The antimony aryloxide compound [κ4-N(CH2ArBu2tO)3]Sb may be readily obtained via the reaction of Sb(OEt) 3 with tris(3,5-di-t-butyl-2-hydroxybenzyl)amine, N(CH2ArBu2tOH)3.[κ4-N(CH2ArBu2tO)3]Sb forms the adduct [κ4-N(CH2ArBu2tO)3]Sb(OSMe2) upon treatment with Me 2 SO, and comparison of the molecular structure of [κ4-N(CH2ArBu2tO)3]Sb(OSMe2) with that of [κ 4 -N(o-C 6 H 4 O) 3 ]Sb(OSMe 2 ) demonstrates that the Sb–OSMe 2 bond length in the former complex is significantly longer than that in the latter. This observation indicates that the [κ4-N(CH2ArBu2tO)3] ligand engenders a less Lewis acidic antimony center than does [κ4-N(o–C6H4O)3]. [κ4-N(CH2ArBu2tO)3]Sb exhibits diverse reactivity. For example, treatment of [κ4-N(CH2ArBu2tO)3]Sb with AcOH cleaves one of the Sb–O bonds to give [κ3-N(CH2ArBu2tO)2(CH2ArBu2tOH)]Sb(κ1-O2CMe), Br 2 undergoes oxidative addition to give N(CH2ArBu2tO)3]SbBr2, while Me 3 NO·2H 2 O yields the oxo and hydroxo complexes {[κ4-N(CH2ArBu2tO)3]Sb(μ-O)}2, [κ4-N(CH2ArBu2tO)3]Sb(OH)2, and {[κ4-N(CH2ArBu2tO)3]SbVO}4{Sb4IIIO6}.