Journal of Thermal Analysis and Calorimetry
Volume/Issue:
Volume 90: Issue 1
Role of structural and macrocrystalline factors in the desolvation behaviour of cortisone acetate solvates
Authors:
S. Petit Université de Rouen Unité de Croissance Cristalline et de Modélisation Moléculaire (UC2M2), Sciences et Méthodes Séparatives (SMS) UPRES EA 3233, IRCOF rue Tesnière F-76821 Mont Saint-Aignan Cedex France

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F. Mallet Université de Rouen Unité de Croissance Cristalline et de Modélisation Moléculaire (UC2M2), Sciences et Méthodes Séparatives (SMS) UPRES EA 3233, IRCOF rue Tesnière F-76821 Mont Saint-Aignan Cedex France

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M. Petit Université de Rouen Unité de Croissance Cristalline et de Modélisation Moléculaire (UC2M2), Sciences et Méthodes Séparatives (SMS) UPRES EA 3233, IRCOF rue Tesnière F-76821 Mont Saint-Aignan Cedex France

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G. Coquerel Université de Rouen Unité de Croissance Cristalline et de Modélisation Moléculaire (UC2M2), Sciences et Méthodes Séparatives (SMS) UPRES EA 3233, IRCOF rue Tesnière F-76821 Mont Saint-Aignan Cedex France

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Pages:
39–47
Online Publication Date:
21 Sep 2007
Publication Date:
01 Oct 2007
Article Category:
Research Article
DOI:
https://doi.org/10.1007/s10973-007-8475-z
Keywords:
crystal structure; desolvation mechanism; solid-solid transformation; solvates
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Abstract  

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.

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Cover Journal of Thermal Analysis and Calorimetry
Journal of Thermal Analysis and Calorimetry
Print ISSN:
1388-6150
Online ISSN:
1572-8943

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Journal of Thermal Analysis and Calorimetry
Language English
Size A4
Year of
Foundation		 1969
Volumes
per Year		 1
Issues
per Year		 24
Founder Akadémiai Kiadó
Founder's
Address		 H-1117 Budapest, Hungary 1516 Budapest, PO Box 245.
Publisher Akadémiai Kiadó
Springer Nature Switzerland AG
Publisher's
Address		 H-1117 Budapest, Hungary 1516 Budapest, PO Box 245.
CH-6330 Cham, Switzerland Gewerbestrasse 11.
Responsible
Publisher		 Chief Executive Officer, Akadémiai Kiadó
ISSN 1388-6150 (Print)
ISSN 1588-2926 (Online)

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