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Crystalline O,O′-di-sec-butyl and O,O′-diethyl dithiophosphate platinum(II) complexes : synthesis, 13C and 31P CP/MAS NMR, single crystal X-ray diffraction studies and thermal behaviour

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Rodina, Tatyana A., Ivanov, A. V., Gerasimenko, Andrey V., Lutsenko, Irina A., Ivanov, Maxim A., Hanna, John V., Antzutkin, O. N. (Oleg N.) and Sergienko, V. I. (Valentin Ivanovich). (2011) Crystalline O,O′-di-sec-butyl and O,O′-diethyl dithiophosphate platinum(II) complexes : synthesis, 13C and 31P CP/MAS NMR, single crystal X-ray diffraction studies and thermal behaviour. Polyhedron, Vol.30 (No.13). pp. 2210-2217. ISSN 02775387

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Abstract

Crystalline bis(O,O'-di-sec-butyldithiophosphato)platinum(II) was prepared and studied by means of (13)C, (31)P CP/MAS NMR spectroscopy and single-crystal X-ray diffraction. The unit cell of the platinum(II) compound is comprised of one centrosymmetric mononuclear molecule [Pt{S(2)P(O-sec-C(4)H(9))(2)}(2)], in which the dithiophosphate groups display structural equivalence in both (31)P NMR and XRD data. A pair of the dithiophosphate ligands exhibit the same S,S'-bidentate chelating structural function and form two planar four-membered chelate rings, [PtS(2)P], in this molecule. The planar configuration of the [PtS(4)] chromophore in structure 1 is governed by the dsp(2)-hybrid state of platinum(II). The structural states of the dithiophosphate groups in two different samples of complex 1 (one crystallised from ethanol and the other one precipitated from an aqueous solution) are all characterised by almost rhombic (31)P chemical shift tensors. The observed essential dispersion of the (31)P NMR chemical shift is caused by a coexistence of six optical isomers of molecule 1. The thermal behaviour of this compound was studied by means of simultaneous thermal analysis (a combination of TG and DSC) under an argon atmosphere. The thermal behaviour shows that the mass of 1 is lost in three steps, involving successive thermal decompositions of the organic and inorganic parts of this compound with platinum(II) dithio-meta-phosphate and reduced metallic platinum as the intermediate and the final products, respectively. (C) 2011 Elsevier Ltd. All rights reserved.

Item Type: Journal Article
Subjects: Q Science > QC Physics
Q Science > QD Chemistry
Divisions: Faculty of Science > Physics
Library of Congress Subject Headings (LCSH): Crystallography, Crystals -- Thermal properties, Nuclear magnetic resonance spectroscopy, Thermal analysis, Anisotropy
Journal or Publication Title: Polyhedron
Publisher: Pergamon
ISSN: 02775387
Official Date: 2011
Volume: Vol.30
Number: No.13
Page Range: pp. 2210-2217
Identification Number: 10.1016/j.poly.2011.05.050
Status: Peer Reviewed
Publication Status: Published
URI: http://wrap.warwick.ac.uk/id/eprint/38403

Data sourced from Thomson Reuters' Web of Knowledge

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