The three new thioantimonates(V) [Ni(chxn)3]3(SbS4)2·4H2O (I), [Co(chxn)3]3(SbS4)2·4H2O (II) (chxn is trans‐1,2‐diaminocyclohexane) and [Co(dien)2][Co(tren)SbS4]2·4H2O (III) (dien is diethylenetriamine and tren is tris(2‐aminoethyl)amine) were synthesized under solvothermal conditions. Compounds I and II are isostructural crystallizing in space group C2/c. The structures are composed of isolated [M(chxn)3]2+ complexes (M = Ni, Co), [SbS4]3− anions and crystal water molecules. Short S···N/S···O/O···O separations indicate hydrogen bonding interactions between the different constituents. Compound III crystallizes in space group $P{\bar 1}$ and is composed of [Co(dien)2]2+ and [Co(tren)SbS4]− anions and crystal water molecules. In the cationic complex the Co2+ ion is in an octahedral environment of two dien ligands whereas in [Co(tren)SbS4]− the Co2+ ion is in a trigonal bipyramidal coordination of four N atoms of tren and one S atom of the [SbS4]3− anion, i.e., two different coordination polyhedra around Co2+ coexist in this compound. Like in the former compounds an extended hydrogen bonding network connects the complexes and the water molecules into a three‐dimensional network.
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