In situ X-ray diffraction monitoring of a mechanochemical reaction reveals a unique topology metal-organic framework

Athanassios D. Katsenis, Andreas Puškarić, Vjekoslav Štrukil, Cristina Mottillo, Patrick A. Julien, Krunoslav Užarević, Minh-Hao Pham, Trong-On Do, Simon A. J. Kimber, Predrag Lazić, Oxana Magdysyuk, Robert E. Dinnebier, Ivan Halasz () and Tomislav Friščić ()
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Athanassios D. Katsenis: McGill University
Andreas Puškarić: Ruđer Bošković Institute
Vjekoslav Štrukil: McGill University
Cristina Mottillo: McGill University
Patrick A. Julien: McGill University
Krunoslav Užarević: Ruđer Bošković Institute
Minh-Hao Pham: Université Laval
Trong-On Do: Université Laval
Simon A. J. Kimber: ESRF—The European Synchrotron
Predrag Lazić: Ruđer Bošković Institute
Oxana Magdysyuk: Scientific Service Group X-ray Diffraction, Max Planck Institute for Solid State Research
Robert E. Dinnebier: Scientific Service Group X-ray Diffraction, Max Planck Institute for Solid State Research
Ivan Halasz: Ruđer Bošković Institute
Tomislav Friščić: McGill University

Nature Communications, 2015, vol. 6, issue 1, 1-8

Abstract: Abstract Chemical and physical transformations by milling are attracting enormous interest for their ability to access new materials and clean reactivity, and are central to a number of core industries, from mineral processing to pharmaceutical manufacturing. While continuous mechanical stress during milling is thought to create an environment supporting nonconventional reactivity and exotic intermediates, such speculations have remained without proof. Here we use in situ, real-time powder X-ray diffraction monitoring to discover and capture a metastable, novel-topology intermediate of a mechanochemical transformation. Monitoring the mechanochemical synthesis of an archetypal metal-organic framework ZIF-8 by in situ powder X-ray diffraction reveals unexpected amorphization, and on further milling recrystallization into a non-porous material via a metastable intermediate based on a previously unreported topology, herein named katsenite (kat). The discovery of this phase and topology provides direct evidence that milling transformations can involve short-lived, structurally unusual phases not yet accessed by conventional chemistry.

Date: 2015
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DOI: 10.1038/ncomms7662

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