Synthesis, crystal structure and properties of μ-tetrathioantimonato-bis[(cyclam)zinc(II)] perchlorate 0.8-hydrate

Abstract

The reaction of Zn(ClO4)2·6H2O with Na3SbS4·9H2O in a water/acetonitrile mixture leads to the formation of the title compound, (μ-tetrathioantimonato-κ2 S:S′)bis[(1,4,8,11-tetraazacyclotetradecane-κ4 N)zinc(II)] perchlorate 0.8-hydrate, [Zn2(SbS4)(C10H24N4)2]ClO4·0.8H2O or [(Zn-cyclam)2(SbS4)]+[ClO4]−·0.8H2O. The asymmetric unit consists of two crystallographically independent [SbS4]3– anions, two independent perchlorate anions and two independent water molecules as well as four crystallographically independent Zn(cyclam)2+ cations that are located in general positions. Both perchlorate anions and one cyclam ligand are disordered and were refined with a split mode using restraints. The water molecules are partially occupied. Two Zn(cyclam)2+ cations are linked via the [SbS4]3– anions into [Zn2(cyclam)2SbS4]+ cations that are charged-balanced by the [ClO4]− anions. The water molecules of crystallization are hydrogen bonded to the [SbS4]3– anions. The cations, anions and water molecules are linked by N—H...O, N—H...S and O—H...S hydrogen bonds into a three-dimensional network. Powder X-ray diffraction proves that a pure sample had been obtained that was additionally investigated for its spectroscopic properties.