Abstract
A new layered germanium–antimony sulphide, [Ge(C 2N 2H 8) 3][GeSb 2S 6], has been prepared at 463 K under solvothermal conditions in the presence of ethylenediamine. The compound has been characterised by single-crystal X-ray diffraction, thermogravimetry, elemental analysis and reflectance spectroscopy. [Ge(C 2N 2H 8) 3][GeSb 2S 6] crystallises in the space group Pbca ( a=13.3284(5), b=17.4801(6), c=18.5447(7) Å). The structure consists of cyclic [GeSb 2S 8] 6− units that form chains which are cross-linked through Sb 2S 2 rings to generate layers of stoichiometry [GeSb 2S 6] 2−, between which [Ge(en) 3] 2+ cations are located. [Ge(C 2N 2H 8) 3][GeSb 2S 6] contains germanium in both the divalent and tetravalent states. The optical band gap of 2.49(4) eV is in excellent agreement with the value expected on the basis of the correlation with the density of metal centres previously identified for thioantimonates, and is consistent with states at the top of the valence band being predominantly of sulphur 3 p character.
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