Exploiting in-situ NMR to monitor the formation of a metal-organic framework

Jones, Corey L., Hughes, Colan E., Yeung, Hamish H.-M., Paul, Alison ORCID: https://orcid.org/0000-0002-7653-9964, Harris, Kenneth D. M. ORCID: https://orcid.org/0000-0001-7855-8598 and Easun, Timothy L. ORCID: https://orcid.org/0000-0002-0713-2642 2021. Exploiting in-situ NMR to monitor the formation of a metal-organic framework. Chemical Science 12 (4) , pp. 1486-1494. 10.1039/D0SC04892E

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Abstract

The formation processes of metal–organic frameworks are becoming more widely researched using in situ techniques, although there remains a scarcity of NMR studies in this field. In this work, the synthesis of framework MFM-500(Ni) has been investigated using an in situ NMR strategy that provides information on the time-evolution of the reaction and crystallization process. In our in situ NMR study of MFM-500(Ni) formation, liquid-phase 1H NMR data recorded as a function of time at fixed temperatures (between 60 and 100 °C) afford qualitative information on the solution-phase processes and quantitative information on the kinetics of crystallization, allowing the activation energies for nucleation (61.4 ± 9.7 kJ mol−1) and growth (72.9 ± 8.6 kJ mol−1) to be determined. Ex situ small-angle X-ray scattering studies (at 80 °C) provide complementary nanoscale information on the rapid self-assembly prior to MOF crystallization and in situ powder X-ray diffraction confirms that the only crystalline phase present during the reaction (at 90 °C) is phase-pure MFM-500(Ni). This work demonstrates that in situ NMR experiments can shed new light on MOF synthesis, opening up the technique to provide better understanding of how MOFs are formed.

Item Type:	Article
Date Type:	Publication
Status:	Published
Schools:	Chemistry
Publisher:	Royal Society of Chemistry
ISSN:	2041-6520
Funders:	EPSRC
Date of First Compliant Deposit:	2 December 2020
Date of Acceptance:	17 November 2020
Last Modified:	08 May 2023 10:11
URI:	https://orca.cardiff.ac.uk/id/eprint/136739

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