The new thioantimonate [Ni(en)(tren)]4Sb14S25 (1) (tren = tris(2-aminoethyl)amine, en = ethylendiamine) was synthesized under solvothermal conditions using the complex [Ni(en)3]Cl2 as a structure-directing molecule in a slurry of Sb, S and tren as solvent. Under these reaction conditions two of the three en ligands in the [Ni(en)3]Cl2 complex are exchanged by one tren molecule. Compound 1 crystallises in the monoclinic space group P21/c with 4 formula units in the unit cell. Four unique Ni2+ complexes are chelated by one tetradentate tren and one bidentate en molecule. The three-dimensional 3∞[Sb14S25]8− anion is constructed by interconnection of [SbS3] and [SbS4] units forming [Sb2S2], [Sb3S3], [Sb14S14] and [Sb20S20] heterorings as the next hierarchical building groups. The two largest rings are condensed to form the three-dimensional thioantimonate(III) anions. Three different types of channels are identified with diameters of about 7 × 9, 9 × 17, and 8 × 9 Å. The Ni2+ complexes occupy the channels and are located above and below the [Sb14S14] and [Sb20S20] heterorings.
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