁵N-¹H dipolar coupling and ¹H CSA tensors are recoupled using our recently developed windowless C-symmetry-based $$C3^{1}_{3}$$-ROCSA (recoupling of chemical shift anisotropy) DIPSHIFT and $$C3^{1}_{3}$$-ROCSA pulse-based methods, respectively. The 2D ¹⁵N-¹H DIP/¹H CSA powder lineshapes extracted using the proposed 3D correlation method are shown to be sensitive to the sign and asymmetry of the ¹H CSA tensor, a feature that allows the determination of the relative orientation between the two correlating tensors with improved accuracy. The experimental method developed in this study is demonstrated on a powdered U-¹⁵N L-Histidine.HCl·H₂O sample.

View Accepted Manuscript (DOE)

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

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES). Materials Sciences & Engineering Division

Grant/Contract Number:: AC02-07CH11358

OSTI ID:: 1969481

Alternate ID(s):: OSTI ID: 1968362

Report Number(s):: IS-J-11,022

Journal Information:: Journal of Magnetic Resonance, Journal Name: Journal of Magnetic Resonance Vol. 350; ISSN 1090-7807

Publisher:: ElsevierCopyright Statement

Country of Publication:: United States

Language:: English

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