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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, O. N. (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, Volume 368 (Number 1). pp. 263-270. doi:10.1016/j.ica.2011.01.006 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 | ||||
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| Subjects: | Q Science > QC Physics Q Science > QD Chemistry |
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| Divisions: | Faculty of Science, Engineering and Medicine > Science > Physics | ||||
| Library of Congress Subject Headings (LCSH): | Pyridine, Dithiocarbamates, Transition metals, Thermochemistry, Cadmium, Nuclear magnetic resonance spectroscopy | ||||
| Journal or Publication Title: | Inorganica Chimica Acta | ||||
| Publisher: | Elsevier Science SA | ||||
| ISSN: | 0020-1693 | ||||
| Official Date: | 15 March 2011 | ||||
| Dates: |
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| Volume: | Volume 368 | ||||
| Number: | Number 1 | ||||
| Page Range: | pp. 263-270 | ||||
| DOI: | 10.1016/j.ica.2011.01.006 | ||||
| Status: | Peer Reviewed | ||||
| Publication Status: | Published | ||||
| Access rights to Published version: | Restricted or Subscription Access | ||||
| Funder: | Rossiĭskiĭ fond fundamentalʹnykh issledovaniĭ [Russian Foundation for Basic Research] (RFBR), Luleå tekniska universitet [Luleå University of Technology], Sweden. Forskningsrådsnämnden [Swedish Council for Planning and Coordination of Research] (FRN) , Foundation to the memory of J.C. and Seth M. Kempe | ||||
| Grant number: | 08-03-00068-a (RFBR), JCK-2003 JCK-2307 JCK-2701 (foundation in memory of J.C. and Seth M. Kempe) |
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