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Article
Proton-Detected Solid-State NMR Spectroscopy of Spin-1/2 Nuclei with Large Chemical Shift Anisotropy
Journal of Magnetic Resonance
  • Amrit Venkatesh, Iowa State University and Ames Laboratory
  • Frédéric A. Perras, Ames Laboratory
  • Aaron J. Rossini, Iowa State University and Ames Laboratory
Document Type
Article
Publication Version
Accepted Manuscript
Publication Date
6-1-2021
DOI
10.1016/j.jmr.2021.106983
Abstract

Constant-time (CT) dipolar heteronuclear multiple quantum coherence (D-HMQC) has previously been demonstrated as a method for proton detection of high-resolution wideline NMR spectra of spin-1/2 nuclei with large chemical shift anisotropy (CSA). However, 1H transverse relaxation and t1-noise often reduce the sensitivity of D-HMQC experiments, preventing the theoretical gains in sensitivity provided by 1H detection from being realized. Here we demonstrate a series of improved pulse sequences for 1H detection of spin-1/2 nuclei under fast MAS, with 195Pt SSNMR experiments on cisplatin as an example. First, a t1-incrementation protocol for D-HMQC dubbed Arbitrary Indirect Dwell (AID) is demonstrated. AID allows the use of arbitrary, rotor asynchronous t1-increments, but removes the constant time period from CT D-HMQC, resulting in improved sensitivity by reducing transverse relaxation losses. Next, we show that short high-power adiabatic pulses (SHAPs), which efficiently invert broad MAS sideband manifolds, can be effectively incorporated into 1H detected symmetry-based resonance echo double resonance (S-REDOR) and t1-noise eliminated (TONE) D-HMQC experiments. The S-REDOR experiments with SHAPs provide approximately double the dipolar dephasing, as compared to experiments with rectangular inversion pulses. We lastly show that sensitivity and resolution can be further enhanced with the use of swept excitation pulses as well as adiabatic magic angle turning (aMAT).

Comments

This is a manuscript of an article published as Venkatesh, Amrit, Frédéric A. Perras, and Aaron J. Rossini. "Proton-detected solid-state NMR spectroscopy of spin-1/2 nuclei with large chemical shift anisotropy." Journal of Magnetic Resonance 327 (2021): 106983. DOI: 10.1016/j.jmr.2021.106983. Posted with permission.

Creative Commons License
Creative Commons Attribution-NonCommercial-No Derivative Works 4.0 International
Copyright Owner
Elsevier Inc.
Language
en
File Format
application/pdf
Citation Information
Amrit Venkatesh, Frédéric A. Perras and Aaron J. Rossini. "Proton-Detected Solid-State NMR Spectroscopy of Spin-1/2 Nuclei with Large Chemical Shift Anisotropy" Journal of Magnetic Resonance Vol. 327 (2021) p. 106983
Available at: http://works.bepress.com/aaron-rossini/113/