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Several new alkali metal oxometallates with anions built up from tetrahedral [MO 4 ] units were obtained in reactions aimed at the formation of alkali metal suboxometallates or by thermally decomposing the latter. Rubidium orthoaluminate tetrahydroxide Rb 9 (AlO 4 )(OH) 4  crystallizes with a new structure type (space group P2 1/c , a = 13.116(1), b = 6.9266(5), c = 18.934(2) A , β = 92.05(1)°, V = 1719.0(3) Å 3 , Z = 4, R1 = 0.0352) and contains orthoaluminate anions [AlO 4 ] 5−  and isolated hydroxide anions. Rubidium orthogallate Rb 5 GaO 4  crystallizes with the Na5GaO 4  structure type (space group Pbca, a = 6.9318(5), b = 21.309(2), c = 11.740(1) Å, V = 1734.2(3) Å 3 , Z = 8, R1 = 0.0423) with isolated orthogallate anions [GaO 4 ] 5− . Cesium chromate oxide Cs10(CrO 4 ) 2 O adopts the Cs 10 (GeO 4 ) 2 O structure type (space group P2 1/c , a = 12.903(1), b = 11.4523(8), c = 19.074(3) Å , β = 127.903(8)°,V = 2223.9(4) Å 3 , Z = 4, R1 = 0.0326) with orthochromate(IV) anions [CrO 4 ] 4−  and isolated oxide anions. In all orthometallates the anions [MO 4 ] n−  deviate only slightly from ideal tetrahedral symmetry. Cesium diindate Cs 8 In 2 O 7  crystallizes with the Cs 8 Fe 2 O 7  structure type (space group P2 1/c , a = 7.4307(6), b = 18.6181(14), c = 7.2639(6) Å , β = 119.225(8)°, V = 877.0(1) Å 3 , Z = 2, R1 = 0.0349). A single-crystal structure investigation at r. t. has shown linear diindate units, but the temperature dependence of the libration angles from TLS studies for the bridging oxygen atom suggests a slightly bent and dynamically disordered diindate anion.

zeitschrift für naturforschung b

Crystal Structures of New Alkali Metal-rich Oxometallates: Rubidium Aluminate Tetrahydroxide, Rb 9 (AlO 4 )(OH) 4 , Rubidium Orthogallate, Rb 5 GaO 4 , Cesiumbis-Chromate(IV) Oxide, Cs 10 (CrO 4 ) 2 O, and Cesium Diindate, Cs 8 In 2 O 7