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The new thioantimonate [Mg(en) 3 ][Sb 4 S 7 ] containing for the first time a [Mg(en) 3 ] 2+  cation as structure-directing unit was synthesized under solvothermal conditions applying elemental Mg, SbCl 3 , S and ethylenediamine. The compound crystallizes in the monoclinic space group P2 1 /c with a = 9.9267(6), b = 14.254(1), c = 17.259(1) A° , β = 102.611(7)°, V = 2383.1(3) °A 3 , Z = 4. In the structure trigonal SbS 3  pyramids are joined to form an Sb 3 S 3  ring. The rings are connected through SbS 3  units yielding an undulated chain anion running along [001]. Considering so-called secondary Sb-S bonds, a layer-like thioantimonate anion is formed. The [Mg(en) 3 ] 2+  cations are located between the layers. Relatively short S・ ・ ・H-N contacts suggest hydrogen bonding interactions between the cation and the [Sb 4 S 7 ] 2−  anion. The compound starts to decompose at about 220 °C. The optical band gap of 2.35 eV is in agreement with the orange color of the crystals. In the Raman spectrum prominent Sb-S resonances are seen between 250 and 400 cm −1  which can be assigned to different Sb-S vibrations

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Solvothermal Synthesis, Crystal Structure and Properties of [Mg(en) 3 ][Sb 4 S 7 ] – the First Thioantimonate(III) Containing a Main Group Metal Complex Cation as Structure Director