Synthesis, crystal structure and properties of μ-tetra-thio-anti-monato-bis-[(cyclam)zinc(II)] perchlorate 0.8-hydrate.

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作者:Näther Christian, Lühmann Henning, Bensch Wolfgang
The reaction of Zn(ClO(4))(2)·6H(2)O with Na(3)SbS(4)·9H(2)O in a water/aceto-nitrile mixture leads to the formation of the title compound, (μ-tetra-thio-anti-monato-κ(2) S:S')bis-[(1,4,8,11-tetra-aza-cyclo-tetra-decane-κ(4) N)zinc(II)] perchlorate 0.8-hydrate, [Zn(2)(SbS(4))(C(10)H(24)N(4))(2)]ClO(4)·0.8H(2)O or [(Zn-cyclam)(2)(SbS(4))](+)[ClO(4)](-)·0.8H(2)O. The asymmetric unit consists of two crystallographically independent [SbS(4)](3-) anions, two independent perchlorate anions and two independent water mol-ecules 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 mol-ecules are partially occupied. Two Zn(cyclam)(2+) cations are linked via the [SbS(4)](3-) anions into [Zn(2)(cyclam)(2)SbS(4)](+) cations that are charged-balanced by the [ClO(4)](-) anions. The water mol-ecules of crystallization are hydrogen bonded to the [SbS(4)](3-) anions. The cations, anions and water mol-ecules 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.

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