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Design, Synthesis, and Traveling Wave Ion Mobility Mass Spectrometry Characterization of Iron(II)- and Ruthenium(II)-Terpyridine Metallomacrocycles.
MedLine Citation:
PMID:  21718066     Owner:  NLM     Status:  Publisher    
Abstract/OtherAbstract:
New metallomacrocycles composed of 2,2':6',2"-terpyridine (tpy) ligands and Ru<sup>II</sup> or Fe<sup>II</sup> transition metal ions were prepared by stepwise directed assembly and characterized by 2D diffusion NMR spectroscopy (DOSY), electrospray ionization traveling wave ion mobility mass spectrometry (ESI TWIM MS), and molecular modeling. The supramolecular polymers synthesized include a homonuclear all-Ru hexamer as well as heteronuclear hexamer and nonamer with alternating Ru/Ru/Fe metal centers. ESI MS yields several charge states from each supramacromolecule. If ESI is interfaced with TWIM MS, overlapping charge states and the isomeric components of an individual charge state are separated based on their unique drift times through the TWIM region. From experimentally measured drift times, collision cross-sections can be deduced. The collision cross-sections obtained for the synthesized supramacromolecules are in good agreement with those predicted by molecular modeling for macrocyclic structures. Similarly, the hydrodynamic radii of the synthesized complexes derived from 2D DOSY NMR experiments, agree excellently with the radii calculated for macrocyclic architectures, confirming the ESI TWIM MS finding. ESI TWIM MS and/or 2D DOSY NMR spectroscopy provide an alternative approach for the structural analysis of supramolecules that are difficult or impossible to crystallize, such as the large macrocyclic assemblies investigated. ESI TWIM MS will be particularly valuable for the characterization of supramolecular assemblies not available in the quantity or purity required for NMR studies.
Authors:
Yi-Tsu Chan; Xiaopeng Li; Jing Yu; Gustavo A Carri; Charles N Moorefield; George Richard Newkome; Chrys Wesdemiotis
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Publication Detail:
Type:  JOURNAL ARTICLE     Date:  2011-6-30
Journal Detail:
Title:  Journal of the American Chemical Society     Volume:  -     ISSN:  1520-5126     ISO Abbreviation:  -     Publication Date:  2011 Jun 
Date Detail:
Created Date:  2011-7-1     Completed Date:  -     Revised Date:  -    
Medline Journal Info:
Nlm Unique ID:  7503056     Medline TA:  J Am Chem Soc     Country:  -    
Other Details:
Languages:  ENG     Pagination:  -     Citation Subset:  -    
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