The Sodium Siloxides (tBu3SiONa)4 and (tBu2PhSiONa)4: Synthesis and X-ray Crystal Structure Analysis

The sodium siloxides ( t Bu 3 SiONa) 4 and ( t Bu 2 PhSiONa) 4 can be synthesized almost quantitatively from the reaction of the sodium silanides t Bu 3 SiNa and t Bu 2 PhSiNa with N 2 O in tetrahydrofuran at −78 °C. ( t Bu 3 SiONa) 4 and ( t Bu 2 PhSiONa) 4 are the first structurally characterized sodium siloxides featuring a heterocubane framework in the solid state. X-ray quality crystals of the supersilanol, t Bu 3 SiOH (monoclinic, C 2/ c ), were obtained from the thermolysis of t Bu 3 SiNaN−N NSi t Bu 3 in the presence of water.