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in a concentrated acidic medium HX (X = Cl, Br, F and I) the chemical interaction between organic molecules, such as diamine and triamine and bismuth(III) oxide, which contain active lone pairs. In the particular case of ethylenediamine, we previously described the chemical preparation and the crystal structures of NH3(CH2)2NH3](BiI4)2·4H2O and [NH3(CH2)2NH3] BiCl5·2H2O. In these compounds the bismuth atom shows a tendency towards distorted octahedral coordination with some rather long Bi–X bonds, which is attributed to an aspherical distribution of lone-pair electrons at Bi(III). These compounds are interesting groups of crystals because they show a phasetransition ferro-paraelectric related to the motion of organic cations.3 Our investigations were extended to five aliphatic diamines, NH2(CH2)nNH2 (with n = 2 to 6), in order to examine the effect of the flexible cation on the geometry of the bismuthate(III) halogenide polyhedra. The title compound is the first salt obtained during investigations of the quaternary system Bi2O3–NH2(CH2)2NH2–HBr–H2O. In the present work, we describe the chemical preparation and the crystal structure of bis ethylenediammonium bromide hexabromobismuthate(III) monohydrate. The complex crystals were obtained by dissolving in a concentrated HBr (48%) solution a stoichiometric mixture of NH2(CH2)2NH2 and Bi2O3 (molar ratio 4/1). The resulting aqueous solution was then kept at room temperature. After several weeks of evaporation, pseudohexagonal prism-shaped monocrystals of bis ethylenediammonium bromide hexabromobismuthate(III) monohydrate appeared in the solution. Chemical analyses of bismuth atoms and bromide anions were carried out. A thermogravimetric analysis showed that the complex crystallized with one water molecule per formula unit. Experimental conditions used for the singlecrystal data collection are reported in Table 1. The positional parameters for the bismuth atoms were obtained from a threedimensional Patterson map, while the remaining atoms were found from successive difference Fourier maps. After introducing anisotropic thermal factors for the nonhydrogen atoms and isotropic ones for H atoms, the hydrogen atoms were localized and optimized to fixed positions. Their contributions were isotropically introduced into the calculation, but not refined. Corrections were applied for Lorentz and polarization effects and for absorption. The final anisotropic full-matrix least-squares refinement resulted in convergence of the R factor to 0.0392 (Rw = 0.0664) incorporating the weighting scheme x183 ANALYTICAL SCIENCES 2007, VOL. 23

Synthesis and Crystal Structure of [NH3(CH2)2NH3]2BrBiBr6 H2O