Add time:07/15/2019         Source:sciencedirect.com

The compounds bis(diorganomonothiophosphinato)trimethylantimony(V), Me3Sb(OSPR2)2, where R = Me, Et and Ph, have been prepared and characterized by IR, multinuclear (1H, 13C, 31P) NMR spectroscopy and mass spectrometry. The structure of Me3Sb(OSPPh2)2 has been determined by single-crystal X-ray diffraction. The crystal consists of discrete monomers. In the molecule there is a trigonal bipyramidal environment around antimony, with the two monothio ligands bound to the metal only through oxygen atoms (SbO(1), 2.107(5) Å; SbO(2), 2.114(5) Å. The antimony—sulphur distances, i.e. 3.924 and 3.998 Å, are consistent with non-bonding van der Waals contacts (ca. 4.0 Å). The average bond distances within the phosphorus ligand are PO = 1.552, PS = 1.945 and PC = 1.808 Å. The SbC3 unit is planar, and the angle between the axial SbO bonds is 177.7(2)°. Coordination of the monothiophosphinato ligand in monodentate mode is unusual; such ligands usually exhibit chelate or bridging coordination through both oxygen and sulphur atoms.

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