Add time:09/04/2019         Source:sciencedirect.com

Crystalline O,O′-di-cyclo-hexyl dithiophosphate (Dtph) tetraphenylantimony(V) complex, [Sb(C6H5)4{S2P(O-cyclo-C6H11)2}] (1) was prepared and studied by means of heteronuclear (31C, 31P) CP MAS NMR spectroscopy, single-crystal X-ray diffraction and thermal analysis. To characterise quantitatively the phosphorous site in complex 1, 31P chemical shift anisotropy parameters (δaniso and η) were successfully defined from spinning sideband manifolds in experimental MAS NMR spectra. The positive sign of the calculated δaniso unambiguously reveals the terminal S,S′-chelating structural function of di-cyclo-hexyl Dtph groups; whereas, the minimal δ22 value among all presently known tetraphenylantimony(V) dialkyl Dtphs points out to extremely low value of the S–P–S angle. Distorted octahedral molecular structure comprising Dtph ligand with S,S′-bidentate chelating coordination mode has been established for the prepared complex. Therefore, in comparison with tetraphenylantimony(V) Dtph complexes containing S-unidentately coordinated Dtph groups, terminally chelating di-cyclo-hexyl Dtph ligand of crystalline complex 1 expectedly exhibits the smallest S–P–S angle of 113.49°. The thermal behaviour of this compound was studied by means of thermal analysis technique as a combination of TG and DSC. The thermal decomposition involves the organic and inorganic parts of 1, yielding almost equal quantities of Sb2S3 and SbPO4, which were identified using powder XRD.

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