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Original Articles

Solvothermal syntheses and characterizations of polysulfido-thioantimonate and thioantimonate templated by Co-phen complex cation

, , , , , & show all
Pages 2334-2346 | Received 11 Sep 2014, Accepted 07 Apr 2015, Published online: 20 May 2015
 

Abstract

Polysulfido-thioantimonate [Co(phen)3][Sb4S5(S4)2] (1), thioantimonates [Co(phen)3]2Sb18S29 (2), and [H3O][Co(phen)3]SbS4·9H2O (3) (phen = 1,10-phenanthroline) were prepared using [Co(phen)3]2+ formed in situ as a structure directing agent in 80 and 50% CH3OH aqueous solution or water solution, respectively. In 1, eight Sb3+ ions are connected by ten μ-S2− and four μ- bridging ligands to form a circular polysulfide thioantimonate anion [Sb8S10(S4)4]4− which contains a sixteen-membered Sb8S8 heteroring. The Sb3+ ions are in trigonal pyramidal SbS3 or trigonal bipyramidal ψ-SbS4 geometries. In 2, sixteen SbS3 and two ψ-SbS4 units are interconnected by sharing S atoms to form a 3-D [Sb18S294−] framework containing an interpenetrating channel system, in which the [Co(phen)3]2+ complexes are enclosed. In 3, by O–H⋯O and O–H⋯S H-bonding, [SbS4]3−,·H2O and H3O+ are interconnected into a anionic layer, which contains a (H2O)6 water cluster. The [Co(phen)3]2+ complexes are located between the layers. The syntheses of 13 show the influences of different solvents on the Co/Sb/S/phen system. The optical band gaps of 13 are 2.02, 2.11, and 2.27 eV, respectively.

Polythioantimonate [Co(phen)3][Sb4S5(S4)2] (1), thioantimonates [Co(phen)3]2Sb18S29 (2), and [H3O][Co(phen)3]SbS4·9H2O (3) were solvothermally prepared using [Co(phen)3]2+ as a structure directing agent in different protic solvents, indicating solvent effects on the solvothermal system of Co/Sb/S/phen.

Disclosure statement

No potential conflict of interest was reported by the authors.

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