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From {Bi 22 O 26 } to Chiral Ligand‐Protected {Bi 38 O 45 }‐Based Bismuth Oxido Clusters
Author(s) -
Mansfeld Dirk,
Miersch Linda,
Rüffer Tobias,
Schaarschmidt Dieter,
Lang Heinrich,
Böhle Tony,
Troff Ralf W.,
Schalley Christoph A.,
Müller Jens,
Mehring Michael
Publication year - 2011
Publication title -
chemistry – a european journal
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.687
H-Index - 242
eISSN - 1521-3765
pISSN - 0947-6539
DOI - 10.1002/chem.201102437
Subject(s) - chemistry , infrared multiphoton dissociation , deprotonation , bismuth , crystallography , mass spectrometry , crystallization , tandem mass spectrometry , dissociation (chemistry) , ligand (biochemistry) , medicinal chemistry , nuclear chemistry , stereochemistry , organic chemistry , ion , chromatography , biochemistry , receptor
The reaction of [Bi 22 O 26 (OSiMe 2 t Bu) 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.