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A new complex, {Bi(Ⅲ)[S2CN(CH2C6H5)2]3}2·2CH3CN, was synthesized and characterized by elemental analysis, IR, TG, 1H NMR and X-ray single-crystal diffraction. The complex crystallizes in the triclinic system, space group P1, with a = 12.705(6), b = 1