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revised on 04.09.2020 and posted on 07.09.2020by Corey Jones, Colan Hughes, Hamish Yeung, Alison Paul, Kenneth D. M. Harris, Timothy Easun
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 5 fixed temperatures afford qualitative information on the solution-phase processes and
quantitative information on the kinetics of crystallization, allowing the activation
energies for nucleation and
growth to be determined. Ex-situ SAXS studies 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 is phase-pure