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New insights into the crystallization of polymorphic materials: from real-time serial crystallography to luminescence analysis

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Abstract

Detailed analysis of reaction mechanisms by in situ techniques are important for detecting metastable intermediates, analysing polymorphic transitions and thereby for the discovery of new compounds. This article presents the first combination of serial crystallography with in situ luminescence and X-ray diffraction (XRD) measurements to monitor the synthesis of [Eu(phen)2(NO3)3] (phen = 1,10-phenanthroline). In a batch reaction, it is found that this complex is polymorphic, crystallizing into two distinct monoclinic structures. We track the evolution of the synthesis conditions for these phases using in situ XRD combined with real time measurements of pH value, ion conductivity, infrared (IR) spectroscopy and in situ luminescence analysis of coordination sensors (ILACS). However, in a flow reactor a different combination of phases is produced. A serial crystallography experiment utilizing a nanofocused synchrotron X-ray beam to identify individual crystallites reveals the simultaneous formation of the two phases, as well as, a third unknown phase. This showcases the feasibility of phase detection on an individual crystallite level to track the synthesis of new materials.

Graphical abstract: New insights into the crystallization of polymorphic materials: from real-time serial crystallography to luminescence analysis

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Publication details

The article was received on 13 May 2019, accepted on 14 Jun 2019 and first published on 10 Jul 2019


Article type: Paper
DOI: 10.1039/C9RE00191C
React. Chem. Eng., 2019, Advance Article
  • Open access: Creative Commons BY-NC license
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    New insights into the crystallization of polymorphic materials: from real-time serial crystallography to luminescence analysis

    P. Lindenberg, L. R. Arana, L. K. Mahnke, P. Rönfeldt, N. Heidenreich, G. Doungmo, N. Guignot, R. Bean, H. N. Chapman, D. Dierksmeyer, J. Knoska, M. Kuhn, J. Garrevoet, V. Mariani, D. Oberthuer, K. Pande, S. Stern, A. Tolstikova, T. A. White, K. R. Beyerlein and H. Terraschke, React. Chem. Eng., 2019, Advance Article , DOI: 10.1039/C9RE00191C

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