TY - JOUR
T1 - The synthesis and characterisation of two new iron thioantimonates
T2 - [Fe(en)3]2Sb2S5·0.55H 2O and [Fe(en)3]2Sb4S8
AU - Lees, R. J E
AU - Powell, Anthony V.
AU - Chippindale, Ann M.
PY - 2005/10/27
Y1 - 2005/10/27
N2 - 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.
AB - 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.
KW - Crystal structure
KW - Solvothermal synthesis
KW - Thioantimonate
KW - X-ray diffraction
UR - http://www.scopus.com/inward/record.url?scp=26444484463&partnerID=8YFLogxK
U2 - 10.1016/j.poly.2005.06.017
DO - 10.1016/j.poly.2005.06.017
M3 - Article
VL - 24
SP - 1941
EP - 1948
JO - Polyhedron
JF - Polyhedron
IS - 15
ER -