The halogenobismuthates Q3Bi2X9 (Q = EtMe2PhN; X = Cl, Br, I) were prepared by reaction of BiX3 with EtMe2PhNX in ethanol. Single crystal structure determinations yielded: [EtMe2PhN]3[Bi2Cl9], S.G. P212121, Nr. 19, a = 952.5(3), b = 1184.1(4), c = 3726.4(9 pm, Z = 2;[EtMe2PhN]3[Bi2Br9] S.G .P21/c , No. 14, a= 1839.4(4),b= 1329.5(3), c = 1817.3(6)pm, β = 92.68(3)°, Z = 4, [EtMe2PhN]3[Bi2l9], ], S.G . P21/c, No. 14, a = 1915.3(2), b = 1379.0(3), c = 1890.9(5) pm, β = 92.48(1)°, Z = 4. The thermal behaviour was investigated with the aid of DSC measurements and temperature dependent X-ray powder diffraction. All compounds undergo a transition into a high temperature modification which could be obtained in case of [EtMe2PhN]3[Bi2Br9-xIx] in form of single crystals: S.G . P21/c, Nr. 14, a = 1002.7(5), b = 1278.7 (8), c = 3584.3(5) pm, β = 90.12(2)°, Z = 4. Surprisingly in this compound the iodine atoms are not statistically distributed over all possible bromine positions, but occupy only one position. Lattice parameters of the other high temperature modifications and enthalpies of transition of the compounds are given. In addition a second iodobismuthate was isolated:[EtMe2PhN]4[Bi6l22], S.G . P1̄, Nr. 2 , with lattice parameters of a = 1343.4(3), b = 1554.3(3), c = 2262.5(6) pm, a = 100.89(3)°, β = 96.63(1)°, 7 = 98.94(2)° and Z = 2.

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Crystal Structure, 1,1 '-Dimethyl-4,4'-bipyridinium-octachlorodiantimonate(III)The title compound was prepared by reaction of SbCl3 with 1,1'-dimethyl-4,4'-bipyridiniumchloride in methanol. The single crystal structure gave the following data: [Cl2Hi4N2] [Sb2Cl8] (1) space group PI, Nr. 1, with a = 570.68(7) pm, b = 938.57(14) pm, c = 1174.27(11)"pm, q = 66.72(9)°, ß = 89.304(12)°, 7 = 78.684(11)°, and Z = 1. The compound has a small SHG effect and a phase transition at 272 °C with an enthalpy of transition of 6.54 kJ mol-1 .

At room temperature, tris(ethyldimethylphenylammonium)tri-

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