Topological Characterization of Coordination-Driven Self-assembly Complexes: Applications of Ion Mobility-Mass Spectrometry
Coordination-driven self-assembly (CDSA) is increasingly used to synthesize coordination complexes containing metal-centered electron acceptors and typically nitrogen-containing electron donors. Characterization of the structures obtained from CDSA via crystallographic or spectroscopic means is limited due to difficulties in forming single crystals for X-ray studies and overlapping precursor and product signals in NMR. Here, we employ ion mobility-mass spectrometry (IM-MS), which provides a direct measure of size and shape of the CDSA complexes, to study the intact reaction products of a rhomboid-shaped complex. This approach negates the need for product isolation and crystallization and allows for tracking of the product distribution as a function of time. A potential challenge of IM-MS is that the size/shape of the observed CDSA complexes can vary with internal energy; however, we show that proper tuning of the instrument reduces the effects of collisional activation thereby allowing for retention of ion conformations that reflect solution-phase ion structures.
KeywordsIon mobility-mass spectrometry Coordination-driven self-assembly Supramolecular coordination complex
- 8.Zhou, Z., Yan, X., Cook, T.R., Saha, M.L., Stang, P.J.: Engineering functionalization in a supramolecular polymer: hierarchical self-organization of triply orthogonal non-covalent interactions on a supramolecular coordination complex platform. J. Am. Chem. Soc. 138(3), 806–809 (2016)CrossRefGoogle Scholar
- 14.Chan, Y.T., Li, X., Yu, J., Carri, G.A., Moorefield, C.N., Newkome, G.R., Wesdemiotis, C.: Design, synthesis, and traveling wave ion mobility mass spectrometry characterization of iron(II)- and ruthenium(II)-terpyridine metallomacrocycles. J. Am. Chem. Soc. 133(31), 11967–11976 (2011)CrossRefGoogle Scholar
- 30.Harrison, J. A.; Kelso, C.; Pukala, T. L.; Beck, J. L.: Conditions for analysis of native protein structures using uniform field drift tube ion mobility mass spectrometry and characterization of stable calibrants for TWIM-MS. J. Am. Soc. Mass. Spectrom. 30(2), 256-267(2019)Google Scholar