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Abstract. Rubidium aluminium pyroarsenate, Mr = 374.29, triclinic, Pi, a = 8.233 (5), b = 6.34 (2), c = 6.241 (5) tk, a = 102.6(1), fl = 103.89(7), y= 96.7 (1) °, V = 303.9 A 3, Z = 2, D,, = 3.9 (3) (pycnometry), Dx --4.09 g cm-3, a(Ag K~) = 0.5608A,, #=108.14cm-1, F(000)=344, T= 296 K, R = 0.049, wR = 0.053 for 2193 reflections.The first structural investigation on a pyroarsenate is reported. It is built from A1As20~I units comprising one A106 octahedron and one As207 pyroarsenate group in which two AsO4 tetrahedra point in opposite directions. These units are connected by heteropolyhedral linkages to form a three-dimensional framework having intersecting tunnels where the Rb + ions are located. Although this structure is not isotypic with the phosphate analogues, it is closely related to that of the pyrophosphates of type I represented by KAIP207.

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