Synthesis of the scandium chloride hydrates ScCl3·3H2O and Sc2Cl4(OH)2·12H2O and their characterisation by X-ray diffraction, 45Sc NMR spectroscopy and DFT calculations
Author:
Bräuniger Thomas1, Bielec Philipp1, Zeman Otto E. O.1, Moudrakovski Igor L.2, Hoch Constantin1, Schnick Wolfgang1
Affiliation:
1. Department of Chemistry , University of Munich (LMU) , Butenandtstr. 5–13, 81377 Munich , Germany 2. Max-Planck-Institute for Solid-State Research , Heisenbergstr. 1, 70569 Stuttgart , Germany
Abstract
Abstract
The compounds ScCl3·3H2O (SCTH) and [{Sc(H2O)5(μ-OH)}2]Cl4·2H2O (SCOH), have been synthesised and characterised by single-crystal XRD, 45Sc NMR spectroscopy and DFT calculations, with the crystal structure of SCTH reported here for the first time. From 45Sc NMR measurements under static and MAS conditions, both chemical shift and quadrupolar coupling parameters have been determined. The quadrupolar coupling constants χ for the octahedrally coordinated scandium sites in SCTH are 2.0 ± 0.1 MHz for Sc(1) and 3.81 ± 0.05 MHz for Sc(2). For SCOH, where the hepta-coordination of the single scandium site constitutes a less symmetric electronic environment, 14.68 ± 0.05 MHz was found. DFT calculations for the static SCTH structure consistently overestimate the quadrupolar coupling constants, indicating the possible presence of crystal water dynamics on the NMR time scale.
Publisher
Walter de Gruyter GmbH
Subject
General Chemistry
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