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Chalcogenidoarsenate materials have attracted much attention for their potential applications such as optical nonlinearity,electrical,and ion–exchange materials.1,2 Two new transition-metal thioarsenates [Cr(trien)(AsS3)](1)and [Cr(en)2(AsS3)](2)(en = ethylenediamine)were solvothermally prepared by reaction of CrCl3·6H2O with As2O3 and S in polyamines.