Abstract
Starting from pure metals and sulphur in evacuated silica tubes single crystals of Cu 7.38(11)Mn 4Sn 12S 32 and Cu 7.07(6)Ni 4Sn 12S 32 have been obtained by quenching from 680 °C. These crystallize in the Fd3̄ m space group and have a=10.4145 (7) and 10.305 (1) Å, respectively. The atomic parameters, occupancies and anisotropic thermal parameters were refined to give a final R-value of 0.0209 and 0.0181 for Cu 7.38Mn 4Sn 12S 32 and Cu 7.07Ni 4Sn 12S 32, respectively. A significant amount of cation deficiency exists at 8a site of the quaternary spinel structure.
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