The title metallacrown (MC) complexes Ln III [15-MC Fe III N(shi) -5](OAc) 2 CI(C 5 H 5 N) 6 ( Ln1 ), where OAc - is acetate, shi 3- is salicylhydroximate, and Ln = Gd and Dy, were synthesized via a self-assembly reaction in methanol and pyridine. Single crystals were grown using slow evaporation and characterized using X-ray diffraction. Seven-coordinate capped octahedron geometries were observed for the lanthanide ion in both complexes, which is uncommon for trivalent lanthanide species. The 15-MC-5 is a ruffled metallacrown archetype similar to previously reported mixed-valent manganese metallacrowns.