Little Live Pets 28847 Cozy DOZYS, Multi-Colour

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L. Sellies, I. Reile, R. Aspers, M. C. Feiters, F. Rutjes and M. Tessari, Chem. Commun., 2019, 55, 7235 RSC .

P. Lameiras and J. M. Nuzillard, Prog. Nucl. Magn. Reson. Spectrosc., 2021, 123, 1 CrossRef CAS PubMed . To investigate its structure further in solution, SAXS was used for 11 and the [4]-rotaxane 12 ( Fig. 7B), which had already been fully characterised with X-ray crystallography. A pair distance distribution function (PDDF) was obtained from each SAXS data set ( Fig. 7C). Such X-ray scattering data provides a probability for the distance between electrons in the investigated molecule. 69 E. Martineau, J. N. Dumez and P. Giraudeau, Magn. Reson. Chem., 2020, 58, 390 CrossRef CAS PubMed . L. Castanar, R. Roldan, P. Clapes, A. Virgili and T. Parella, Chemistry, 2015, 21, 7682 CrossRef CAS PubMed . V. Daniele, F.-X. Legrand, P. Berthault, J.-N. Dumez and G. Huber, Chem. Phys. Chem., 2015, 16, 3413 CrossRef CAS PubMed .

DOSY

D. Dai, X. Wang, Y. Liu, X. L. Yang, C. Glaubitz, V. Denysenkov, X. He, T. Prisner and J. Mao, Nat. Commun., 2021, 12, 6880 CrossRef CAS PubMed . N. Eshuis, R. L. E. G. Aspers, B. J. A. van Weerdenburg, M. C. Feiters, F. P. J. T. Rutjes, S. S. Wijmenga and M. Tessari, Angew. Chem., Int. Ed., 2015, 54, 14527 CrossRef CAS PubMed . Y. Cohen, L. Avram, T. Evan-Salem, S. Slovak, N. Shemesh and L. Frish, Analytical Methods in Supramolecular Chemistry, Wiley, 2nd edn, 2012, pp. 197–285 Search PubMed. A. Herrera, E. Fernandez-Valle, R. Martinez-Alvarez, D. Molero, Z. D. Pardo, E. Saez and M. Gal, Angew. Chem., Int. Ed., 2009, 48, 6274 CrossRef CAS PubMed .

D. Li, I. Keresztes, R. Hopson and P. G. Williard, Acc. Chem. Res., 2009, 42, 270 CrossRef CAS PubMed . The potential of UF 2D NMR for mixture analysis was recognised early on, with the use of UF implementations of 2D correlation experiments such as TOCSY. 143,144 Examples were reported of reaction monitoring, including the detection of a short-lived intermediates, 145 and of the in-line acquisition of 2D spectra for a liquid chromatography type setup. 143 A series of examples of reaction monitoring applications were then described by Herrera and co-workers who, for example, obtained mechanistic insights into the synthesis of pyrimidines. 144,146–149 They notably made use of a rapid-injection device, to capture intermediate species with a half-life of a few minutes. Small-angle neutron and X-ray scattering Techniques Small-angle scattering techniques are powerful methods to investigate structures of supramolecular assemblies in solution or of soft matter, e.g. gels. Neutron (SANS) and X-ray scattering (SAXS) often require that samples are transported to specialist beam lines, although for example SAXS is increasingly available also as a lab-based technique. C. Kjeldsen, J. H. Ardenkjaer-Larsen and J. O. Duus, J. Am. Chem. Soc., 2018, 140, 3030 CrossRef CAS PubMed . Left) array of 1H PFGSTE spectra measured with linearly increasing field gradient, for a mixture containing TSP, choline and acetone in D 2O, and (right) the resultant DOSY spectrum, showing TSP signals in blue, choline in green and acetone in red.

