The synthesis and characterisation of two new iron thioantimonates: [Fe(en)3]2Sb2S5·0.55H 2O and [Fe(en)3]2Sb4S8

R. J E Lees, Anthony V. Powell, Ann M. Chippindale

Research output: Contribution to journalArticle

36 Citations (Scopus)

Abstract

Two new iron thioantimonates, [Fe(en)3]2Sb 2S5·0.55H2O (1) and [Fe(en) 3]2Sb4S8 (2), were synthesised under solvothermal conditions from the reactions of Sb2S3, FeCl2 and S in the presence of ethylenediamine at 413 and 438 K, respectively. The products were characterised by single-crystal X-ray diffraction, elemental analysis and SQUID magnetometry. Compound 1 is unusual in containing isolated Sb2S54- anions formed from two corner-sharing SbS33- trigonal pyramids. These units are arranged in rippled layers, 4 Å apart, parallel to the bc-plane. Octahedrally coordinated [Fe(en)3]2+ cations lie in depressions within these anionic layers. In compound (2), repeated corner linking of SbS33- trigonal pyramids generates SbS 2- chains, which may be considered as a polymerised form of the Sb2S54- anions in 1. The SbS 2- chains are separated by [Fe(en)3] 2+ cations. In both compounds, there is an extensive network of hydrogen bonds between the nitrogen atoms of the ethylenediamine ligands and the sulfur atoms of the anions and, in the case of 1, the uncoordinated water molecule. © 2005 Elsevier Ltd. All rights reserved.

Original languageEnglish
Pages (from-to)1941-1948
Number of pages8
JournalPolyhedron
Volume24
Issue number15
DOIs
Publication statusPublished - 27 Oct 2005

Keywords

  • Crystal structure
  • Solvothermal synthesis
  • Thioantimonate
  • X-ray diffraction

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