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A one-pot synthesis of the tetrasilatetrahedrane (tBu3Si)4Si4 was achieved by the reaction of HSiCl3 and Na[SitBu3]. In this reaction the silane tBu3SiH was obtained along with (tBu3Si)4Si4 and tBu3SiSitBu3. The tetrasilatetrahedrane (tBu3Si)4Si4 was also obtained via a one-pot approach by treatment of Cl3SiSiCl3 or Cl3SiSiCl2SiCl3 with Na[SitBu3]. In the reaction of HSiCl3 with Na[SitBu3], two molecules of the tetrasilatetrahedrane (tBu3Si)4Si4 crystallize together with one molecule of tBu3SiSitBu3 and one molecule of benzene. Single crystals suitable for X-ray diffraction composed of one molecule of (tBu3Si)4Si4 and two molecules of benzene were obtained by recrystallization from benzene.
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Meyer‐Wegner et al. (2009) studied this question.
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