Abstract
Reaction of Co(ClO4)2·6H2O with cyclam (cyclam = 1,4,8,11-tetra-aza-cyclo-tetra-deca-ne) and Na3SbS4·9H2O (Schlippesches salt) in a mixture of aceto-nitrile and water leads to the formation of crystals of the title compound with the composition {[Co3(SbS4)2(C10H24N4)3]·2CH3CN·2H2O} n or {[(Co-cyclam)3(SbS4)2]·2(aceto-nitrile)·2H2O} n . The crystal structure of the title compound consists of three crystallographically independent [Co-cyclam]2+ cations, which are located on centers of inversion, one [SbS4]3- anion, one water and one aceto-nitrile mol-ecule that occupy general positions. The aceto-nitrile mol-ecule is disordered over two orientations and was refined using a split model. The CoII cations are coordinated by four N atoms of the cyclam ligand and two trans-S atoms of the tetra-thio-anti-monate anion within slightly distorted octa-hedra. The unique [SbS4]3- anion is coordinated to all three crystallographically independent CoII cations and this unit, with its symmetry-related counterparts, forms rings composed of six Co-cyclam cations and six tetra-thio-anti-monate anions that are further condensed into layers. These layers are perfectly stacked onto each other so that channels are formed in which acetontrile solvate mol-ecules that are hydrogen bonded to the anions are embedded. The water solvate mol-ecules are located between the layers and are connected to the cyclam ligands and the [SbS4]3- anions via inter-molecular N-H⋯O and O-H⋯S hydrogen bonding.
Highlights
Reaction of Co(ClO4)2Á6H2O with cyclam and Na3SbS4Á9H2O (Schlippesches salt) in a mixture of acetonitrile and water leads to the formation of crystals of the title compound with the composition {[Co3(SbS4)2(C10H24N4)3]Á2CH3CNÁ2H2O}n or {[(Co-cyclam)3(SbS4)2]Á2(acetonitrile)Á2H2O}n
The crystal structure of the title compound consists of three crystallographically independent [Co-cyclam]2+ cations, which are located on centers of inversion, one [SbS4]3À anion, one water and one acetonitrile molecule that occupy general positions
The acetonitrile molecule is disordered over two orientations and was refined using a split model
Summary
Inorganic–organic chalcogenidometallates are an important class of compounds and many such compounds have been reported in the literature (Sheldrick & Wachhold, 1988; Bensch et al, 1997; Dehnen & Melullis, 2007; Wang et al, 2016; Zhou, 2016; Zhu & Dai, 2017; Nie et al, 2017). E78, 270–274 research communications many of these compounds are available under solvothermal conditions if Schlippesches salt (Na3SbS4Á9H2O) or NaSbS3 are used as reactants (Anderer et al, 2014, 2016; Danker et al, 2020). In the course of this project we became interested in cyclam (cyclam = 1,4,8,11-tetraazacyclotetradecane), which is a tetradentate ligand This means that in an octahedral coordination of a transition-metal cation, two coordination sites are provided to which thioantimonate(V) anions can coordinate, which, depending on the nature of the anion, can lead to the formation of the desired thioantimonate(V) networks. This led to crystals of the title compound, which were characterized by single-crystal X-ray diffraction
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