Issue 4, 2021

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

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.

Graphical abstract: Exploiting in situ NMR to monitor the formation of a metal–organic framework

Supplementary files

Article information

Article type
Edge Article
Submitted
04 Sep 2020
Accepted
17 Nov 2020
First published
20 Nov 2020
This article is Open Access

All publication charges for this article have been paid for by the Royal Society of Chemistry
Creative Commons BY license

Chem. Sci., 2021,12, 1486-1494

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

C. L. Jones, C. E. Hughes, H. H.-M. Yeung, A. Paul, Kenneth. D. M. Harris and T. L. Easun, Chem. Sci., 2021, 12, 1486 DOI: 10.1039/D0SC04892E

This article is licensed under a Creative Commons Attribution 3.0 Unported Licence. You can use material from this article in other publications without requesting further permissions from the RSC, provided that the correct acknowledgement is given.

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