Complexation of lead(II) with O,O-dialkyldithiophosphate ligands: P and C CP/MAS NMR and single-crystal X-ray diffraction studies |
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Authors: | Anna-Carin Larsson Oleg N Antzutkin |
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Affiliation: | a Division of Chemistry, Luleå University of Technology, Luleå S-97187, Sweden b Amur Integrated Research Institute, Far Eastern Branch of the Russian Academy of Sciences, 675000, Blagoveschensk, Amur Region, Russia c Institute of Chemistry, Far Eastern Branch of the Russian Academy of Sciences, Vladivostok 690022, Russia |
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Abstract: | Polycrystalline lead(II) complexes with O,O′-dipropyl- and O,O′-di-cyclo-hexyldithiophosphate ions were prepared and studied by means of 31P, 31C CP/MAS NMR spectroscopy and single-crystal X-ray diffraction. Prepared complexes are characterised by polynuclear structures, in which pairs of dithiophosphate groups asymmetrically link neighbouring lead atoms, forming infinite linear zigzag chains. In spite of the same combined structural function, dithiophosphate ligands in both complexes display structural inequivalence. To characterise the combined structural state of the dialkyldithiophosphate ligands, 31P chemical shift anisotropy parameters, δaniso and η, were estimated from spinning sideband patterns in experimental CP/MAS NMR spectra for each of the two prepared complexes as well as the initial potassium O,O′-dipropyl- and O,O′-di-cyclo-hexyldithiophosphate salts. |
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Keywords: | 31P and 13C CP/MAS NMR spectroscopy 31P chemical shift anisotropy Single-crystal X-ray diffraction O,O&prime -Dialkyldithiophosphate lead(II) complexes Molecular structures |
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