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Wu Y, Breeze MI, Clarkson GJ, et al. Exchange of Coordinated Solvent During Crystallization of a Metal-Organic Framework Observed by In Situ High-Energy X-ray Diffraction. Angew Chem Int Ed Engl. 2016;55(16):4992-6doi: 10.1002/anie.201600896.
Wu, Y., Breeze, M. I., Clarkson, G. J., Millange, F., O'Hare, D., & Walton, R. I. (2016). Exchange of Coordinated Solvent During Crystallization of a Metal-Organic Framework Observed by In Situ High-Energy X-ray Diffraction. Angewandte Chemie (International ed. in English), 55(16), 4992-6. https://doi.org/10.1002/anie.201600896
Wu, Yue, et al. "Exchange of Coordinated Solvent During Crystallization of a Metal-Organic Framework Observed by In Situ High-Energy X-ray Diffraction." Angewandte Chemie (International ed. in English) vol. 55,16 (2016): 4992-6. doi: https://doi.org/10.1002/anie.201600896
Wu Y, Breeze MI, Clarkson GJ, Millange F, O'Hare D, Walton RI. Exchange of Coordinated Solvent During Crystallization of a Metal-Organic Framework Observed by In Situ High-Energy X-ray Diffraction. Angew Chem Int Ed Engl. 2016 Apr 11;55(16):4992-6. doi: 10.1002/anie.201600896. Epub 2016 Mar 09. PMID: 26959076; PMCID: PMC6680260.
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Angew Chem Int Ed Engl. 2016 Apr 11;55(16):4992-6. doi: 10.1002/anie.201600896. Epub 2016 Mar 09.

Exchange of Coordinated Solvent During Crystallization of a Metal-Organic Framework Observed by In Situ High-Energy X-ray Diffraction.

Angewandte Chemie (International ed. in English)

Yue Wu, Matthew I Breeze, Guy J Clarkson, Franck Millange, Dermot O'Hare, Richard I Walton

Affiliations

  1. Department of Chemistry, University of Oxford, Oxford, OX1 3TA, UK.
  2. Department of Chemistry, University of Warwick, Coventry, CV4 7AL, UK).
  3. Département de Chimie, Université de Versailles-St-Quentin-en-Yvelines, 45 Avenue des États-Unis, 78035, Versailles cedex, France.
  4. Department of Chemistry, University of Warwick, Coventry, CV4 7AL, UK). [email protected].

PMID: 26959076 PMCID: PMC6680260 DOI: 10.1002/anie.201600896

Abstract

Using time-resolved monochromatic high energy X-ray diffraction, we present an in situ study of the solvothermal crystallisation of a new MOF [Yb2(BDC)3(DMF)2]⋅H2O (BDC=benzene-1,4-dicarboxylate and DMF=N,N-dimethylformamide) under solvothermal conditions, from mixed water/DMF solvent. Analysis of high resolution powder patterns obtained reveals an evolution of lattice parameters and electron density during the crystallisation process and Rietveld analysis shows that this is due to a gradual topochemical replacement of coordinated solvent molecules. The water initially coordinated to Yb(3+) is replaced by DMF as the reaction progresses.

© 2016 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA.

Keywords: X-ray diffraction; crystal growth; host-guest systems; metal-organic frameworks; microporous materials

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