Novel Drums and Mixed-Drum Organooxotin Clusters from Carboxylic, Phosphinic, and Phosphoric Acids

Abstract

A variety of new “drum” geometries were synthesized by a condensation reaction of an alkylstannonic acid with either a carboxylic acid or a phosphorus-based acid. The structures of [MeSn(O)O2CMe]6(1), [(MeSn(O)O2CMe)(MeSn(O)O2P(t-Bu)2)]3(2), and [n-BuSn(O)O2P(OPh)2]6(3) were revealed by X-ray analysis. Interestingly, the mixed-drum composition 2 resulted from the reaction of the drum formulation 1 with di-tert-butylphosphinic acid. Also an oxygen-capped cluster [(n-BuSn(OH)O2P-(OPh)2)3O] [(PhO)2PO2] (8) is formed when the same reaction that was used to prepare 3 is conducted at 25 °C rather than at reflux. 1 crystallizes in the rhombohedral space group R3 with aH= 17.420 (5) Å, cH= 9.963 (2) Å, and Z = 3. 2 crystallizes in the monoclinic space group C2/c with a = 21.495 (4) Å, b = 28.032 (6) Å, c = 10.013 (2) Å, β = 95.34 (2)°, and Z = 4. 3 crystallizes in the monoclinic space group P21/n with a = 14.252 (3) Å, b = 17.346 (2) Å, c = 21.987 (3) Å, β = 91.62 (1)°, and Z = 2. The conventional unweighted residuals were 0.023 (1), 0.036 (2), and 0.040 (3). © 1988, American Chemical Society. All rights reserved.