Diphenylantimony(V) oxo/chloro carboxylates and phosphinates: crystal structures of {SbPh2Cl[O2P(C6H11)2]}2O and [SbPh2(O2CPh)2]2O
作者:Musa A. Said、K. C. Kumara Swamy、Kamlesh Babu、K. Aparna、M. Nethaji
DOI:10.1039/dt9950002151
日期:——
Reaction of SbPh(2)Cl(3) (1 mol) with the silver salt of dicyclohexylphosphinic acid (2 mol) afforded SbPh(2)Cl[O2P(C6H11)(2)]}O-2 1, a similar reaction with AgO2P(C8H15)(2) gave a product formulated as SbPh(2)Cl[O2P(C8H15)(2)]}O-2 2. Similar reactions with silver carboxylates (1:3 stoichiometry) led to the crystalline derivatives [SbPh(2)(O(2)CR)(2)]O-2 (R = Ph 3, CHPh(2) 4, 2,4,6-Me(3)C(6)H(2) 5, 2-MeC(6)H(4) 6 or 4-MeC(6)H(4) 7), whereas the 1:2 reaction afforded crystalline SbPh(2)Cl(O(2)CR)(2) (R = Ph 8, 2-MeC(6)H(4) 9 or 4-MeC(6)H(4) 10). Interconversion of the previously known compounds [SbPh(2)(O(2)CMe)(2)]O and Sb(4)Ph(8)O(6) . 3MeCO(2)H was achieved and established by H-1 NMR spectroscopy. Compounds 1 and 3 were further characterized by X-ray diffraction; the antimony in 1 is six-co-ordinated with bridging phosphinates whereas in 3 it is seven-co-ordinated with chelating benzoates. Short Sb-O (oxo) distances (1.923 Angstrom) and near linearity at the bridging oxygen (Sb-O-Sb 173.9 degrees) are observed for 3.
Dinuclear and Tetranuclear Cages of Oxodiphenylantimony Phosphinates: Synthesis and Structures
作者:Musa A. Said、K. C. Kumara Swamy、Damodara M. Poojary、Abraham Clearfield、M. Veith、V. Huch
DOI:10.1021/ic950713w
日期:1996.1.1
)](2)O (4) was isolated and characterized. Treatment of 2 with acetic acid/water affords the tetranuclear cage Ph(8)Sb(4)O(4)(OH)(2)(O(2)P(C(6)H(11))(2))(2).CH(3)COOH.CH(2)Cl(2) (5); it is possible to convert 5 to 2 by heating it with an excess of the phosphinic acid. Compounds2, 3, and 5 have been characterized by X-ray structural analysis. All of them possess four membered Sb(2)O(2) rings with hexacoordinated