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The crystal structures of the title compounds, which were synthesized at temperatures between 500 and 850 °C via reaction of Al 2 O 3 , M 2 O 3  and M 2 O 5  (M = As, Sb) with the respective elemental alkaline and alkaline earth elements, have been determined by single crystal X-ray diffraction. The two isotypic compounds A I  2 Sb 2 Al 2 O 7 (K 2 Sb 2 Al 2 O 7  structure type, A I =Rb/Cs; trigonal, space group P3̄̅m1, a = 566.04(10)/570.23(8), c = 836.8(2)/888.0(2) pm, Z = 1, R1 = 0.0511/0.0461) contain double layers consisting of vertex-sharing tetrahedra [Al 2 O 7 ], which are connected to ψ- tetrahedra SbO 3  via common vertices. These double layers are stacked in identical orientation (AA sequence), while in the barium compound BaSb 2 Al 2 O 7  (trigonal, space group R32, a = 545.5(7), c = 2377.3(12) pm, Z = 3, R1 = 0.0427) similar layers [Sb 2 Al 2 O 7 ] are stacked in an ABC sequence. In the arsenic(III) aluminate Cs 2 As 2 Al 2 O 7  (orthorhombic, space group Imm2, a = 546.9(3), b = 1003.81(16), c = 888.5(3) pm, Z = 2, R1 = 0.0313) the Al 2 O 7  moieties are similarly connected via [AsO 3 ] units, in this case not only forming layers, but a three-dimensional network. In the three antimonates, the A cations are not coordinated by the lone electron pairs of M(III), which are oriented towards the interior of the sheets, whereas in the arsenate the lone electron pairs play a significant role in the coordination of one of the two crystallographically independent Cs sites

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Aluminat-Pentelate(III) A I  2 M 2 Al 2 O 7  und A II M 2 Al 2 O 7  (A I  = Rb, Cs; A II  = Ba; M = As, Sb) / Aluminate-Pentelates(III) A I  2 M 2 Al 2 O 7  and A II M 2 Al 2 O 7  (A I  = Rb, Cs; A II  = Ba; M = As, Sb)