Separation and characterization of metallosupramolecular libraries by ion mobility mass spectrometry.
Identifieur interne : 002435 ( Main/Exploration ); précédent : 002434; suivant : 002436Separation and characterization of metallosupramolecular libraries by ion mobility mass spectrometry.
Auteurs : Xiaopeng Li [États-Unis] ; Yi-Tsu Chan ; Madalis Casiano-Maldonado ; Jing Yu ; Gustavo A. Carri ; George R. Newkome ; Chrys WesdemiotisSource :
- Analytical chemistry [ 1520-6882 ] ; 2011.
Abstract
The self-assembly of Zn(II) ions and bis(terpyridine) (tpy) ligands carrying 120° or 180° angles between their metal binding sites was utilized to prepare metallosupramolecular libraries with the connectivity. These combinatorial libraries were separated and characterized by ion mobility mass spectrometry (IM MS) and tandem mass spectrometry (MS(2)). The 180°-angle building blocks generate exclusively linear complexes, which were used as standards to determine the architectures of the assemblies resulting from the 120°-angle ligands. The latter ligand geometry promotes the formation of macrocyclic hexamers, but other n-mers with smaller (n = 5) or larger ring sizes (n = 7-9) were identified as minor products, indicating that the angles in the bis(terpyridine) ligand and within the coordinative tpy-Zn(II)-tpy bonds are not as rigid, as previously believed. Macrocyclic and linear isomers were detected in penta- and heptameric assemblies; in the larger octa- and nonameric assemblies, ring-opened conformers with compact and folded geometries were observed in addition to linear extended and cyclic architectures. IM MS(2) experiments provided strong evidence that the macrocycles present in the libraries were already formed in solution, during the self-assembly process, not by dissociation of larger complexes in the gas phase. The IM MS/MS(2) methods provide a means to analyze, based on size and shape (architecture), supramolecular libraries that are not amenable to liquid chromatography, LC-MS, NMR, and/or X-ray techniques.
DOI: 10.1021/ac201161u
PubMed: 21744807
Affiliations:
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Carri</name></author><author><name sortKey="Newkome, George R" sort="Newkome, George R" uniqKey="Newkome G" first="George R" last="Newkome">George R. Newkome</name></author><author><name sortKey="Wesdemiotis, Chrys" sort="Wesdemiotis, Chrys" uniqKey="Wesdemiotis C" first="Chrys" last="Wesdemiotis">Chrys Wesdemiotis</name></author></analytic><series><title level="j">Analytical chemistry</title><idno type="eISSN">1520-6882</idno><imprint><date when="2011" type="published">2011</date></imprint></series></biblStruct></sourceDesc></fileDesc><profileDesc><textClass></textClass></profileDesc></teiHeader><front><div type="abstract" xml:lang="en">The self-assembly of Zn(II) ions and bis(terpyridine) (tpy) ligands carrying 120° or 180° angles between their metal binding sites was utilized to prepare metallosupramolecular libraries with the connectivity. These combinatorial libraries were separated and characterized by ion mobility mass spectrometry (IM MS) and tandem mass spectrometry (MS(2)). The 180°-angle building blocks generate exclusively linear complexes, which were used as standards to determine the architectures of the assemblies resulting from the 120°-angle ligands. The latter ligand geometry promotes the formation of macrocyclic hexamers, but other n-mers with smaller (n = 5) or larger ring sizes (n = 7-9) were identified as minor products, indicating that the angles in the bis(terpyridine) ligand and within the coordinative tpy-Zn(II)-tpy bonds are not as rigid, as previously believed. Macrocyclic and linear isomers were detected in penta- and heptameric assemblies; in the larger octa- and nonameric assemblies, ring-opened conformers with compact and folded geometries were observed in addition to linear extended and cyclic architectures. IM MS(2) experiments provided strong evidence that the macrocycles present in the libraries were already formed in solution, during the self-assembly process, not by dissociation of larger complexes in the gas phase. The IM MS/MS(2) methods provide a means to analyze, based on size and shape (architecture), supramolecular libraries that are not amenable to liquid chromatography, LC-MS, NMR, and/or X-ray techniques.</div> </front></TEI><affiliations><list><country><li>États-Unis</li></country></list><tree><noCountry><name sortKey="Carri, Gustavo A" sort="Carri, Gustavo A" uniqKey="Carri G" first="Gustavo A" last="Carri">Gustavo A. Carri</name><name sortKey="Casiano Maldonado, Madalis" sort="Casiano Maldonado, Madalis" uniqKey="Casiano Maldonado M" first="Madalis" last="Casiano-Maldonado">Madalis Casiano-Maldonado</name><name sortKey="Chan, Yi Tsu" sort="Chan, Yi Tsu" uniqKey="Chan Y" first="Yi-Tsu" last="Chan">Yi-Tsu Chan</name><name sortKey="Newkome, George R" sort="Newkome, George R" uniqKey="Newkome G" first="George R" last="Newkome">George R. Newkome</name><name sortKey="Wesdemiotis, Chrys" sort="Wesdemiotis, Chrys" uniqKey="Wesdemiotis C" first="Chrys" last="Wesdemiotis">Chrys Wesdemiotis</name><name sortKey="Yu, Jing" sort="Yu, Jing" uniqKey="Yu J" first="Jing" last="Yu">Jing Yu</name></noCountry><country name="États-Unis"><noRegion><name sortKey="Li, Xiaopeng" sort="Li, Xiaopeng" uniqKey="Li X" first="Xiaopeng" last="Li">Xiaopeng Li</name></noRegion></country></tree></affiliations></record>Pour manipuler ce document sous Unix (Dilib)
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