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

DOI: 10.1002/anie.201508763 DOI Help

Authors: Hamish Yeung (NIMS) , Yue Wu (University of Oxford) , Sebastian Henke (University of Cambridge) , Anthony K. Cheetham (University of Cambridge) , Dermot O' Hare (University of Oxford) , Richard Walton (University of Warwick)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Angewandte Chemie International Edition , VOL 55 , PAGES 2012 - 2016

State: Published (Approved)
Published: February 2016
Diamond Proposal Number(s): 9661

Abstract: Understanding the driving forces controlling crys-tallization is essential for the efficient synthesis and design ofnew materials,particularly metal–organic frameworks(MOFs), where mild solvothermal synthesis often allowsaccess to various phases from the same reagents.Using high-energy in situ synchrotron X-ray powder diffraction, wemonitor the crystallization of lithium tartrate MOFs,observingthe successive crystallization and dissolution of three compet-ing phases in one reaction. By determining rate constants andactivation energies,wefully quantify the reaction energylandscape,gaining important predictive power for the choice ofreaction conditions.Different reaction rates are explained bythe structural relationships between the products and thereactants;larger changes in conformation result in higheractivation energies.The methods we demonstrate can easily beapplied to other materials,opening the door to agreaterunderstanding of crystallization in general.

Journal Keywords: Crystal growth; metal–organic frameworks; metastable compounds; reaction kinetics; X-ray diffraction

Subject Areas: Chemistry

Instruments: I12-JEEP: Joint Engineering, Environmental and Processing