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The diethyl dithiophosphate complex of tetraphenylantimony(V) and its solvated form, [Sb(C6H5)(4){S2P(OC2H5)(2)}] center dot 1/2 C6H6: Synthesis, crystal structure, and C-13, P-31 CP/MAS NMR study: an example of monodentate coordination of dithio ligands
Institute of Geology and Nature Management, Far East Branch, Russian Academy of Sciences, Blagoveshchensk.
Institute of Chemistry, Far Eastern Branch of the Russian Academy of Sciences, 690022, Vladivostok.
Institute of Geology and Nature Management, Far East Branch, Russian Academy of Sciences, Blagoveshchensk.
Institute of Comprehensive Exploitation of Mineral Resources, Russian Academy of Sciences, Kryukovsky Tupik 4, Moscow.
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2013 (English)In: Russian Journal of Inorganic Chemistry, ISSN 0036-0236, E-ISSN 1531-8613, Vol. 58, no 2, p. 197-205Article in journal (Refereed) Published
Abstract [en]

The O,O'-diethyl dithiophosphate complex of tetraphenylantimony(V) [Sb(C6H5)(4){S2P(OC2H5)(2)}] (I) and its benzene-solvated form I center dot 1/2C(6)H(6) (II) were synthesized and studied by high-resolution solid-state C-13 and P-31 NMR (MAS NMR). The diethyl dithiophosphate (Dtph) groups in I and II were quantitatively characterized by the P-31 chemical shift anisotropy (delta(aniso)), the asymmetry parameter (eta), and the principal values of chemical shift tensors (delta (xx) , delta (yy) , delta (zz) ). The calculation of the anisotropy parameters included construction of chi(2) statistic diagrams from full P-31 MAS NMR spectra. In both complexes, the Dtph groups were found to have mainly axially symmetric P-31 chemical shift tensors (for delta (zz) < delta (xx) a parts per thousand delta (yy) ) with similar anisotropy parameters (delta(aniso) and eta), which is due to their identical S-monodentate function. According to X-ray diffraction data, II has a trigonal bipyramidal (TBP) molecular structure with Smonodentate coordination of Dtph in the TBP axial position and outer-sphere position of the benzene molecule. The desorption of the outer-sphere benzene solvent molecules from structure II, which was noted in MAS NMR experiment, passes through the formation of three intermediate solvated forms with benzene content n < 1/2.

Place, publisher, year, edition, pages
2013. Vol. 58, no 2, p. 197-205
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Physical Chemistry
Research subject
Chemistry of Interfaces
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URN: urn:nbn:se:ltu:diva-10790DOI: 10.1134/S0036023613020071ISI: 000315386000015Scopus ID: 2-s2.0-84879667528Local ID: 9a735682-8cfd-45de-bd89-1c261b08744eOAI: oai:DiVA.org:ltu-10790DiVA, id: diva2:983737
Note
Validerad; 2013; 20130402 (andbra)Available from: 2016-09-29 Created: 2016-09-29 Last updated: 2018-07-10Bibliographically approved

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Larsson, Anna-CarinAntzutkin, Oleg

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