Proton-detected 15N-1H dipolar coupling/1H chemical shift correlation experiment for the measurement of NH distances in biological solids under fast MAS solid-state NMR
Abstract
Measurement of distances from dipolar couplings is essential for structural characterization, refinement and validation using the solid-state nuclear magnetic resonance (ssNMR) spectroscopy. Particularly, knowledge about NH dipolar interactions in biological solids is important for understanding the hydrogen (H)-bonding interactions, molecular geometry and spin dynamics. In this regard, we have proposed a proton-detected two-dimensional (2D) 15N-1H dipolar coupling/1H chemical shift correlation experiment using the C-symmetry based windowless recoupling of chemical shift anisotropy (ROCSA) in combination with the DIPSHIFT pulse-based method for the measurement of short NH distances in the isotopically labeled and naturally abundant biological solids at fast magic angle spinning (MAS) rates (40–70 kHz). Our proposed method results in undistorted recoupled 15N-1H dipolar coupling powder lineshapes that are free from the recoupled 1H CSA contributions under the 15N evolution, a feature that is essential for the measurement of NH distances with improved accuracy (± 500 Hz in terms of the NH dipolar couplings). The pulse sequence developed in the present study is also insensitive to the 1H–1H homonuclear dipolar interactions, relaxation effects owing to its constant-time implementation, and t1-noise from the fluctuations in the MAS.
- Authors:
-
- Indian Inst. of Technology (IIT), Rupnagar (India)
- Ames Lab., and Iowa State Univ., Ames, IA (United States)
- Institute of Physical and Chemical Research (RIKEN), Yokohama (Japan). RIKEN-JEOL Collaboration Center; JEOL RESONANCE Inc., Tokyo (Japan)
- Publication Date:
- Research Org.:
- Ames Lab., Ames, IA (United States)
- Sponsoring Org.:
- USDOE Office of Science (SC), Basic Energy Sciences (BES). Materials Sciences & Engineering Division; JSPS KAKENHI; Science and Engineering Research Board (SERB)
- OSTI Identifier:
- 1837758
- Report Number(s):
- IS-J-10,681
Journal ID: ISSN 2666-4410
- Grant/Contract Number:
- AC02-07CH11358; ECR/2017/000713; 20K05483; JPMJMI17A2
- Resource Type:
- Accepted Manuscript
- Journal Name:
- Journal of Magnetic Resonance Open
- Additional Journal Information:
- Journal Volume: 10-11; Journal ID: ISSN 2666-4410
- Publisher:
- Elsevier
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS; Solid-state NMR; ROCSA; DIPSHIFT; Dipolar couplings; Fast MAS
Citation Formats
Nehra, Ekta, Sehrawat, Neelam, Kobayashi, Takeshi, Nishiyama, Yusuke, and Pandey, Manoj Kumar. Proton-detected 15N-1H dipolar coupling/1H chemical shift correlation experiment for the measurement of NH distances in biological solids under fast MAS solid-state NMR. United States: N. p., 2021.
Web. doi:10.1016/j.jmro.2021.100028.
Nehra, Ekta, Sehrawat, Neelam, Kobayashi, Takeshi, Nishiyama, Yusuke, & Pandey, Manoj Kumar. Proton-detected 15N-1H dipolar coupling/1H chemical shift correlation experiment for the measurement of NH distances in biological solids under fast MAS solid-state NMR. United States. https://doi.org/10.1016/j.jmro.2021.100028
Nehra, Ekta, Sehrawat, Neelam, Kobayashi, Takeshi, Nishiyama, Yusuke, and Pandey, Manoj Kumar. Tue .
"Proton-detected 15N-1H dipolar coupling/1H chemical shift correlation experiment for the measurement of NH distances in biological solids under fast MAS solid-state NMR". United States. https://doi.org/10.1016/j.jmro.2021.100028. https://www.osti.gov/servlets/purl/1837758.
@article{osti_1837758,
title = {Proton-detected 15N-1H dipolar coupling/1H chemical shift correlation experiment for the measurement of NH distances in biological solids under fast MAS solid-state NMR},
author = {Nehra, Ekta and Sehrawat, Neelam and Kobayashi, Takeshi and Nishiyama, Yusuke and Pandey, Manoj Kumar},
abstractNote = {Measurement of distances from dipolar couplings is essential for structural characterization, refinement and validation using the solid-state nuclear magnetic resonance (ssNMR) spectroscopy. Particularly, knowledge about NH dipolar interactions in biological solids is important for understanding the hydrogen (H)-bonding interactions, molecular geometry and spin dynamics. In this regard, we have proposed a proton-detected two-dimensional (2D) 15N-1H dipolar coupling/1H chemical shift correlation experiment using the C-symmetry based windowless recoupling of chemical shift anisotropy (ROCSA) in combination with the DIPSHIFT pulse-based method for the measurement of short NH distances in the isotopically labeled and naturally abundant biological solids at fast magic angle spinning (MAS) rates (40–70 kHz). Our proposed method results in undistorted recoupled 15N-1H dipolar coupling powder lineshapes that are free from the recoupled 1H CSA contributions under the 15N evolution, a feature that is essential for the measurement of NH distances with improved accuracy (± 500 Hz in terms of the NH dipolar couplings). The pulse sequence developed in the present study is also insensitive to the 1H–1H homonuclear dipolar interactions, relaxation effects owing to its constant-time implementation, and t1-noise from the fluctuations in the MAS.},
doi = {10.1016/j.jmro.2021.100028},
journal = {Journal of Magnetic Resonance Open},
number = ,
volume = 10-11,
place = {United States},
year = {Tue Dec 28 00:00:00 EST 2021},
month = {Tue Dec 28 00:00:00 EST 2021}
}
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