Reactions of Group 13 Organometallics t Bu 3 M with Distibanes Sb 2 R 4

Tetraalkyldistibanes Sb 2 R 4 (R = n Pr, i Bu) react with t Bu 3 M (M = Al, Ga) at –30 °C with the formation of the Lewis acid–base adducts [ t Bu 3 M] 2 [Sb 2 R 4 ] [M = Al, R = n Pr ( 1 ), i Bu ( 2 ); M = Ga, R = n Pr ( 3 ), i Pr 4 )]. Compounds 1 and 2 are stable in solution whereas 3 undergoes a Sb–Sb bond‐breakage reaction with the subsequent formation of [ t Bu 2 GaSb( n Pr) 2 ] 2 ( 5 ). The same trend was observed for the reaction of Sb 2 ( i Bu) 4 with t Bu 3 Ga, which yielded the heterocyclic stibanylgallane [ t Bu 2 GaSb( i Bu) 2 ] 2 ( 6 ). In addition, the simple trialkylstibane adduct t Bu 3 Al–Sb( i Bu) 3 ( 7 ) was obtained as a byproduct from the reaction of Sb 2 ( i Bu) 4 with t Bu 3 Al. Compounds 1 – 7 were characterized by multinuclear NMR ( 1 H, 13 C{ 1 H}) and mass spectroscopy and elemental analysis. Compounds 1 , 3 , 5 , and 7 were also investigated by single‐crystal X‐ray diffraction. (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2007)