Abstract: | Kx(MgxIn1–x)F3 (x = 0.38) is monoclinic, pseudo tetragonal: a = 12.781(2) Å, b = 12.787(2) Å, c = 7.930(1) Å, β = 90,00(1)°, Z = 20. The crystal structure was solved in the space group P21/a (No. 14), subgroup of the tetragonal space group P4/mbm (No. 127), from X‐ray single crystal data using 4302 unique reflections (1770 with Fo/σ(Fo) > 4). The final observed R factor is 0.053. Kx(MgxIn1–x)F3 has the Magnéli‐bronze structural type, which consists in a tridimensional framework of mixed (MgxIn1–x)F6] octahedra linked together by corners. The potassium ions are mainly located in large almost fully occupied 15‐coordinated sites and in practically empty 12‐coordinated cavities. |