Synthesis, Crystal Structure and Properties of μ-tetra-thio-anti-monato-bis-[(cyclam)zinc(II)] Perchlorate 0.8-hydrate

Overview

Journal Acta Crystallogr E Crystallogr Commun

Date 2024 Dec 23

PMID 39712171

Authors

Christian Nather

Henning Luhmann

Wolfgang Bensch

Affiliations

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Abstract

The reaction of Zn(ClO)·6HO with NaSbS·9HO in a water/aceto-nitrile mixture leads to the formation of the title compound, (μ-tetra-thio-anti-monato-κ :')bis-[(1,4,8,11-tetra-aza-cyclo-tetra-decane-κ )zinc(II)] perchlorate 0.8-hydrate, [Zn(SbS)(CHN)]ClO·0.8HO or [(Zn-cyclam)(SbS)][ClO]·0.8HO. The asymmetric unit consists of two crystallographically independent [SbS] anions, two independent perchlorate anions and two independent water mol-ecules as well as four crystallographically independent Zn(cyclam) 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) cations are linked the [SbS] anions into [Zn(cyclam)SbS] cations that are charged-balanced by the [ClO] anions. The water mol-ecules of crystallization are hydrogen bonded to the [SbS] 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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