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Updated: Jun 19, 2026

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
Published on: September 17, 2017
Solid-state NMR and computational studies of tetratolyl urea calix[4]arene inclusion compounds
Chulsoon Moon1, Gunther Brunklaus, Daniel Sebastiani
1Max-Planck Institute for Polymer Research, Ackermannweg 10, 55128, Mainz, Germany.
Abstract:
Solid-state guest dynamics of tetratolyl tetraurea calix[4]arene tetrapentylether dimeric capsules filled with different types of aromatic guests such as benzene-d6, fluorobenzene-d5 and 1,4-difluorobenzene were studied. Upon inclusion, all guest moieties revealed complexation-induced shifts varying from 2.8 ppm to 5.1 ppm. All guest molecules were shown to undergo distinct motions, ranging from mere C6-rotations of benzene-d6 to (ill-defined) 180 degrees phenyl flips of fluorobenzene-d5. In all cases, dynamic heterogeneities were identified based on 2H lineshape deconvolution. In addition, by combination of both a computed nucleus independent chemical shift (NICS) map and explicit 19F and 2H ab initio DFT chemical shift calculations, the preferred orientation of the guest molecules within the host was derived.
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