From {Bi22O26} to chiral ligand-protected {Bi38O45}-based bismuth oxido clusters |
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Authors: | Mansfeld Dirk Miersch Linda Rüffer Tobias Schaarschmidt Dieter Lang Heinrich Böhle Tony Troff Ralf W Schalley Christoph A Müller Jens Mehring Michael |
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Affiliation: | 1. Professur für Koordinationschemie, Technische Universit?t Chemnitz, Strasse der Nationen 62, 09111 Chemnitz (Germany), Fax: (+49)‐371‐531‐21219;2. Professur für Anorganische Chemie, Technische Universit?t Chemnitz, Strasse der Nationen 62, 09111 Chemnitz (Germany);3. Institut für Chemie und Biochemie und Center of Supramolecular Interactions (CSI Berlin), Freie Universit?t Berlin, Takustrasse 3, 14195 Berlin (Germany);4. University of Münster, Institute of Inorganic and Analytical Chemistry, Correnstrasse 28/30, 48149 Münster (Germany) |
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Abstract: | The reaction of [Bi(22)O(26)(OSiMe(2)tBu)(14)] (1) in THF with salicylic acid gave [Bi(22)O(24)(HSal)(14)] (2) first, which was converted into [Bi(38)O(45)(HSal)(22)(OH)(2)(DMSO)(16.5)]·DMSO·H(2)O (3·DMSO·H(2)O) after dissolution and crystallization from DMSO. Single-crystal X-ray diffraction analysis and ESI mass spectrometry associated with infrared multi-photon dissociation (IRMPD) tandem MS experiments confirm the formation of the large and quite stable bismuth oxido cluster 3. The reaction of compound 2 with the butoxycarbonyl(BOC)-protected amino acids phenylalanine and valine (BOC-PheOH and BOC-ValOH), respectively, resulted in the formation of chiral [Bi(38)O(45)(BOC-AA)(22)(OH)(2)] (AA=deprotonated amino acid), as shown by a combination of different analytical techniques such as elemental analysis, dynamic light scattering, circular dichroism spectroscopy, and ESI mass spectrometry. |
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Keywords: | amino acids bismuth oxido clusters chirality mass spectrometry salicylic acid |
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