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Updated: May 10, 2025

Preparation of Fungal and Plant Materials for Structural Elucidation Using Dynamic Nuclear Polarization Solid-State NMR
Published on: February 12, 2019
Bridging Dynamic Nuclear Polarization and Solid-State NMR Dipolar Recoupling: From Static Single Crystal to Spinning
José P Carvalho1, Anders Bodholt Nielsen1, Enikő Baligács1
1Interdisciplinary Nanoscience Center (iNANO) and Department of Chemistry, Aarhus University, Gustav Wieds Vej 14, DK-8000 Aarhus C, Denmark.
Abstract:
Spin engineering of advanced pulse sequences has had a transformative impact on the development of nuclear magnetic resonance (NMR) spectroscopy, to an extending degree also electron paramagnetic resonance (EPR), and the hybrid between the two, dynamic nuclear polarization (DNP). Based on a simple formalism, we demonstrate that (i) single-crystal static-sample optimizations may tremendously ease design and understanding of experiments for rotating powders and (ii) pulse sequences may readily be exchanged between these distinct spectroscopies. Specifically, we design broadband heteronuclear solid-state NMR magic-angle-spinning (MAS) dipolar recoupling experiments based on the recently developed PLATO (PoLarizAtion Transfer via nonlinear Optimization) microwave (MW) pulse sequence optimized on a single crystal for powder static-sample DNP. Using this concept, we demonstrate design of ultrabroadband 13C-15N and 2H-13C cross-polarization experiments, using PLATO on the 13C radio frequency (RF) channel and square/ramped or RESPIRATION (Rotor Echo Short Pulse IRrAdiaTION) RF irradiation on the 15N and 2H RF channels, respectively.
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