48653 20200221144326.0 doi 10.1039/c5sc04287a sideral 94582 ART-2016-94582 eng Aromí, G. Snapshots of a solid-state transformation: Coexistence of three phases trapped in one crystal 2016 Access copy available to the general public Unrestricted Crystal-to-crystal transformations have been crucial in the understanding of solid-state processes, since these may be studied in detail by means of single crystal X-ray diffraction (SCXRD) techniques. The description of the mechanisms and potential intermediates of those processes remains very challenging. In fact, solid-state transient states have rarely been observed, at least to a sufficient level of detail. We have investigated the process of guest extrusion from the non-porous molecular material Fe(bpp)(H2L)](ClO4)2·1.5C3H6O (bpp = 2,6-bis(pyrazol-3-yl)pyridine; H2L = 2,6-bis(5-(2-methoxyphenyl)-pyrazol-3-yl)pyridine; C3H6O = acetone), which occurs through ordered diffusion of acetone in a crystal-to-crystal manner, leading to dramatic structural changes. The slow kinetics of the transition allows thermal trapping of the system at various intermediate stages. The transiting single crystal can be then examined at these points through synchrotron SCXRD, offering a window upon the mechanism of the transformation at the molecular scale. These experiments have unveiled the development of an ordered intermediate phase, distinct from the initial and the final states, coexisting as the process advances with either of these two phases or, at a certain moment with both of them. The new intermediate phase has been structurally characterized in full detail by SCXRD, providing insights into the mechanism of this diffusion triggered solid-state phenomenon. The process has been also followed by calorimetry, optical microscopy, local Raman spectroscopy and powder X-ray diffraction. The discovery and description of an intermediate ordered state in a molecular solid-state transformation is of great interest and will help to understand the mechanistic details and reaction pathways underlying these transformations. info:eu-repo/grantAgreement/ES/MICINN/MAT2011-24284 info:eu-repo/grantAgreement/ES/MINECO/CTQ2012-32247 info:eu-repo/grantAgreement/ES/MINECO/CTQ-2014-59209-P info:eu-repo/semantics/openAccess by http://creativecommons.org/licenses/by/3.0/es/ 8.668 2016 CHEMISTRY, MULTIDISCIPLINARY 17 / 166 = 0.102 2016 Q1 T1 4.516 2016 Chemistry (miscellaneous) 2016 Q1 info:eu-repo/semantics/article info:eu-repo/semantics/publishedVersion Beavers, C.M. Sánchez Costa, J. Craig, G.A. Mínguez Espallargas, G. (orcid)0000-0001-8751-0983 Orera, A. (orcid)0000-0003-2095-5843 Roubeau, O. Universidad de Zaragoza 2003 395 Universidad de Zaragoza Dpto. Física Materia Condensa. Área Física Materia Condensada 7, 4 (2016), 2907-2915 Chem. sci. CHEMICAL SCIENCE 2041-6520 2449248 http://zaguan.unizar.es/record/48653/files/texto_completo.pdf Versión publicada 112914 http://zaguan.unizar.es/record/48653/files/texto_completo.jpg?subformat=icon icon Versión publicada oai:zaguan.unizar.es:48653 articulos driver 2020-02-21-13:43:48 ARTICLE