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The two new oxoferrates(III) Cs 6 [Fe 2 O 6 ] and Rb 4 [Fe 2 O 5 ] were synthesized at temperatures of 500 and 600 °C via reaction of Fe 2 O 3  with the elemental alkali metals (A) and their hyperoxides AO 2  in the form of dark-red crystals. Their crystal structures have both been determined by single crystal X-ray diffraction. The structure of Cs 6 [Fe 2 O 6 ] (monoclinic,  P 2 1 / c ,  a  = 724.6(2),  b  = 1212.1(5),  c  = 767.6(3) pm,  β  = 105.03(4)°,  Z  = 2,  R 1 = 0.0272, K 6 [Mn 2 O 6 ] structure type) contains isolated bi nuclear anions [O 2 FeO 2 FeO 2 ] 6-  composed of two edge sharing FeO 4  tetrahedra, which are also known from the potassium and rubidium compounds A 6 [Fe 2 O 6 ] that crystallize in the  klassengleiche  super group  C 2/ m . Comparable building blocks are connected via common O vertices to form chains  1  ∞ [O 1/2 OFeO 2 FeOO 1/2 ] 4–  in the rubidium ferrate(III) Rb 4 [Fe 2 O 5 ] (monoclinic,  C 2/ c ,  a  = 711.43(14),  b  = 1750.0(5),  c  = 725.3(2) pm,  β  = 104.72(2)°,  Z  = 4,  R 1 = 0.0611). As a consequence of the edge sharing of FeO 4  tetrahedra, both compounds show short Fe—Fe distances of 273.3(2) pm in Cs 6 [Fe 2 O 6 ] and 265.6(3) pm in Rb 4 [Fe 2 O 5 ] respectively. Based on similarities in the packing of the (Fe III /A I ) cations, a structural relationship between the two compounds can be derived. The influence of the different counterions on the structure of the oxoferrate units in the phases of general composition A 6 [Fe 2 O 6 ] and A 4 [Fe 2 O 5 ] is discussed.

Cs 6 [Fe 2 O 6 ] and Rb 4 [Fe 2 O 5 ]: New oxoferrates(III) with edge sharing FeO 4 tetrahedra