Synthesis and structure of an open-type trinuclear molybdenum cluster compound[Mo_3(μ_3-S)(μ-S)_2-(μ-OAc)(S_2CNC_4H_8)_3(O)_2]·0.5CH_2Cl_2·2H_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)(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)}.

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) Å, α =101.97(2), β =108.32 (2), γ =86.14(3)°. V=1759.6(9)Ų, Z =2, Dc =1.85 g/cm², F(000) =962, μ(Mo K_α) =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)Å 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)}.