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Exchange of Coordinated Solvent During Crystallization of a Metal–Organic Framework Observed by In Situ High‐Energy X‐ray Diffraction
Author(s) -
Wu Yue,
Breeze Matthew I.,
Clarkson Guy J.,
Millange Franck,
O'Hare Dermot,
Walton Richard I.
Publication year - 2016
Publication title -
angewandte chemie international edition
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 5.831
H-Index - 550
eISSN - 1521-3773
pISSN - 1433-7851
DOI - 10.1002/anie.201600896
Subject(s) - crystallization , solvent , crystallography , materials science , dimethylformamide , diffraction , molecule , powder diffraction , x ray crystallography , in situ , chemistry , organic chemistry , optics , physics
Using time‐resolved monochromatic high energy X‐ray diffraction, we present an in situ study of the solvothermal crystallisation of a new MOF [Yb 2 (BDC) 3 (DMF) 2 ]⋅H 2 O (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.