A one-pot synthesis of the tetrasilatetrahedrane (tBu(3)Si)(4)Si-4 was achieved by the reaction of HSiCl3 and Na[SitBu(3)]. In this reaction the silane tBu(3)SiH was obtained along with (tBu(3)Si)(4)Si-4 and tBu(3)SiSitBu(3). The tetrasilatetrahedrane (tBu(3)Si)(4)S-4 was also obtained via a one-pot approach by treatment of Cl3SiSiCl3 or Cl3SiSiCl2SiCl3 with Na[SitBu(3)]. In the reaction of HSiCl3 with Na[SitBu(3)], two molecules of the tetrasilatetrahedrane (tBu(3)Si)(4)Si-4 crystallize together with one molecule a tBu(3)SiSitBu(3) and one molecule of benzene. Single crystals suitable for X-ray diffraction composed of one molecule of (tBu(3)Si)(4)Si-4 and two molecules of benzene were obtained by recrystallization from benzene.
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