Abstract: The structure of triphenylstibine oxide has long been the subject of considerable controversy in the chemical literature. Crystals, obtained by the slow cooling of a xylene solution of the crystalline form of the compound I, were subjected to a single-crystal X-ray analysis and shown to exist as a dimer with a four-membered ring containing Sb-0-Sb linkages. Molecular weight determinations and the infrared spectrum showed that this ...