Abstract

The asymmetric unit of the title compound, 3(C13H24N3)+[Bi2I9]3−, comprises two cations and one half of a [Bi2I9]3−ion. The C—N bond lengths of the CN3units in both cations range from 1.336 (3) to 1.364 (5) Å, indicating partial double-bond character pointing towards charge delocalization within the NCN planes. All five-membered rings adopt an envelope conformation with the C atoms as the flap. One of the pyrrolidine rings (cation I) is disordered over two alternative envelope conformations. Two sets of positions were found for two of the methylene groups with an occupancy ratio of 0.757 (10):0.243 (10). The second disordered pyrrolidine moiety (cation II) is disordered around a twofold rotation axis and exhibits two half-occupied symmetry equivalent counterparts. The two BiIIIions are coordinated by six iodide ions in a distorted octahedral manner, with the Bi–I bond lengths ranging from 2.9544 (2) to 3.2414 (2) Å. Two [BiI6]3−octahedra are fused together through face-sharing, forming a dinuclear [Bi2I9]3−unit. The bond lengths of bismuth to the terminal iodides [2.9544 (2)–2.9889 (2) Å] are shorter than the bridging ones [3.1450 (2)–3.2414 (2) Å].

Highlights

  • The asymmetric unit of the title compound, 3(C13H24N3)+ [Bi2I9]3À, comprises two cations and one half of a [Bi2I9]3À ion

  • By testing various guanidinium salts with different inorganic complex anions, we found out that guanidinium iodobismuthates(III) are very suitable candidates for this purpose (Knobloch et al, 2016)

  • One of the pyrrolidine rings is disordered over two alternative envelope conformations

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Summary

Structure description

Peralkylated guanidinium ions with complex inorganic anions are considered as organicinorganic hybrid compounds. Their physical behaviour makes them interesting for application in scanning electron microscopy (SEM), where the contrast and the brightness of the obtained pictures depend on the heaviest atom present in the anions. The asymmetric unit comprises two tris(pyrrolidin-1-yl)carbenium ions and one half of a [Bi2I9]3À ion (Fig. 1). One of the pyrrolidine rings (cation I) is disordered over two alternative envelope conformations (details of the disorder are described in Refinement). The second pyrrolidine moiety (cation II) is disordered (Fig. 2). The C—N bond lengths of the CN3 units in both cations range from 1.336 (3) to 1.364 (5) A , indicating partial double-bond character. (C13H24N3)3[Bi2I9] 2227.11 Monoclinic, C2/c 100 14.1643 (7), 16.7047 (8), 24.9505 (12) 91.601 (2) 5901.2 (5) 4 Mo K 10.70 0.18 Â 0.14 Â 0.08

Data collection Diffractometer Absorption correction
No of restraints
Synthesis and crystallization
Bruker Kappa APEXII DUO diffractometer
Special details
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