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Through the reactions of ferrous thiolates with tetrathiomolybdate, we discussed thereaction pathways and possible intermediates during the formation of double-cubane type Mo-Fe-Scluster compounds. We also reported the synthesis, crystal structure, IR and magnetic susceptibi-lity measurements of the title compound 2. The crystal of 2 belongs to triclinic system, M_r=2670.3;P1; a=12.755(4)A, b=13.076(3)A, c=20.576(4) A; α=80.00 (2)°, β=81.39(2)°, γ=61.51(2)°;V=2966.3(14)A~3; Z=1; D_c=1.495 g/cm~2. Final R factor is 0.077 for 4031 observed reflections.The compound was obtained through the reaction of (Et_4N)_2[Fe_4(SPh)_(10)] (1) with (Et_4N)_2MoS_4 inacetonitrile solution. The structure of anion 2 is two cubane clusters bridged by a Fe(SPh)_6 group.The Mo…Mo′ distance of 7.188A is the longest among all double-cubane cluster compounds ofknown structures.
Through the reactions of ferrous thiolates with tetrathiomolybdate, we discussed thereaction pathways and possible intermediates during the formation of double-cubane type Mo-Fe-Scluster compounds. We also reported the synthesis, crystal structure, IR and magnetic susceptibility measurements of the title Compound 2. The crystal of 2 belongs to triclinic system, M_r = 2670.3; P1; a = 12.755 (4) A, b = 13.076 (3) A, c = 20.576 (4) A; β = 81.39 (2) °, γ = 61.51 (2) °; V = 2966.3 (14) A~3; Z = 1; D_c = 1.495 g / cm~2. Final R factor is 0.077 for 4031 observed reflections. compound was obtained through the reaction of (Et_4N) _2 [Fe_4 (SPh) _ (10)] with (Et_4N) _2MoS_4 inacetonitrile solution. The structure of anion 2 is two cubane clusters bridged by a Fe (SPh) _6 group The Mo ... distance of 7.188A is the longest among all double-cubane cluster compounds of known structures.