Studies on solid state reactions of coordination compounds——XLⅦ.Solid state syntheses and crystal st

来源 :Chinese Journal of Chemistry | 被引量 : 0次 | 上传用户:xpzcz1994
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Reactions of [NH_4]_2[MS_4](M=Mo,W),CuX(X=Br,I)and PPh_3 in the solid state producedfour mixed-metal sulfur containing clusters{Cu_3MS_3X}(PPh_3)_3S(M=Mo,W;X=Br,I),two of which(1:M=Mo,X=I;2:M=W,X=Br)were structurally determined.Crystals of 1 and 2 are triclinic,space group P(1:a=11.895(3),b=13.107(1),c=20.473(2),α=74.95(6),β=84.87(8),γ=64.27(7)°,Z=2,V=2776.1 ,Rw=0.064 for 6443 observed reflections.2:α=11.876 (1),b=13.065 (2),c=20.325(2),α=74.95(1),β=85.39(1),γ=64.09(1)°,Z=2,V=2737.3,R_w=0.055 for 5303 observedreflections).The results of the structure determination showed that the central units of the two cubane-like cluster compounds are composed of four metal atoms and four non-metal atoms situated at alter-nate comers.The differences of cubane-like cluster compounds obtained from solid state reactions andfrom solution reactions are discussed. Reactions of [NH_4] _2 [MS_4] (M = Mo, W), CuX (X = Br, I) and PPh_3 in the solid state produced mixed metal-sulfur containing clusters {Cu_3MS_3X} (PPh_3) (1: M = Mo, X = I; 2: M = W, X = Br) were structurally determined. Crystals of 1 and 2 are triclinic, space group P : a = 11.895 (3) b = 13.107 (1) c = 20.473 (2) α = 74.95 (6) β = 84.87 (8) γ = 64.27 (7) ° Z = 2 V = 2776.1, Rw = 0.064 for 6443 observed reflections.2: α = 11.876 1, b = 13.065 2, c = 20.325 2, α = 74.95 1, β = 85.39 1, γ = 64.09 (1) °, Z = 2, V = 2737.3, R_w = 0.055 for 5303 observed reflections). The results of the structure determination showed that the central units of the two cubane-like cluster compounds are composed of four metal atoms and four non- metal atoms situated at alter-nate comers. These differences of cubane-like cluster compounds obtained from solid state reactions and from solution reactions are discussed.
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