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A pyridine adduct of bis(di-iso-butyldithiocarbamato-S,S′)cadmium(II) : multinuclear (13C, 15N, 113Cd) CP/MAS NMR spectroscopy, crystal and molecular structure, and thermal behaviour
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Rodina, Tatyana A., Ivanov, Alexander V., Gerasimenko, Andrey V., Ivanov, Maxim A., Zaeva, Anna S., Philippova, Tatyana S. and Antzutkin, Oleg N.. (2011) A pyridine adduct of bis(di-iso-butyldithiocarbamato-S,S′)cadmium(II) : multinuclear (13C, 15N, 113Cd) CP/MAS NMR spectroscopy, crystal and molecular structure, and thermal behaviour. Inorganica Chimica Acta, Vol.368 (No.1). pp. 263-270. ISSN 0020-1693
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Official URL: http://dx.doi.org/10.1016/j.ica.2011.01.006
Abstract
Crystalline bis(N, N-di-iso-butyldithiocarbamato-S,S')(pyridine)cadmium(II) - adduct 1 was prepared and studied by means of multinuclear (13)C, (15)N, (113)Cd CP/MAS NMR spectroscopy, single-crystal X-ray diffraction and simultaneous thermal analysis (STA). In molecular structure 1, the cadmium atom coordinates with four sulphur atoms and one nitrogen atom of pyridine, forming a coordination polyhedron [CdS(4)N], whose geometry is an almost ideal tetragonal pyramidal (C(4v)). The coordinated py molecule is in the apical position, while two structurally non-equivalent di-iso-butyldithiocarbamate ligands, playing the same terminal S,S'-chelating function, define the basal plane. To characterise additionally the structural state of the cadmium atom in this fivefold coordination, (113)Cd chemical shift anisotropy (CSA) parameters, delta(aniso) and eta, were calculated from experimental MAS NMR spectra that revealed an almost axially symmetric (113)Cd chemical shift tensor. From a combination of TG and DSC measurements taken under an argon atmosphere, we found that the mass of adduct 1 is lost in two steps involving initial desorption of coordinated py molecules with subsequent thermal destruction of liberated cadmium(II) di-iso-butyldithiocarbamate, with yellow-orange, fine-powdered solid CdS as the final product. (C) 2011 Elsevier B.V. All rights reserved.
| Item Type: | Journal Article |
|---|---|
| Subjects: | Q Science > QC Physics |
| Divisions: | Faculty of Science > Physics |
| Journal or Publication Title: | Inorganica Chimica Acta |
| Publisher: | Elsevier Science SA |
| ISSN: | 0020-1693 |
| Date: | 15 March 2011 |
| Volume: | Vol.368 |
| Number: | No.1 |
| Page Range: | pp. 263-270 |
| Identification Number: | 10.1016/j.ica.2011.01.006 |
| Status: | Peer Reviewed |
| Publication Status: | Published |
| Access rights to Published version: | Restricted or Subscription Access |
| Funder: | Russian Foundation for Basic Research , Lulea University of Technology , Swedish Council for Planning and Coordination of Research (FRN) , foundation in memory of J.C. and Seth M. Kempe |
| Grant number: | 08-03-00068-a (Russian Foundation for Basic Research), JCK-2003 JCK-2307 JCK-2701 (foundation in memory of J.C. and Seth M. Kempe) |
| URI: | http://wrap.warwick.ac.uk/id/eprint/41594 |
Data sourced from Thomson Reuters' Web of Knowledge
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