Document Type

Article

Publication Date

2025

DOI

10.1107/S1600576724012068

Publication Title

Journal of Applied Crystallography

Volume

58

Issue

2

Pages

398-411

Abstract

This study successfully implemented microcrystal electron diffraction (microED) and X-ray powder diffraction (XRPD) for the crystal structure determination of a new phase, TAF-CNU-1, Ni(C₈H₄O₄)·3H₂O, solved by microED from single microcrystals in the powder and refined at the kinematic and dynamic electron diffraction theory levels. This nickel metal–organic framework (MOF), together with its cobalt and manganese analogues with formula M (C₈H₄O₄)·2H₂O with M = Mn II or CoII, were synthesized in aqueous media as one-pot preparations from the corresponding hydrated metal chlorides and sodium terephthalate, as a promising `green' synthetic route to moisture-stable MOFs. The crystal structures of the two latter materials have been previously determined ab initio from X-ray powder diffraction. The advantages and disadvantages of both structural characterization techniques are briefly summarized. Additional solid-state property characterization was carried out using thermogravimetric analysis, scanning electron microscopy and Fourier transform infrared spectroscopy.

Rights

© 2025 The Authors.

Published under a Creative Commons Attribution 4.0 International (CC BY 4.0) License.

Original Publication Citation

Biehler, E., Pagola, S., Stam, D., Merkelbach, J., Jandl, C., & Abdel-Fattah, T. (2025). A comparison of microcrystal electron diffraction and X-ray powder diffraction for the structural analysis of metal–organic frameworks. Journal of Applied Crystallography, 58(2), 398-411. https://doi.org/10.1107/S1600576724012068

ORCID

0000-0003-2083-7599 (Pagola)

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