TRIORGANOANTIMONY(V) DIORGANOPHOSPHINATES - CRYSTAL AND MOLECULAR-STRUCTURE OF DIPHENYLPHOSPHINATO)(HYDROXO)TRIMETHYLANTIMONY(V), EXHIBITING A POLYMERIC CHAIN SUPRAMOLECULAR SELF-ASSEMBLY THROUGH HYDROGEN-BONDS

The reaction between R3SbCl2 (R = Me, Ph) and R'2PO2Na (R' = Me, Ph) a fforded R3Sb(O2PR'(2))(2) derivatives, which were investigated by IR a nd multinuclear (H-1, C-13, P-31) NMR spectroscopy. Attempts to grow c rystals of Me3Sb(O2PPh2)(2) led to colorless needles identified by X-r ay diffractometry as Me3Sb(OH) [O(O)PPh2], produced by partial hydroly sis. Coordination around the central metal atom is distorted trigonal bipyramidal with carbon atoms of the SbMe3 unit in equatorial position s and two oxygen atoms occupying the axial positions [O--Sb--O 175.7(1 )degrees]. The two antimony-oxygen distances are significantly differe nt [Sb--O(H) 1.967(3) Angstrom, Sb--O(P) 2.235(2) Angstrom], as are th e phosphorus-oxygen bond lengths in the basically monodentate diphenyl phosphinato ligand [P double bond O 1.528(3) Angstrom, P double bond O 1.490(3) Angstrom]. The molecules are associated into polymeric chain s through intermolecular hydrogen bonds between hydrogen of the hydrox o group and oxygen double bonded to phosphorus. (C) 1997 Elsevier Scie nce Ltd.