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Mechanochemistry-Accessed MOF Polymorphism Revealed by an Integrated 3DED/DFT-Assisted Rietveld Analysis.

Created on 17 Aug 2026

Authors

Giorgio Cagossi, Andrea Daolio, Dario Giovanardi, Iryna Andrusenko, Enrico Mugnaioli, Lucia Carlucci, Paolo P Mazzeo, Alessia Bacchi, Paolo Pelagatti

Published in

Inorganic chemistry. Volume 65. Issue 32. Pages 18639-18647. Aug 17, 2026.

Abstract

A combined 3DED, plane-wave DFT, and Rietveld refinement workflow uncovers the first example of interlayer-twisting polymorphism in a pillared MOF. While the parent material, PUM198, a Zn-based mixed-ligand MOF, was previously synthesized under solvothermal conditions, mechanochemistry selectively affords a new polymorph, PUM198-m. Although the two phases share identical composition and connectivity, they differ in symmetry, layer arrangement, pore architecture, and topology. Accessible only as a microcrystalline powder, PUM198-m is unsuitable for conventional single-crystal X-ray diffraction, and its flexibility and solvent-filled pores preclude structure solution from the XRPD data. The crystal structure was therefore derived from a multitechnique blueprint in which the starting model was derived from 3DED data and subsequently refined through iterative DFT-assisted Rietveld analysis to describe the as-synthesized, guest-loaded material. This integrated workflow provides a broadly applicable structural elucidation strategy for flexible MOFs that are mechanochemically synthesized, for which conventional crystallographic analysis fails.

PMID:
42606265
Bibliographic data and abstract were imported from PubMed on 17 Aug 2026.

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