Synthesis and structure of an open-type trinuclear molybdenum cluster compound [Mo3(μ3-S)(μ-S)2-(μ-OAc)(S2CNC4H8)3(O)2] · 0.5CH2Cl2 · 2H2O

The title compound was prepared by the reaction of Mo3S4(dtp)4(H2O) [dtp =S2P(OEt)2] with NaOAc·3H2O and C4H2NCS2NH4. Crystallographic data: [Mo3(μ-S)(μ-S)2(μ-OAc)-(S2CNC4H2)3(O)2] · 0.5CH2Cl2 · 2H2O,Mr=980.18, triclinic, space group P1, a =12.360(3), b =16.653(6), c =9.206(2) A, α =101.97(2), β =108.32 (2), γ =86.14(3)°. V=1759.6(9)A2, Z =2, Dc =1.85 g/cm2, F(000) =962, μ(Mo Kα) =16.53 cm−1. Final R =0.044 for 4301 reflections with I>3σ (I). This compound may be regarded as a mixed-valent trinuclear molybdenum cluster {Mo3(V) Mo(V) (μ2-S) (μ-S)2-(μ-OAc) (S2CNC4H8)3 (O)2}. The Mo—Mo distances are 2.783(1), 2.833(1) and 3.374(2)A in the Mo3 non-equilateral triangle and there exist only two Mo—Mo bonds. The cluster was obtained by oxidation and ligand substitution of {Mo2(μ2-S) (μ-S)2[μ-S2P(OEt)2)] [S2P(OEt)2]3 (H2O)}.