Add time:09/08/2019         Source:sciencedirect.com

The reaction between R3SbCl2 (R = Me, Ph) and R′2PO2Na (R′ = Me, Ph) afforded R3Sb(O2PR′2)2 derivatives, which were investigated by IR and multinuclear (1H, 13C, 31P) NMR spectroscopy. Attempts to grow crystals of Me3Sb(O2PPh2)2 led to colorless needles identified by X-ray diffractometry as Me3Sb(OH) [O(O)PPh2], produced by partial hydrolysis. Coordination around the central metal atom is distorted trigonal bipyramidal with carbon atoms of the SbMe3 unit in equatorial positions and two oxygen atoms occupying the axial positions [OSbO 175.7(1)°]. The two antimony-oxygen distances are significantly different [SbO(H) 1.967(3) Å, SbO(P) 2.235(2) Å], as are the phosphorus-oxygen bond lengths in the basically monodentate diphenylphosphinato ligand [PO 1.528(3) Å, PO 1.490(3) Å]. The molecules are associated into polymeric chains through intermolecular hydrogen bonds between hydrogen of the hydroxo group and oxygen double bonded to phosphorus.

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