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Single‐crystal potassium tetrafluoaluminate‐doped substitutionally with iron has been prepared. The room‐temperature spectrum of isolated iron ions may be described by a conventional spin Hamiltonian with parameters: g‖=2.005, g⊥=1.999, D=0.1471 cm-1, a=0.0020 cm-1, and F=0.007 cm-1. From the linewidths an upper limit to the fluorine hyperfine structure is estimated.