Employment of 2-pyrrole aldoxime in iron cluster chemistry: Trinuclear and hexanuclear clusters

Canaj, A. B. , Siczek, M., Douvalis, A. P., Bakas, T., Lis, T. and Milios, C. J. (2013) Employment of 2-pyrrole aldoxime in iron cluster chemistry: Trinuclear and hexanuclear clusters. Polyhedron, 52, pp. 1411-1415. (doi:10.1016/j.poly.2012.04.037)

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Abstract

The reaction of Fe(ClO4)3·9H2O with 2-pyrrole aldoxime (pyroxH2) and two equivalents of sodium benzoate in MeCN afforded the complex {[FeIII6O2(OH)2(pyroxH)2(PhCOO)10(H2O)2]·[FeIII3O(pyroxH2)2(PhCOO)6(MeCN)](ClO4)·6.6MeCN} (1·6.6MeCN) in moderate yield. Repeating the same reaction in EtOH gave the complex [FeIII6O2(OH)2(pyroxH)2(PhCOO)10(EtOH)2] (2) in good yield. The crystal structures of 1 and 2 have been determined by single-crystal X-ray crystallography. Complex 1 contains two different clusters in the crystal: a trinuclear [FeIII3] molecule and a hexanuclear [FeIII6] unit, both of which contain different forms of the 2-pyrrole aldoxime ligand. Complex 2 is a hexanuclear [FeIII6] cluster almost identical with the hexametallic unit found in 1, with the difference being the presence of two terminal EtOH molecules in 2 versus two terminal H2O molecules in the hexametallic sub-unit of 1. DC magnetic susceptibility studies were performed on polycrystalline sample of 2, revealing the presence of strong antiferromagnetic interactions within the cluster leading to a well isolated diamagnetic ground-state. The oxidation state of the iron atoms in 2 were further established by Mössbauer studies performed at 77 K.

Item Type:Articles
Additional Information:C.J.M. would like to thank the University of Crete (ELKE, Research Grant KA 3390) for funding.
Status:Published
Refereed:Yes
Glasgow Author(s) Enlighten ID:Tsanai, Mr Angelos
Authors: Canaj, A. B., Siczek, M., Douvalis, A. P., Bakas, T., Lis, T., and Milios, C. J.
College/School:College of Science and Engineering > School of Chemistry
Journal Name:Polyhedron
Publisher:Elsevier
ISSN:0277-5387
ISSN (Online):1873-3719
Published Online:09 May 2012

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