Trimethylantimony(V) diorganomonothiophosphinates: the crystal structure of bis(diphenylmonothiophosphinato)trimethylantimony(V), Me3Sb(OSPPh2)2, containing a monodentate monothiophosphinato ligand
摘要:
The compounds bis(diorganomonothiophosphinato)trimethylantimony(V), Me3Sb(OSPR2)2, where R = Me, Et and Ph, have been prepared and characterized by IR, multinuclear (H-1, C-13, P-31) 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) angstrom; Sb-O(2), 2.114(5) angstrom. The antimony-sulphur distances, i.e. 3.924 and 3.998 angstrom, are consistent with non-bonding van der Waals contacts (ca. 4.0 angstrom). The average bond distances within the phosphorus ligand are P-O = 1.552, P=S = 1.945 and P-C = 1.808 angstrom. 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.