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AlCp*-complexes with transition metals have shown to be highly reactive and enable C-H or Si-H bond activation. Yet, complexes of AlCp* with low-valent main-group metals are scarce. Here, we report the syntheses of [M(AlCp*)3][Al(ORF)4] (RF = C(CF3)3) with M = Ga, In, Tl, which include the first covalent Al-In and Al-Tl bonds. For M = Ga, AlCp*-coordination induced the formation of the dication [Ga2(AlCp*)6]2+ in the solid state, which exhibits a solvent and temperature dependent monomer-dimer equilibrium in solution. By contrast, the In a
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