Synthesis and structure of an open‐type trinuclear molybdenum cluster compound [Mo 3 (μ 3 ‐S)(μ‐S) 2 ‐(μ‐OAc)(S 2 CNC 4 H 8 ) 3 (O) 2 ] · 0.5CH 2 Cl 2 · 2H 2 O

The title compound was prepared by the reaction of Mo 3 S 4 (dtp) 4 (H 2 O) [dtp =S 2 P(OEt) 2 ] with NaOAc·3H 2 O and C 4 H 2 NCS 2 NH 4 . Crystallographic data: [Mo 3 (μ‐S)(μ‐S) 2 (μ‐OAc)‐(S 2 CNC 4 H 2 ) 3 (O) 2 ] · 0.5CH 2 Cl 2 · 2H 2 O,Mr=980.18, triclinic, space group P 1 , 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)Å 2 , Z =2, Dc =1.85 g/cm 2 , 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 {Mo 3 (V) Mo(V) (μ 2 ‐S) (μ‐S) 2 ‐(μ‐OAc) (S 2 CNC 4 H 8 ) 3 (O) 2 }. The Mo—Mo distances are 2.783(1), 2.833(1) and 3.374(2)Å in the Mo 3 non‐equilateral triangle and there exist only two Mo—Mo bonds. The cluster was obtained by oxidation and ligand substitution of {Mo 2 (μ 2 ‐S) (μ‐S) 2 [μ‐S 2 P(OEt) 2 )] [S 2 P(OEt) 2 ] 3 (H 2 O)}.