Six new thioantimonates(III) with the [Sb4S7](2-) anion were obtained Under solvothermal conditions with in-situ formed transition metal complexes as Structure directors. In the two isostructural compounds [Fe(dien)(2)]Sb4S7 center dot H2O (1) and [Co(dien)(2)]Sb4S7 center dot 0.5 H2O (2) (dien = diethylenetriamine; space group: P2(1)/c) the layered [Sb4S7](2-) anion is characterized by Sb8S8 rings with a diameter of about 9.6 center dot 7.6 angstrom. The cation complexes are located above and below the pores of the rings. Despite the larger size of the cation complex the network topology of the third thioantimonate [Ni(dien)(tren)]Sb4S7 (3) (tren = tris(2-aminoethyl)amine; space group: P2(1)/n) is similar to that of the first two compounds. In the isostructual thioantimonates [M(trien)]Sb4S7 (M = Zn (4); M = Mn (5); trien = triethylenetetramine; space group: P (l) over bar) the M2+ ions are fivefold coordinated by four N atoms of the amine molecule and by one S atom of the thioantimonate anion forming a MN4S trigonal bipyramid. Sb8S16 building blocks are the central structural motifs of the anion. Two of the terminal S atoms at the periphery of the Sb8S16 units are bound to M2+ ions and the four remaining terminal S atoms connect adjacent Sb8S16 groups into the final [Sb4S7](2-) anion which is a unique feature in the thioantimonate(111) chemistry. The NiN4S2 octahedron is severly distorted with one very long Ni-S bond of 2.782(2) angstrom. In all compounds several short S ... H distances indicate hydrogen bonding interactions.

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The new thiostannate (1,4-dabH)2MnSnS4 (1,4-dab=1,4-diaminobutane) was synthesized under solvothermal conditions. The compound crystallizes in the non-centrosymmetric space group Fdd2 with a=22.8124(15)Å, b=24.7887(16)Å, c=6.4153(6)Å, Z=8, and V=3627.8(5)Å3. The structure consists of one-dimensional straight anionic chains composed of alternating SnS4 and MnS4 tetrahedra sharing common edges. The chains are directed along [001] and are surrounded by the organic cations which form undulated chains along [100] by strong intermolecular N–H⋯N hydrogen bonding interactions. Several S⋯H contacts suggest weak interactions between the anionic chains and the cations. The band gap amounts to 2.9eV indicating that the compound is a photo-conductor. The compound is stable up to about 190°C and decomposes in two distinct steps above this temperature.

The new charge neutral complex [Cr(tren)SbS3] center dot H2O was synthesized under solvothermal conditions applying CrCl3 center dot 6H(2)O, Sb2S3, and S as starting material in an aqueous tren solution (tren = tris(2-aminoethyl)amine)). The compound crystallizes in the non-centrosymmetric space group P2(1)2(1)2(1), with a = 8.7779(15), b = 10.7122(17), c = 15.4286(18) angstrom, V = 1450.8(4) angstrom(3). In the structure the Cr3+ ion is surrounded by four N atoms of the amine molecules and by two S atoms of a trigonal pyramidal [SbS3](3-) group, i.e., the latter acts as a bidentate ligand. A three-dimensional network is formed via hydrogen bonds between the complexes and water molecules. The main resonances in the Raman spectrum can be explained on the basis of calculated data. The most intense band is due to the Sb-S stretching vibration. The thermal properties were investigated by DTA-TG measurements. On heating [Cr(tren)SbS3] center dot H2O decomposes in two distinct steps. The first step corresponds to the removal of the water molecules and the second step to the loss of the tren ligand.

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