NDLI: Ex-Situ Kinetic Investigations of the Formation of the Poly-Oxo Cluster $U_{38}$

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Ex-Situ Kinetic Investigations of the Formation of the Poly-Oxo Cluster $U_{38}$

Content Provider	World Health Organization (WHO)-Global Index Medicus
Author	Falaise, Clément Volkringer, Christophe Hennig, Christoph Loiseau, Thierry
Description	Author Affiliation: Falaise C ( Unité de Catalyse et Chimie du Solide (UCCS) - UMR CNRS 8181, Université de Lille, USTL-ENSCL, Bat C7, BP 90108, 59652 Villeneuve d'Ascq (France).); Volkringer C ( Unité de Catalyse et Chimie du Solide (UCCS) - UMR CNRS 8181, Université de Lille, USTL-ENSCL, Bat C7, BP 90108, 59652 Villeneuve d'Ascq (France).); Hennig C ( Institut Universitaire de France (IUF), 1, rue Descartes, 75231 Paris (France).); Loiseau T ( Helmholtz-Zentrum Dresden-Rossendorf, Institute of Resource Ecology, Bautzner Landstr. 400, 01314 Dresden (Germany).)
Abstract	The ex-situ qualitative study of the kinetic formation of the poly-oxo cluster $U_{38},$ has been investigated after the solvothermal reaction. The resulting products have been characterized by means of powder XRD and scanning electron microscopy (SEM) for the solid phase and UV/Vis, X-ray absorption near edge structure (XANES), extended X-ray absorption fine structure (EXAFS), and NMR spectroscopies for the supernatant liquid phase. The analysis of the different synthesis batches, stopped at different reaction times, revealed the formation of spherical crystallites of $UO_{2}$ from t=3 h, after the formation of unknown solid phases at an early stage. The crystallization of $U_{38}$ occurred from t=4 h at the expense of $UO_{2},$ and is completed after t=8 h. Starting from pure uranium(IV) species in solution (t=0–1 h), oxidation reactions are observed with a $U^{IV}/U^{VI}$ ratio of 70:30 for t=1–3 h. Then, the ratio is inversed with a $U^{IV}/U^{VI}$ ratio of 25/75, when the precipitation of $UO_{2}$ occurs. Thorough SEM observations of the $U_{38}$ crystallites showed that the $UO_{2}$ aggregates are embedded within. This may indicate that $UO_{2}$ acts as reservoir of uranium(IV), for the formation of $U_{38},$ stabilized by benzoate and THF ligands. During the early stages of the $U_{38}$ crystallization, a transient crystallized phase appeared at t=4 h. Its crystal structure revealed a new dodecanuclear moiety $(U_{12}),$ based on the inner hexanuclear core of $\{U_{6}O_{8}\}$ type, decorated by three additional pairs of dinuclear $U_{2}$ units. The $U_{12}$ motif is stabilized by benzoate, oxalates, and glycolate ligands.
ISSN	09476539
e-ISSN	15213765
Journal	Chemistry - A European Journal
Issue Number	46
Volume Number	21
Language	English
Publisher	Wiley-VCH;ChemPubSoc Europe
Publisher Date	2015-11-09
Publisher Place	Germany
Access Restriction	Open
Subject Keyword	Chemistry
Content Type	Text
Resource Type	Article
Subject	Organic Chemistry Catalysis

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