Diffusion-Ordered NMR Spectroscopy

When comparing the 1H-NMR spectra of resorcin[4]arene 1 with and without glutaric acid 2, different guest signals of 2 are found upfield-shifted. Additionally, integration yielded a host–guest stoichiometry of around 1 : 1, indicating six enclosed guest molecules. The extend of the encapsulation process was shown to increase with higher concentrations of glutaric acid and longer reaction times, which was readily observable due to the high sensitivity of the host aryl peak at 6.1 ppm. This supported the proposed encapsulation mechanism and additionally indicated a slowly occurring exchange mechanism at the expense of solvent molecules, in this case chloroform. L. Rouger, B. Gouilleux, M. Pourchet-Gellez, J. N. Dumez and P. Giraudeau, Analyst, 2016, 141, 1686 RSC . R. Pievo, C. Casati, P. Franchi, E. Mezzina, M. Bennati and M. Lucarini, ChemPhysChem, 2012, 13, 2659–2661 CrossRef CAS PubMed. Fig. 6 (A) Structure of the non-fluorinated gel 9 and SANS curves without further treatment (blue dots) and after thin-film shearing (green dots). (B) Structure of the fluorinated gel 10 and SANS curves without further treatment (green dots) and after thin-film shearing (cyan dots). Reproduced from ref. 66 with permission from the Royal Society of Chemistry.

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C. Tedesco, Comprehensive Supramolecular Chemistry II, Elsevier, 2nd edn, 2017, vol. 2, pp. 45–73 Search PubMed. A. P. Deshmukh, D. Koppel, C. Chuang, D. M. Cadena, J. Cao and J. R. Caram, J. Phys. Chem. C, 2019, 123, 18702–18710 CrossRef CAS. M. H. Lerche, D. Yigit, A. B. Frahm, J. H. Ardenkjaer-Larsen, R. M. Malinowski and P. R. Jensen, Anal. Chem., 2018, 90, 674 CrossRef CAS PubMed .

T. Evan-Salem, I. Baruch, L. Avram, Y. Cohen, L. C. Palmer and J. Rebek, Proc. Natl. Acad. Sci. U. S. A., 2006, 103, 12296–12300 CrossRef CAS PubMed. Introduction Starting with the discovery of the inclusion complexes in the late 19th century, supramolecular chemistry developed into an independent field of research until the mid-1960s. 1 From then on, the discipline received considerably more attention culminating in the 2016 chemistry Nobel Prize for molecular machines. Supramolecular chemists initially were driven by the synthesis of ‘chemically beautiful’ molecules, but more recently there has been a shift in focus to synthesise compounds with potential application in a range of disciplines including medicine, 2,3 catalysis 4,5 and materials science. 6 Selective experiment can also be combined with broadband homonuclear decoupling, to yield pure-shift spectra of selected components in mixtures. One advantage of this approach is that the spectra of the minor components are not contaminated by the decoupling artefacts of the major components. 71 Additional proof came from ion mobility mass spectrometry, which showed smaller CCS values for the species [ 17 2 − H] − and [ 17 2 + S − H] − compared to [ 17 2 + PF 6] − and [ 17 2 + PF 6 + S] − (with S = acetone, ΔCCS = 8 Å, Fig. 12A on the left side). This again underlines the exo complexation of PF 6 −, since the biggest change in CCS values should be caused by the species that is attached to the cavity rather than encapsulated in its interior. Moreover, the authors assumed a spherical shape for the molecules and calculated their diameter based on CCS values. For the dimeric species in general, the comparison of those values (between 2.2 and 2.3 nm) with the hydrodynamic radius obtained from DOSY NMR (2.0 nm) and with the X-ray crystal structure (1.9 nm) proved similar structures of the host–guest complex in solution, gas phase and in the solid state. A. C. Toma and T. Pfohl, Supramolecular Chemistry: From Molecules to Nanomaterials, John Wiley & Sons, Ltd, 2012 Search PubMed.

Abstract

S. Korchak, L. Kaltschnee, R. Dervisoglu, L. Andreas, C. Griesinger and S. Gloggler, Angew. Chem., Int. Ed., 2021, 60, 20984 CrossRef CAS PubMed .