[Bi6O4.5(OH)3.5]2(NO3)11: a new anhydrous bismuth basic nitrate. Synthesis and structure determination from twinned crystals |
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Authors: | N. Henry,P. Deniard,O. Mentré |
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Affiliation: | a Laboratoire de Chimie des Solides (UMR 6502), Institut des Matériaux Jean Rouxel, 2 rue de la Houssinière BP 32229, 44322 Nantes cedex 3, France b Laboratoire de Cristallochimie et Physicochimie du Solide (UPRES A 8012) ENSC Lille—UST Lille, BP 108 59652 Villeneuve d'Ascq cedex, France |
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Abstract: | The bismuth basic nitrate [Bi6O4.5(OH)3.5]2(NO3)11 crystallizes in the monoclinic space group P21 with , , , β=107.329(17)° and . Its structure has been determined from , twinned crystal X-ray data (16 781 reflections, 683 parameters, R=0.0703). It is built upon [Bi6Ox(OH)8−x](10−x)+, x=4 and x=5 hexanuclear complexes and nitrate groups. The polycationic entities are linked to the nitrate anions either by hydrogen bonds or through bismuth-oxygen coordination. Even at , the [Bi6O4(OH)4]6+ and [Bi6O5(OH)3]5+ polycations could not be observed as such, the crystal structure refinement only detecting an average [Bi6O4.5(OH)3.5]5.5+ polycation. To prove the presence of both hexanuclear complexes in the structure, we report the existence of a correlation between the bismuth-linked oxygen bond-valence parameters and the presence, or not, of hydroxyl groups. Moreover, the Raman spectrum of the new anhydrous bismuth basic nitrate is compared to those of [Bi6O5(OH)3](NO3)5·3H2O, [Bi6O4(OH)4](NO3)6·4H2O, and two yet uncharacterized bismuth nitrates. |
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Keywords: | Anhydrous bismuth basic nitrate Twinned crystal Structure determination |
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