caa a22 4500 46318940X CHVBK 20180406164904.0 cr unu---uuuuu 170326e20071001xx s 000 0 eng 10.1007/s10973-007-8475-z doi (NATIONALLICENCE)springer-10.1007/s10973-007-8475-z Role of structural and macrocrystalline factors in the desolvation behaviour of cortisone acetate solvates [Elektronische Daten] [S. Petit, F. Mallet, M. Petit, G. Coquerel] A combined analysis of structural data and experimental results (DSC, temperature-resolved XRPD and hot stage optical microscopy) revealed that the dehydration mechanism of cortisone acetate monohydrate (CTA·H2O) involves a collective and anisotropic departure of water molecules followed by a cooperative structural reorganization toward the anhydrous polymorph CTA (form 2). In spite of the lack of crystal structure data, it can be postulated from experimental data that thermal decomposition of the dihydrated form (CTA·2H2O) and of the tetrahydrofuran solvate (CTA·THF) toward another polymorph (CTA (form 3)) also proceeds according to a cooperative mechanism, thus giving rise to probable structural filiations between these crystalline forms of CTA. The crystal structure determination of two original solvates (CTA·DMF and CTA·DMSO) indicates that these phases are isomorphous to the previously reported acetone solvate. However, their desolvation behaviour does not involve a cooperative mechanism, as could be expected from structural data only. Instead, the decomposition mechanism of CTA·DMF and CTA·DMSO starts with the formation of a solvent-proof superficial layer, followed by the partial dissolution of the enclosed inner part of crystals. Hot stage optical microscopy observations and DSC measurements showed that dissolved materials (resulting from a peritectic decomposition) is suddenly evacuated through macroscopic cracks about 30°C above the ebullition point of each solvent. From this unusual behaviour, the necessity to investigate rigorously the various aspects (thermodynamics, kinetics, crystal structures and physical factors) of solvate decompositions is highlighted, including factors related to the particular preparation route of each sample. Springer Science+Business Media, LLC., 2007 crystal structure nationallicence desolvation mechanism nationallicence solid-solid transformation nationallicence solvates nationallicence Petit S. Unité de Croissance Cristalline et de Modélisation Moléculaire (UC2M2), Sciences et Méthodes Séparatives (SMS) UPRES EA 3233, IRCOF, Université de Rouen, rue Tesnière, F-76821, Mont Saint-Aignan Cedex, France aut Mallet F. Unité de Croissance Cristalline et de Modélisation Moléculaire (UC2M2), Sciences et Méthodes Séparatives (SMS) UPRES EA 3233, IRCOF, Université de Rouen, rue Tesnière, F-76821, Mont Saint-Aignan Cedex, France aut Petit M. Unité de Croissance Cristalline et de Modélisation Moléculaire (UC2M2), Sciences et Méthodes Séparatives (SMS) UPRES EA 3233, IRCOF, Université de Rouen, rue Tesnière, F-76821, Mont Saint-Aignan Cedex, France aut Coquerel G. Unité de Croissance Cristalline et de Modélisation Moléculaire (UC2M2), Sciences et Méthodes Séparatives (SMS) UPRES EA 3233, IRCOF, Université de Rouen, rue Tesnière, F-76821, Mont Saint-Aignan Cedex, France aut Journal of Thermal Analysis and Calorimetry Springer US; http://www.springer-ny.com 90/1(2007-10-01), 39-47 1388-6150 90:1<39 2007 90 10973 https://doi.org/10.1007/s10973-007-8475-z text/html Onlinezugriff via DOI 1 research-article jats NATIONALLICENCE 856 40 https://doi.org/10.1007/s10973-007-8475-z text/html Onlinezugriff via DOI NATIONALLICENCE 700 1- Petit S. Unité de Croissance Cristalline et de Modélisation Moléculaire (UC2M2), Sciences et Méthodes Séparatives (SMS) UPRES EA 3233, IRCOF, Université de Rouen, rue Tesnière, F-76821, Mont Saint-Aignan Cedex, France aut NATIONALLICENCE 700 1- Mallet F. Unité de Croissance Cristalline et de Modélisation Moléculaire (UC2M2), Sciences et Méthodes Séparatives (SMS) UPRES EA 3233, IRCOF, Université de Rouen, rue Tesnière, F-76821, Mont Saint-Aignan Cedex, France aut NATIONALLICENCE 700 1- Petit M. Unité de Croissance Cristalline et de Modélisation Moléculaire (UC2M2), Sciences et Méthodes Séparatives (SMS) UPRES EA 3233, IRCOF, Université de Rouen, rue Tesnière, F-76821, Mont Saint-Aignan Cedex, France aut NATIONALLICENCE 700 1- Coquerel G. Unité de Croissance Cristalline et de Modélisation Moléculaire (UC2M2), Sciences et Méthodes Séparatives (SMS) UPRES EA 3233, IRCOF, Université de Rouen, rue Tesnière, F-76821, Mont Saint-Aignan Cedex, France aut NATIONALLICENCE 773 0- Journal of Thermal Analysis and Calorimetry Springer US; http://www.springer-ny.com 90/1(2007-10-01), 39-47 1388-6150 90:1<39 2007 90 10973 Metadata rights reserved Springer special CC-BY-NC licence nationallicence BK010053 XK010053 XK010000 NATIONALLICENCE NATIONALLICENCE NL-springer