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The title compounds were synthesized from potassium rich mixtures of Fe 2 O 3 , elemental potassium and the hyperoxide KO 2  by applying short reaction times, a maximum temperature of 875 K and subsequent quenching of the samples. The structures of the two new oxoferrates(III) have been determined by single crystal X-ray diffraction. The orthoferrate(III) K 5 [FeO 4 ] (Na 5 [GaO 4 ] structure type, space group Pbca, a = 1124,0(2), b = 667,95(9), c = 2034,8(3) pm, Z = 4, R1 = 0,0585) exhibits isolated ortho-anions [FeO 4 ] 5−  with nearly ideal tetrahedral geometry and Fe-O distance in the narrow range of 189 to 192 pm. The pentaferrate K 17 [Fe 5 O 16 ] (space group Cm, a = 671,71(5), b=3560,8(3), c=670,81(5) pm, β =119,687(5)°, Z =2, R1=0,0291) crystallizes with a new structure type. Its building units are isolated novel penta-nuclear anions composed of five corner sharing [FeO 4 ] tetrahedra. These linear chain pieces [Fe 5 O 16 ] are arranged in a hexagonal rod packing, with a stacking sequence according to |:AB:| along the large monoclinic b axis. The structure is thus related to that of the tetra-ferrate K 14 [Fe 4 O 13 ] with a comparable packing of tetra-nuclear ferrate(III) anions.

K 5 [FeO 4 ] und K 17 [Fe 5 O 16 ]: Zwei neue Kalium-Oxoferrate(III) / K 5 [FeO 4 ] and K 17 [Fe 5 O 16 ]: Two New Potassium Oxoferrates(III)