Abstract
We report the direct preparation of two new octahedral hexanuclear molybdenum cluster complexes containing phosphine oxide ligands, namely, [Mo6(μ3-Cl)8{OP(n-Pr)3}2Cl4] and [Mo6(μ3-Cl)8(OPEt3)2Cl4], from Mo6Cl12 and the corresponding phosphine oxide ligands. Both of these complexes were characterized by NMR and IR spectroscopies, cyclic voltammetry and elemental analysis. Further, a single-crystal X-ray structure determination of [Mo6(μ3-Cl)8{OP(n-Pr)3}2Cl4] was obtained: [Mo6(μ3-Cl)8{OP(n-Pr)3}2Cl4] crystallizes in the monoclinic space group, P21/n with a = 10.0685(16) A, b = 15.617(2) A, c = 15.693(3) A, β = 91.799(5)°, and R1 = 0.0288. A trans arrangement of the phosphine oxide ligands was observed, where both ligands are bonded to the molybdenum cluster through the oxygen atoms. We also investigated the reaction of [Mo6(μ3-Cl)8{P(n-Pr)3}2Cl4] with a variety of oxidizing agents and found that the coordinated tri(n-propyl)phosphine ligands are cleanly oxidized by H2O2 to the corresponding phosphine oxides, yielding [Mo6(μ3-Cl)8{OP(n-Pr)3}2Cl4].
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