Issue 34, 2015

Solid-state NMR as a probe of anion binding: molecular dynamics and associations in a [5]polynorbornane bisurea host complexed with terephthalate

Abstract

A range of solid-state NMR techniques is used to characterise a molecular host:guest complex consisting of a [5]polynorbornane bisurea host binding a terephthalate dianion guest. Detailed information is obtained on the molecular dynamics and associations from the point of view of both the host and guest molecules. The formation of the complex in the solid state is confirmed using 1H 2D exchange NMR, and the 180° flipping of the 2H-labelled terephthalate guest and its eventual expulsion from the complex at elevated temperatures are quantified using variable-temperature 2H spin-echo experiments. Two-dimensional 1H–13C HETCOR spectra obtained under fast magic angle spinning conditions (60 kHz) show a high resolution despite the poor crystallinity of the solid complex, and clearly reveal changes in the rigidity of the host molecule when complexed. Short-range intra- and intermolecular 1H–1H proximities are also detected using 2D SQ–DQ correlation methods, providing insight into the molecular packing in the solid phase.

Graphical abstract: Solid-state NMR as a probe of anion binding: molecular dynamics and associations in a [5]polynorbornane bisurea host complexed with terephthalate

Supplementary files

Article information

Article type
Paper
Submitted
23 Jun 2015
Accepted
28 Jul 2015
First published
28 Jul 2015

Phys. Chem. Chem. Phys., 2015,17, 22195-22203

Author version available

Solid-state NMR as a probe of anion binding: molecular dynamics and associations in a [5]polynorbornane bisurea host complexed with terephthalate

A. Rawal, J. M. Hook, R. N. Robson, D. Gunzelmann, F. M. Pfeffer and L. A. O'Dell, Phys. Chem. Chem. Phys., 2015, 17, 22195 DOI: 10.1039/C5CP03628C

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