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A fixation mode of gold from solutions using heterogeneous reaction of cadmium dicyclohexyl dithiophosphate with H[AuCl4]. Structural and (13C, 31P) CP/MAS NMR studies and thermal behaviour of crystalline polymeric gold(I) dicyclohexyl dithiophosphate and bis(dicyclohexylthiophosphoryl) disulphide
Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
Far Eastern Branch of the Russian Academy of Sciences, 675000, Blagoveschensk, Amur Region.
Far Eastern Branch of the Russian Academy of Sciences, 675000, Blagoveschensk, Amur Region.
Institute of Chemistry, Far Eastern Branch of the Russian Academy of Sciences, 690022, Vladivostok.
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2013 (English)In: Journal of Molecular Structure, ISSN 0022-2860, E-ISSN 1872-8014, Vol. 1034, p. 152-161Article in journal (Refereed) Published
Abstract [en]

Two novel compounds: polynuclear catena-poly[bis(3-O,O’-di-cyclo-hexyldithiophosphato-S,S,S’)digold(I)] (Au–Au) (1) and crystalline bis(O,O’-di-cyclo-hexylthiophosphoryl)disulphide, (cyclo-C6H11O)2P(S)S–S(S)P(O-cyclo-C6H11) (2) were prepared using heterogeneous reaction between freshly precipitated binuclear cadmium(II) dithiophosphate (Dtph), [Cd2{S2P(O-cyclo-C6H11}4] and H[AuCl4] in 2 M hydrochloric acid. The isolated compounds 1 and 2 (the fixation mode of gold from the solution and the oxidised form of Dtph groups, respectively) have been studied by means of single-crystal X-ray diffraction, 13C and 31P cross-polarisation / magic-angle-spinning (CP/MAS) NMR spectroscopy and simultaneous thermal analysis (STA). Centrosymmetric binuclear molecule of 1, [Au2{S2P(O-cyclo-C6H11)2}2] comprises a pair of -bridging di-cyclo-hexyl Dtph ligands, linking two neighbouring gold atoms, and displays additional intramolecular aurophilic bond Au···Au. At the supramolecular level of structural self-organisation of complex 1, infinite polymeric zigzag chains arise due to pairs of the secondary bonds Au···S between neighbouring binuclear molecules. Centrosymmetric molecule of 2 displays two O,O-di-cyclo-hexythiophosphoryl fragments, which are connected by the chemical bond S(1)–S(1)a, and a planar zigzag array [S=P–S–S–P=S] passing through the central part of the molecule. To characterise additionally the Dtph groups in both compounds 1 and 2, chemical shift anisotropy (CSA) parameters (aniso and) were calculated from spinning sideband manifolds in experimental 31P MAS NMR spectra. The thermal behaviour of complex 1 was studied using simultaneous thermal analysis (a combination of TG and DSC) under an argon atmosphere. The thermal behaviour displays stepwise mass loss, comprising thermal decompositions of the organic and inorganic parts of 1 with gold(I) dithio-meta-phosphate and reduced metallic gold as the intermediate and the final products, respectively.

Place, publisher, year, edition, pages
2013. Vol. 1034, p. 152-161
National Category
Physical Chemistry
Research subject
Chemistry of Interfaces
Identifiers
URN: urn:nbn:se:ltu:diva-13180DOI: 10.1016/j.molstruc.2012.08.052ISI: 000314554800021Scopus ID: 2-s2.0-84867132154Local ID: c5e6a5d3-167f-4da0-afbf-4125570049f5OAI: oai:DiVA.org:ltu-13180DiVA, id: diva2:986132
Note
Validerad; 2013; 20120914 (ysko)Available from: 2016-09-29 Created: 2016-09-29 Last updated: 2018-07-10Bibliographically approved

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Ivanov, AlexanderAntzutkin, OlegLarsson, Anna-Carin

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