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Reactions of[NH_4]_2[MS_4](M=Mo,W),AgX(X=Cl,Br,I,CN,SCN)and PPh_3in the solid state produced six new mixed-metal sulfur containing cluster compounds,two ofwhich,{Ag_3MoS_3I}(PPh_3)_3S(1)and{Ag_3WS_3Cl}(PPh_3)_3S·0.5P(S)Ph_3·3H_2O(2),were determinedby single crystal X-ray analysis.The crystal data:1,triclinic,P,a=12.114(2),b=13.420(2),c=20.346(3),α=74.53(1),β=86.73(1),γ=63.74(1)°,Z=2,R=0.043 for 4805 independentdata;2,hexagonal,R3,a=b=16.201(3),c=45.091(10),Z=6,R=0.042 for 2729 independentdata.The central unit{Ag_3MS_3X}(M=Mo,W;X=Cl,I)of the two compounds can be des-cribed as a slightly distorted cube,four corners being formed by the MS_4~(2-) ligand(with a ter-minal S atom).The remaining corners are occupied by one X(Cl or I)atom and three Agatoms(with one PPh_3 ligand bound to each of the latter).The generation of different types ofAg-Mo(W)-S cluster compounds prepared from solid state reactions under different reactiontemperatues is discussed.
Reactions of [NH_4] _2 [MS_4] (M = Mo, W), AgX (X = Cl, Br, I, CN, SCN) and PPh_3in the solid state produced six new mixed-metal sulfur containing cluster compounds, (PPh_3) _3S · 0.5P (S) Ph_3 · 3H_2O (2), were determined by single crystal X-ray analysis.The crystal data: 1, triclinic, P, a = 12.114 (2), b = 13.420 (2), c = 20.346 (3), α = 74.53 (1), β = 86.73 (1), γ = 63.74 (1) °, Z = 2, R = for 4805 independentdata; 2, hexagonal, R3, a = b = 16.201 (3), c = 45.091 (10), Z = 6, R = 0.042 for 2729 independentdata.The central unit {Ag_3MS_3X} X = Cl, I) of the two compounds can be des-cribed as a slightly distorted cube, four corners being formed by the MS_4 ~ (2-) ligand (with a ter-minal S atom). The remaining corners are occupied by one X (Cl or I) atom and three Agatoms (with one PPh_3 ligand bound to each of the latter). The generation of different types of Ag-Mo (W) -S cluster compounds prepared from solid state reactions under different reaction conditions is discussed.