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Article

Structure Solution of Nano-Crystalline Small Molecules Using MicroED and Solid-State NMR Dipolar-Based Experiments

1
RIKEN-JEOL Collaboration Center, RIKEN, Yokohama, Kanagawa 230-0045, Japan
2
JEOL Ltd., Akishima, Tokyo 196-8558, Japan
3
System in Frontier Inc., Tachikawa, Tokyo 190-0012, Japan
4
RIKEN Center for Biosystems Dynamics Research, RIKEN, Yokohama, Kanagawa 230-0045, Japan
5
JEOL RESONANCE Inc., Akishima, Tokyo 196-8558, Japan
*
Author to whom correspondence should be addressed.
Academic Editor: Jan Sýkora
Molecules 2021, 26(15), 4652; https://doi.org/10.3390/molecules26154652
Received: 1 July 2021 / Revised: 24 July 2021 / Accepted: 27 July 2021 / Published: 31 July 2021
(This article belongs to the Special Issue Intermolecular Interactions in Crystal Lattice)
Three-dimensional electron diffraction crystallography (microED) can solve structures of sub-micrometer crystals, which are too small for single crystal X-ray crystallography. However, R factors for the microED-based structures are generally high because of dynamic scattering. That means R factor may not be reliable provided that kinetic analysis is used. Consequently, there remains ambiguity to locate hydrogens and to assign nuclei with close atomic numbers, like carbon, nitrogen, and oxygen. Herein, we employed microED and ssNMR dipolar-based experiments together with spin dynamics numerical simulations. The NMR dipolar-based experiments were 1H-14N phase-modulated rotational-echo saturation-pulse double-resonance (PM-S-RESPDOR) and 1H-1H selective recoupling of proton (SERP) experiments. The former examined the dephasing effect of a specific 1H resonance under multiple 1H-14N dipolar couplings. The latter examined the selective polarization transfer between a 1H-1H pair. The structure was solved by microED and then validated by evaluating the agreement between experimental and calculated dipolar-based NMR results. As the measurements were performed on 1H and 14N, the method can be employed for natural abundance samples. Furthermore, the whole validation procedure was conducted at 293 K unlike widely used chemical shift calculation at 0 K using the GIPAW method. This combined method was demonstrated on monoclinic l-histidine. View Full-Text
Keywords: microED; NMR crystallography; GIPAW calculations; 1H-14N PM-S-RESPDOR; 1H-1H SERP microED; NMR crystallography; GIPAW calculations; 1H-14N PM-S-RESPDOR; 1H-1H SERP
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MDPI and ACS Style

Duong, N.T.; Aoyama, Y.; Kawamoto, K.; Yamazaki, T.; Nishiyama, Y. Structure Solution of Nano-Crystalline Small Molecules Using MicroED and Solid-State NMR Dipolar-Based Experiments. Molecules 2021, 26, 4652. https://doi.org/10.3390/molecules26154652

AMA Style

Duong NT, Aoyama Y, Kawamoto K, Yamazaki T, Nishiyama Y. Structure Solution of Nano-Crystalline Small Molecules Using MicroED and Solid-State NMR Dipolar-Based Experiments. Molecules. 2021; 26(15):4652. https://doi.org/10.3390/molecules26154652

Chicago/Turabian Style

Duong, Nghia T., Yoshitaka Aoyama, Katsumi Kawamoto, Toshio Yamazaki, and Yusuke Nishiyama. 2021. "Structure Solution of Nano-Crystalline Small Molecules Using MicroED and Solid-State NMR Dipolar-Based Experiments" Molecules 26, no. 15: 4652. https://doi.org/10.3390/molecules26154652

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