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[Fe(C 6 H 14 N 2 ) 2 ][Sb 6 S 10 ] – Using a Transition Metal Complex Acting as a Pillar for the Generation of a Three‐dimensional Thioantimonate(III) Network
Author(s) -
Kiebach Ragnar,
Warratz Ralph,
Näther Christian,
Bensch Wolfgang
Publication year - 2009
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.200801390
Subject(s) - crystallography , raman spectroscopy , trigonal crystal system , transition metal , bond length , metal , band gap , materials science , mössbauer spectroscopy , chemistry , crystal structure , stereochemistry , physics , optics , metallurgy , biochemistry , optoelectronics , catalysis
Abstract The new three‐dimensional thioantimonate [Fe(C 6 H 14 N 2 ) 2 ][Sb 6 S 10 ] was obtained under solvothermal conditions. The compound crystallizes in space group P $\bar{1}$ with a = 6.174(4), b = 9.679(2), c = 12.772(3) Å, α = 72.08(3), β = 88.15(3), γ = 89.51(3)°, Z = 2. Trigonal pyramidal [SbS 3 ] units and [SbS 4 ] groups are joined to form a two‐dimensional [Sb 6 S 10 ] 2– layer. The in‐situ formed [Fe(C 6 H 14 N 2 ) 2 ] 2+ complexes act like pillars joining the layers into a three‐dimensional framework through Fe–S bonds. The Fe–S bond lengths are long which may be caused by a pronounced Jahn–Teller distortion. The optical bandgap of 2.0 eV is in agreement with the brownish color of the compound. The Mössbauer spectrum shows a doublet with an isomer shift typical for Fe 2+ in the high spin state. In the Raman spectrum the Sb–S stretching modes of the [SbS 3 ] and [SbS 4 ] groups can be distinguished. Upon heating in nitogen the compound is decomposed in one step yielding Sb 2 S 3 and FeSb 2 S 4 .