Aspects of the synthesis of metallophenylsiloxanes using crystal solvates of cyclic sodium organosilanolates

Abstract

Metallosiloxane (II) is unstable and disproportionates to form insoluble (IIl) with a metal content greater than (II) and siloxane (IV), which does not contain the metal. Found for (III) with M = Co: Si 13.62; Co 28.68%. Calculated: Si 13.76; Co 28.88%. Found for (III) with M = Cu: Si 13.31; Cu 30.28%. Calculated: Si 13.45; Cu 30.45%. Product (IV) is a crystalline octaphenylsilsesquioxane which is a cube having four-unit eyclosiloxane fragments at the base and the sides [2]. The structure of (IV) was supported by x-ray diffraction structural analysis by comparison of the unit cell parameters of crystals of the compound obtained with a reference, (C6HsSiOi.5)e. Comparison of the structure of the starting compound (I) containing trisiloxane cyclic fragments with the structure of (IV), which contains tetrasiloxane rings, indicates complete rearrangement of the siloxane fragments of the starting compound as a result of disproportionation.