title: Exchange of Coordinated Solvent During Crystallization of a Metal-Organic Framework Observed by In Situ High-Energy X-ray Diffraction.
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.
authors.affiliation: Department of Chemistry, University of Oxford, Oxford, OX1 3TA, UK.
authors.forename: Yue
authors.initials: Y
authors.lastname: Wu
authors.affiliation: Department of Chemistry, University of Warwick, Coventry, CV4 7AL, UK).
authors.forename: Matthew I
authors.initials: MI
authors.lastname: Breeze
authors.affiliation: Department of Chemistry, University of Warwick, Coventry, CV4 7AL, UK).
authors.forename: Guy J
authors.initials: GJ
authors.lastname: Clarkson
authors.affiliation: Département de Chimie, Université de Versailles-St-Quentin-en-Yvelines, 45 Avenue des États-Unis, 78035, Versailles cedex, France.
authors.forename: Franck
authors.initials: F
authors.lastname: Millange
authors.affiliation: Department of Chemistry, University of Oxford, Oxford, OX1 3TA, UK.
authors.forename: Dermot
authors.initials: D
authors.lastname: O'Hare
authors.affiliation: Department of Chemistry, University of Warwick, Coventry, CV4 7AL, UK). r.i.walton@warwick.ac.uk.
authors.forename: Richard I
authors.initials: RI
authors.lastname: Walton
keywords: X-ray diffraction; crystal growth; host-guest systems; metal-organic frameworks; microporous materials