A direct route to closo-SBCl thiaboranes from simple electron-precise synthons: the different role of chalcogen bonding in SB5Cl5 and SB11Cl11 crystals
Six-vertex closo-SB5Cl5 (1) and ten-vertex closo-1-SB9Cl9 (2) thiaboranes have been prepared, besides the already known 12-vertex closo-SB11Cl11 (3), from the co-pyrolysis reaction of B2Cl4 with S2Cl2 at 280 °C in vacuo. The compounds are sublimable, off-white solids. Their elemental composition has...
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| Hauptverfasser: | , , , , , |
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| Dokumenttyp: | Article (Journal) |
| Sprache: | Englisch |
| Veröffentlicht: |
November 11, 2024
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| In: |
Angewandte Chemie. International edition
Year: 2024, Jahrgang: 63, Heft: 46, Pages: 1-9 |
| ISSN: | 1521-3773 |
| DOI: | 10.1002/anie.202406751 |
| Online-Zugang: | Verlag, lizenzpflichtig, Volltext: https://doi.org/10.1002/anie.202406751 Verlag, lizenzpflichtig, Volltext: https://onlinelibrary.wiley.com/doi/abs/10.1002/anie.202406751 
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| Verfasserangaben: | Willi Keller, Falk Lissner, Joachim Ballmann, Jindřich Fanfrlík, Drahomír Hnyk, and Thomas Schleid |
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| 245 | 1 | 2 | |a A direct route to closo-SBCl thiaboranes from simple electron-precise synthons |b the different role of chalcogen bonding in SB5Cl5 and SB11Cl11 crystals |c Willi Keller, Falk Lissner, Joachim Ballmann, Jindřich Fanfrlík, Drahomír Hnyk, and Thomas Schleid |
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| 520 | |a Six-vertex closo-SB5Cl5 (1) and ten-vertex closo-1-SB9Cl9 (2) thiaboranes have been prepared, besides the already known 12-vertex closo-SB11Cl11 (3), from the co-pyrolysis reaction of B2Cl4 with S2Cl2 at 280 °C in vacuo. The compounds are sublimable, off-white solids. Their elemental composition has been determined by high-resolution mass spectrometry. They were further characterized by one- and two-dimensional 11B NMR spectroscopy and X-ray structure determination for 1 and 3. Ab initio/GIAO/NMR computations support octahedral, bicapped square-antiprismatic, and icosahedral geometries for 1, 2 and 3, respectively, as expected based on their closo-electron counts. 1 is the first isolated example of a neutral polyhedral closo-thiaborane with a cluster size smaller than ten vertices. The solid-state structure of 3 is one of the rare examples of a single-crystal X-ray structure determination of an icosahedral heteroborane reported. The corresponding crystal-packing forces show the different role of chalcogen bonding in these octahedral and icosahedral crystals. In addition, there is a mass-spectrometry evidence for the recurrent formation of further thiaborane homologs of closo-SBnCln with n=4, 6, 10, and supra-icosahedral 12. | ||
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