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The new alkaline metal arsenates(III) were synthesized at a temperature of 500 °C via reaction of stoichiometric mixtures of the elemental alkali metals A and As 2 O 3 . In the crystal structures of the four title compounds, which have been determined by single crystal x-ray diffraction, the As(III) atoms are in ψ-tetrahedral coordination by oxygen exclusively. In NaAsO 2  (orthorhombic, space group Pbcm, a = 1429.6(9), b = 677.3(3), c = 509.1(2) pm, Z = 8) and the compounds AAsO 2  (A = K/Rb, orthorhombic, space group Pbcm, a = 715.1(2)/729.7(5), b =748.0(1)/775.2(5), c = 539.20(17)/541.1(3) pm, Z = 4) the AsO 3  ψ-tetrahedra are condensed to form zig-zag chains [AsOO 2/2 ] − . In the Cs phase Cs3As5O9 with a lower alkaline metal content (trigonal, space group P31m, a = 845.5(3), c = 602.6(2) pm, Z = 1) the two crystallographically independent ψ-tetrahedra AsO 3/2  and AsOO 2/2  are connected in a 2:3 ratio to give polar sheets [As 5 O 9 ] 3− .

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Die neuen Oxoarsenate(III) AAsO 2  (A = Na, K, Rb) und Cs 3 As 5 O 9 . Darstellung, Kristallstrukturen und Raman-Spektren /  The New Oxoarsenates(III) AAsO2 (A = Na, K, Rb) and Cs3As5O9. Synthesis, Crystal Structures and Raman Spectra