Syntheses of the Antimonides R2Sb− (R = Ph,Mes, tBu,tBu2Sb) and Sb73− by Reactions of Organoantimony Hydrides or cyclo‐(tBuSb)4 with Li,Na, K,or BuLi

Reactions of R₂SbH with BuLi at ?70 °C in tetrahydrofuran (thf) lead to R₂SbLi(thf)₃] R = Ph ( 1 ) or R = Mes ( 2 )]. The antimonides tBu₂SbK(pmdeta)] ( 3 ) (pmdeta = pentamethyldiethylenetriamine), Li(tmeda)₂]tBu₄Sb₃]·benzene ( 4 ) (tmeda = tetramethylethylenediamine), and tBu₄Sb₃Na(tmeda, thf)] ( 5 ) result from the reduction of cyclo‐(tBuSb)₄ by Li, Na, or K with pmdeta or tmeda in thf. The primary stibanes RSbH₂ R = Mes ( 6 ), 2‐(Me₂NCH₂)C₆H₂ ( 7 )] are synthesized by reactions of RSbCl₂ with LiAlH₄. PhSbH₂ reacts with BuLi, and tmeda in toluene to give Sb₇Li₃(tmeda)₃]·toluene ( 8 ). Sb₇Na₃(pmdeta)₃]·toluene ( 9 ) is obtained from PhSbH₂, Na in liqu. NH₃, pmdeta and toluene. Crystal structures are reported for 1 – 5 and 9 .