The two novel thioantimonate(III) compounds [Co(C6H18N4)]2Sb4S81 and [Co(C6H18N4)]2Sb2S52 were synthesised under solvothermal conditions by reacting elemental Co, Sb and S in a 95% solution of tris(2-aminoethyl)amine (tren). Compound 1 crystallises in the monoclinic space group P21/c, a = 17.936(4) Å, b = 13.442(3) Å, c = 14.000(3) Å, β = 101.73(3)°, and compound 2 crystallises in the monoclinic space group C2/c, a = 30.157(6) Å, b = 7.720(2) Å, c = 22.875(8) Å, β = 94.68(3)°. The [Sb4S8]4− anion in compound 1 is composed of two SbS3 and two SbS4 units. The two SbS4 moieties share a common edge and each SbS4 has a common edge with a SbS3 pyramid. This interconnection leads to the formation of three Sb2S2 heterorings. The two remaining terminal S atoms of the anion are bound in a monodentate fashion to the [Co(C6H18N4)]2+ cation. The [Sb2S5]4− anion in 2 is formed by two corner linked SbS3 units. Two terminal S atoms are bound to the [Co(C6H18N4)]2+ cation in a monodentate manner. Compounds 1 and 2 are the first compounds that contain thioantimonate(III) anions acting as bridging ligands. Both compounds start to decompose at about 240 °C due to the removal of the organic ligands. In the X-ray powder patterns of the decomposition products Sb2S3, CoSbS and CoS could be identified.
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