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The synthesis and molecular structures of tris(pentamethylphenyl)aluminum, (C6Me5)3Al, (I), and the magnesium cluster [Mg6(μ3-OH)2(μ3-Br)2(μ2-Br)8(OEt2)8] (II), are reported. Both compounds were isolated from the same system. The aluminum atom in (I) resides in an almost idealized trigonal planar environment. The dihedral angles of the pentamethylphenyl rings relative to the AlC3plane in (I) are 67.2, 62.4, and 61.2°. The neutral magnesium cluster, (II), is interesting in that contains six magnesium atoms each of which resides in octahedral environments.