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From {Bi22O26} to chiral ligand-protected {Bi38O45}-based bismuth oxido clusters.

Chemistry (Weinheim an der Bergstrasse, Germany) (2011-11-29)
Dirk Mansfeld, Linda Miersch, Tobias Rüffer, Dieter Schaarschmidt, Heinrich Lang, Tony Böhle, Ralf W Troff, Christoph A Schalley, Jens Müller, Michael Mehring
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.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Bismuth(III) oxide, ReagentPlus®, powder, 10 μm, 99.9% trace metals basis
Sigma-Aldrich
Bismuth(III) oxide, powder, 99.999% trace metals basis
Sigma-Aldrich
Bismuth(III) oxide, nanopowder, 90-210 nm particle size, 99.8% trace metals basis
Sigma-Aldrich
Bismuth(III) oxide, purum, ≥98.0% (KT)