Synthesis and structure of an open-type trinuclear molybdenum cluster compound[Mo_3(μ_3-S)(μ-S)_2-(μ

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The title compound was prepared by the reaction of Mo_3S_4(dtp)_4(H_2O)[ctp=S_2P(OEt)_2]with NaOAc·3H_2O and C_4H_8NCS_2NH_4.Crystallographic data:[Mo_3(μ_3-S)(μ-S)_2(μ-OAc)-(S_2CNC_4H_8)_3(O)_2]·0.5CH_2CI_2·2H_2O,Mr=980.18,triclinic,space group P,α=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)A~3,Z=2,Dc=1.85 g/cm~3,F(000)=962,μ(Mo K_α)=16.53 cm~(-1).Final R=0.044 for 4301 reflections with I≥3σ(I).This compoundmay be regarded as a mixed-valent trinuclear molybdenum cluster{Mo_2(V)Mo(Ⅳ)(μ_3-S)(μ-S)_2-(μ-OAc)(S_2CNC_4H_8)_3(O)_2}.The Mo-Mo distances are 2.783(1),2.833(1)and 3.374(2)A in the Mo_3non-equilateral triangle and there exist only two Mo-Mo bonds.The cluster was obtained by oxi-dation and ligand substitution of{Mo_3(μ_3-S)(μ-S)_3[μ-S_2P(OEt_2)][S_2P(OEt)_2]_3(H_2O)}. The title compound was prepared by the reaction of Mo_3S_4 (dtp) _4 (H_2O) [ctp = S_2P (OEt) _2] with NaOAc · 3H_2O and C_4H_8NCS_2NH_4.Crystallographic data: [Mo_3 (μ_3-S) (3), b = 16.653 (6), c = 9.206 (2) μ-OAc - (S_2CNC_4H_8) _3 (O) _2] · 0.5CH_2CI_2 · 2H_2O, Mr = 980.18, triclinic, space group P, A = 101.97 (2), β = 108.32 (2), γ = 86.14 (3) °. V = 1759.6 (9) A~3, Z = 2, Dc = 1.85 g / cm~3, F = 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 {Mo_2 (V) Mo-Mo distances are 2.783 (1), 2.833 (1) and 3.374 (2), and Mo (IV) (μ_3-S) (μ-S) _2- (μ_OAc) (S_2CNC_4H_8) _3 (O) _2} ) A in the Mo_3non-equilateral triangle and there exist only two Mo-Mo bonds. The cluster was obtained by oxi-dation and ligand substitution of {Mo_3 (μ_3-S) (μ_S) _3 [μS_2P (OEt_2) ] [S_2P (OEt) _2] _3 (H_2O)}.
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