Pursuing the excision of carbon-centred hexanuclear scandium clusters {CSc6} from solid {CSc6}I12Sc†
Selvan Demir
A B * , Wieland Tyrra A , Simon Schmitz A , Axel Klein A * and Gerd H. Meyer A C *
+ Author Affiliations
- Author Affiliations
A Department für Chemie, Mathematisch-Naturwissenschaftliche Fakultät, Universität zu Köln, Institut für Anorganische Chemie, Greinstraße 6, D-50939 Köln, Germany.
B Department of Chemistry, Michigan State University, 578 S Shaw Lane Room 437, East Lansing, MI 48824, USA.
C Department of Chemistry, KTH Royal Institute of Technology, Teknikringen 30, SE-100 44 Stockholm, Sweden.
Handling Editor: George Koutsantonis
Australian Journal of Chemistry 75(9) 523-531 https://doi.org/10.1071/CH21267
Submitted: 11 October 2021 Accepted: 23 November 2021 Published: 23 February 2022
© 2022 The Author(s) (or their employer(s)). Published by CSIRO Publishing.
Abstract
A multi-gram synthetic route to black solid {CSc6}I12Sc (1) was developed which comprises the reaction of scandium triiodide, ScI3, with graphite and scandium metal at 850°C. Compound 1 dissolved in N,N-dimethylacetamide (DMA) to form a red solution. Results derived from 45Sc NMR and EPR spectroscopy indicated that a scandium cluster species exists in this solution along with a complex cation [Sc(DMA)6]3+. From these solutions crystals of [Sc(DMA)6]I3 (2) and a red oily product was isolated. Compound 2 was also prepared independently by dissolving ScI3 in DMA and two polymorphs, orthorhombic 2O and monoclinic 2M were crystallised. {CSc6}I12Sc (1) also dissolved in THF yielding a red solution which contains [ScI6]3− and a scandium cluster species, as analysed by 45Sc NMR and EPR spectroscopy.
Keywords: 45Sc NMR, cluster compounds, complexes, crystal structure, endohedral C, EPR, iodide ligands, polymorphs, Scandium.
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