DIPHENYLANTIMONY(V) OXO CHLORO CARBOXYLATES AND PHOSPHINATES - CRYSTAL-STRUCTURES OF (SBPH(2)CL[O2P(C6H11)(2)])O-2 AND [SBPH(2)(O(2)CPH)(2)]O-2/

Reaction of SbPh(2)Cl(3) (1 mol) with the silver salt of dicyclohexylp hosphinic acid (2 mol) afforded {SbPh(2)Cl[O2P(C6H11)(2)]}O-2 1, a sim ilar 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 o r 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). Interco nversion 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 spe ctroscopy. Compounds 1 and 3 were further characterized by X-ray diffr action; the antimony in 1 is six-co-ordinated with bridging phosphinat es whereas in 3 it is seven-co-ordinated with chelating benzoates. Sho rt Sb-O (oxo) distances (1.923 Angstrom) and near linearity at the bri dging oxygen (Sb-O-Sb 173.9 degrees) are observed for 3.