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

被引：35
|
作者：
Wu, Yue [2 ]
Breeze, Matthew I. [1 ]
Clarkson, Guy J. [1 ]
Millange, Franck [3 ]
O'Hare, Dermot [2 ]
Walton, Richard I. [1 ]
机构：
[1] Univ Warwick, Dept Chem, Coventry CV4 7AL, W Midlands, England
[2] Univ Oxford, Dept Chem, Oxford OX1 3TA, England
[3] Univ Versailles St Quentin En Yvelines, Dept Chim, 45 Ave Etats Unis, F-78035 Versailles, France
来源：
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION | 2016年 / 55卷 / 16期
基金：
英国工程与自然科学研究理事会;
关键词：
crystal growth; host-guest systems; metal-organic frameworks; microporous materials; X-ray diffraction; HYDROTHERMAL SYNTHESIS; KINETIC FACTORS; TIME;
D O I：
10.1002/anie.201600896
中图分类号：
O6 [化学];
学科分类号：
0703 ;
摘要：
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)]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 Yb3+ is replaced by DMF as the reaction progresses.
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页码：4992 / 4996
页数：5
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