Preparation and structural organisation of heteroleptic tetraphenylantimony(V) complexes comprising unidentately and bidentately coordinated O,O′-dialkyldithiophosphate groups: Multinuclear (C, P) CP/MAS NMR and single-crystal X-ray diffraction studies |
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Authors: | Maxim A Ivanov Vladimir V Sharutin Antonya P Pakusina Willis Forsling |
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Institution: | a Institute of Geology and Nature Management, Far Eastern Branch of the Russian Academy of Sciences, 675000 Blagoveschensk, Amur Region, Russia b Division of Chemistry, Luleå University of Technology, S-97187 Luleå, Sweden c Blagoveschensk State Pedagogical University, 675000 Blagoveschensk, Amur Region, Russia d Institute of Chemistry, Far Eastern Branch of the Russian Academy of Sciences, 690022 Vladivostok, Russia |
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Abstract: | O,O′-dipropyldithiophosphate and O,O′-di-iso-butyldithiophosphate (Dtph) tetraphenylantimony(V) complexes of the general formula Sb(C6H5)4{S2P(OR)2}] (R = C3H7, i-C4H9) were prepared and studied by means of 13C, 31P CP/MAS NMR spectroscopy and single-crystal X-ray diffraction. Distorted octahedral and trigonal bipyramidal molecular structures have been established for prepared complexes. These unexpected structural distinctions between chemically related compounds are defined by the principally different coordination modes of O,O′-dipropyldithiophosphate and O,O′-di-iso-butyldithiophosphate ligands in their molecular structures (i.e., S,S′-bidentate chelating and S-unidentately coordinated, respectively). To characterise quantitatively phosphorus sites in both species of dithiophosphate ligands, 31P chemical shift anisotropy parameters (δaniso and η) were calculated from spinning sideband manifolds in MAS NMR spectra. The 31P chemical shift tensors for the bidentate chelating and unidentately coordinated dithiophosphate ligands display a profoundly rhombic and nearly axially symmetric characters, respectively. |
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Keywords: | Heteroleptic dialkyldithiophosphate tetraphenylantimony(V) complexes Molecular structures 13C 31P CP/MAS NMR spectroscopy 31P chemical shift anisotropy Single-crystal X-ray diffraction |
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