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Synthesis and crystal structure of poly[[di-μ 3 -tetra-thio-anti-monato-tris-[(cyclam)cobalt(II)]] aceto-nitrile disolvate dihydrate] (cyclam = 1,4,8,11-tetra-aza-cyclo-tetra-deca-ne).

Christian NätherFelix DankerWolfgang Bensch
Published in: Acta crystallographica. Section E, Crystallographic communications (2022)
Reaction of Co(ClO 4 ) 2 ·6H 2 O with cyclam (cyclam = 1,4,8,11-tetra-aza-cyclo-tetra-deca-ne) and Na 3 SbS 4 ·9H 2 O (Schlippesches salt) in a mixture of aceto-nitrile and water leads to the formation of crystals of the title compound with the composition {[Co 3 (SbS 4 ) 2 (C 10 H 24 N 4 ) 3 ]·2CH 3 CN·2H 2 O} n or {[(Co-cyclam) 3 (SbS 4 ) 2 ]·2(aceto-nitrile)·2H 2 O} 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 [SbS 4 ] 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 Co II 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 [SbS 4 ] 3- anion is coordinated to all three crystallographically independent Co II 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 [SbS 4 ] 3- anions via inter-molecular N-H⋯O and O-H⋯S hydrogen bonding.
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