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Org. Biomol. Chem., 2008, 6, 278 - 286, DOI: 10.1039/b716325h

Monitoring the thermodynamically-controlled formation of diimide-based resin-attached rotaxanes by gel-phase HR MAS 1H NMR spectroscopy

Kathleen M. Mullen, Ken D. Johnstone, Matthew Webb, Nick Bampos, Jeremy K. M. Sanders and Maxwell J. Gunter

The thermodynamically controlled self-assembly of rotaxane and pseudorotaxane systems consisting of (i) a naphthodiimide thread unit terminated at one end with a pyridine ligand, and covalently linked at the other to a gel-phase polystyrene resin support, (ii) a dinaphtho-crown ether shuttle unit, and (iii) a ruthenium carbonyl metalloporphyrin stopper unit, is investigated by high resolution magic angle spinning proton (HR MAS 1H) NMR spectroscopy. The effects of variable concentration of the solution-phase components, the temperature, and added Li+ and Na+ ions are described, and the limitations of the technique are addressed. The dynamic behaviour is compared directly to the solution-phase analogues, where a bulky stopper group is substituted for the polystyrene resin bead.

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