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Yeung HH, Wu Y, Henke S, et al. In Situ Observation of Successive Crystallizations and Metastable Intermediates in the Formation of Metal-Organic Frameworks. Angew Chem Int Ed Engl. 2016;55(6):2012-6doi: 10.1002/anie.201508763.
Yeung, H. H., Wu, Y., Henke, S., Cheetham, A. K., O'Hare, D., & Walton, R. I. (2016). In Situ Observation of Successive Crystallizations and Metastable Intermediates in the Formation of Metal-Organic Frameworks. Angewandte Chemie (International ed. in English), 55(6), 2012-6. https://doi.org/10.1002/anie.201508763
Yeung, Hamish H-M, et al. "In Situ Observation of Successive Crystallizations and Metastable Intermediates in the Formation of Metal-Organic Frameworks." Angewandte Chemie (International ed. in English) vol. 55,6 (2016): 2012-6. doi: https://doi.org/10.1002/anie.201508763
Yeung HH, Wu Y, Henke S, Cheetham AK, O'Hare D, Walton RI. In Situ Observation of Successive Crystallizations and Metastable Intermediates in the Formation of Metal-Organic Frameworks. Angew Chem Int Ed Engl. 2016 Feb 05;55(6):2012-6. doi: 10.1002/anie.201508763. Epub 2016 Jan 06. PMID: 26836335.
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Angew Chem Int Ed Engl. 2016 Feb 05;55(6):2012-6. doi: 10.1002/anie.201508763. Epub 2016 Jan 06.

In Situ Observation of Successive Crystallizations and Metastable Intermediates in the Formation of Metal-Organic Frameworks.

Angewandte Chemie (International ed. in English)

Hamish H-M Yeung, Yue Wu, Sebastian Henke, Anthony K Cheetham, Dermot O'Hare, Richard I Walton

Affiliations

  1. International Center for Materials Nanoarchitectonics (MANA), National Institute for Materials Science, Namiki 1-1, Tsukuba, Ibaraki, 305-0044, Japan. [email protected].
  2. International Center for Young Scientists (ICYS), National Institute for Materials Science, Sengen 1-2-1, Tsukuba, Ibaraki, 305-0047, Japan. [email protected].
  3. Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford, OX1 3TA, UK.
  4. Lehrstuhl für Anorganische Chemie II, Ruhr-Universität Bochum, Universitätstrasse 150, 44801, Bochum, Germany.
  5. Department of Materials Science and Metallurgy, Cambridge University, 27 Charles Babbage Road, Cambridge, CB3 0FS, UK.
  6. Department of Chemistry, University of Warwick, Coventry, CV4 7AL, UK. [email protected].

PMID: 26836335 DOI: 10.1002/anie.201508763

Abstract

Understanding the driving forces controlling crystallization is essential for the efficient synthesis and design of new materials, particularly metal-organic frameworks (MOFs), where mild solvothermal synthesis often allows access to various phases from the same reagents. Using high-energy in situ synchrotron X-ray powder diffraction, we monitor the crystallization of lithium tartrate MOFs, observing the successive crystallization and dissolution of three competing phases in one reaction. By determining rate constants and activation energies, we fully quantify the reaction energy landscape, gaining important predictive power for the choice of reaction conditions. Different reaction rates are explained by the structural relationships between the products and the reactants; larger changes in conformation result in higher activation energies. The methods we demonstrate can easily be applied to other materials, opening the door to a greater understanding of crystallization in general.

© 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Keywords: X-ray diffraction; crystal growth; metal-organic frameworks; metastable compounds; reaction kinetics

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