Single crystal structure and Mِssbauer studies of a new cation-deficient thiospinel: Cu5.47Fe2.9Sn13.1S32

Starting from pure metals and sulphur in evacuated silica tubes single crystals of Cu5.47(9)Fe2.9(3)Sn13.1(3)S32 have been obtained by quenching from 680°C. It crystallizes in the Fd3m space group with a = 10.3022 (6) إ. The atomic parameters, occupancies, and anisotropic thermal parameters were refined to give a final R-value of 0.0116. The 119Sn Mِssbauer study shows the presence of Sn (IV) in an octahedral environment and 57Fe Mِssbauer indicates the presence of Fe (II) in an octahedral environment, statistically distributed in both low- and high-spin configurations.