Abstract
The title compounds were synthesized from potassium rich mixtures of Fe2O3, elemental potassium and the hyperoxide KO2 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) K5[FeO4] (Na5[GaO4] 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 [FeO4]5− with nearly ideal tetrahedral geometry and Fe-O distance in the narrow range of 189 to 192 pm. The pentaferrate K17[Fe5O16] (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 [FeO4] tetrahedra. These linear chain pieces [Fe5O16] 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 K14[Fe4O13] with a comparable packing of tetra-nuclear ferrate(III) anions.
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