Abstract
Starting from pure metals and sulfur in evacuated silica tubes, single crystals of Cu5.52(8)Si1.04(8)□1.44Fe4Sn12S32 have been obtained by quenching from 680°C. The above cation-deficient thiospinel crystallizes in the Fd3m space group with a=10.3322(6) Å. Si doping leads to additional vacancies in the copper site. 119Sn Mössbauer data show the presence of Sn in II as well as IV oxidation states and all the Sn is present in the octahedral 16d sites. 57Fe Mössbauer studies show Fe to be present in the octahedral sites in both II and III oxidation states. The above thiospinel shows semiconducting behavior with resistivity of ∼1×102 Ω-cm at room temperature and a small band gap of ∼0.1 eV.
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