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Kinetic Analysis as a Tool to Distinguish Pathway Complexity in Molecular Assembly: An Unexpected Outcome of Structures in Competition Article Options
Daan van der Zwaag†‡, Pascal A. Pieters†, Peter A. Korevaar†‡, Albert J. Markvoort†§, A. J. H. Spiering‡, Tom F. A. de Greef*†§, and E. W. Meijer*†‡ † Institute for Complex Molecular Systems, ‡ Laboratory of Macromolecular and Organic Chemistry, and § Computational Biology Group, Eindhoven University of Technology, P.O. Box 513, 5600 MB Eindhoven, The Netherlands
Cite this: J. Am. Chem. Soc. 137, 39, 12677-12688
J. Am. Chem. Soc., 2015, 137 (39), pp 12677–12688 DOI: 10.1021/jacs.5b08138 Publication Date (Web): September 10, 2015 Copyright © 2015 American Chemical Society *
[email protected], *
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While the sensitive dependence of the functional characteristics of self-assembled nanofibers on van der Zwaag, Daan
the molecular structure of their building blocks is well-known, the crucial influence of the
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dynamics of the assembly process is often overlooked. For natural protein-based fibrils, various aggregation mechanisms have been demonstrated, from simple primary nucleation to
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secondary nucleation and off-pathway aggregation. Similar pathway complexity has recently been described in synthetic supramolecular polymers and has been shown to be intimately linked to their morphology. We outline a general method to investigate the consequences of the
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presence of multiple assembly pathways, and show how kinetic analysis can be used to distinguish different assembly mechanisms. We illustrate our combined experimental and
Received 3 August 2015 Published online 10 September 2015 Published in print 7 October 2015
theoretical approach by studying the aggregation of chiral bipyridine-extended 1,3,5benzenetricarboxamides (BiPy-1) in n-butanol as a model system. Our workflow consists of nonlinear least-squares analysis of steady-state spectroscopic measurements, which cannot
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provide conclusive mechanistic information but yields the equilibrium constants of the selfassembly process as constraints for subsequent kinetic analysis. Furthermore, kinetic
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nucleation-elongation models based on one and two competing pathways are used to interpret time-dependent spectroscopic measurements acquired using stop-flow and temperature-jump
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methods. Thus, we reveal that the sharp transition observed in the aggregation process of BiPy1 cannot be explained by a single cooperative pathway, but can be described by a competitive two-pathway mechanism. This work provides a general tool for analyzing supramolecular polymerizations and establishing energetic landscapes, leading to mechanistic insights that at first sight may seem unexpected and counterintuitive.
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