The Sodium Siloxides (<i>t</i>Bu₃SiONa)₄ and (<i>t</i>Bu₂PhSiONa)₄:  Synthesis and X-ray Crystal Structure Analysis

Abstract

The sodium siloxides (tBu3SiONa)4 and (tBu2PhSiONa)4 can be synthesized almost quantitatively from the reaction of the sodium silanides tBu3SiNa and tBu2PhSiNa with N2O in tetrahydrofuran at −78 °C. (tBu3SiONa)4 and (tBu2PhSiONa)4 are the first structurally characterized sodium siloxides featuring a heterocubane framework in the solid state. X-ray quality crystals of the supersilanol, tBu3SiOH (monoclinic, C2/c), were obtained from the thermolysis of tBu3SiNaN−NNSitBu3 in the presence of water