Single-crystal X-ray diffraction study, NMR and electrochemical analysis of a copper( i ) 5,11,17,23-tetra- tert -butyl-25,26,27,28-tetrakis-[(6-methyl-2,2′-bipyridyl-6-yl)methoxy]calix[4]arene complex: an original M 4 L 2 'hand-to-hand' system
| Autor: | Sabine Bouguet-Bonnet, Marc Beley, Sophie Poinsignon, Bernard Malaman, Sébastien Leclerc, Jean-Bernard Regnouf-de-Vains |
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| Přispěvatelé: | Laboratoire Lorrain de Chimie Moléculaire (L2CM), Institut de Chimie du CNRS (INC)-Université de Lorraine (UL)-Centre National de la Recherche Scientifique (CNRS), Institut Jean Lamour (IJL), Université de Lorraine (UL)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Cristallographie, Résonance Magnétique et Modélisations (CRM2), Université de Lorraine (UL)-Centre National de la Recherche Scientifique (CNRS), Laboratoire Énergies et Mécanique Théorique et Appliquée (LEMTA ) |
| Jazyk: | angličtina |
| Rok vydání: | 2019 |
| Předmět: |
Chemistry
[CHIM.ORGA]Chemical Sciences/Organic chemistry Supramolecular chemistry chemistry.chemical_element 02 engineering and technology General Chemistry Nuclear magnetic resonance spectroscopy 010402 general chemistry 021001 nanoscience & nanotechnology 01 natural sciences Copper Catalysis 0104 chemical sciences [CHIM.THEO]Chemical Sciences/Theoretical and/or physical chemistry Crystallography Bipyridine chemistry.chemical_compound Ultraviolet visible spectroscopy Calixarene X-ray crystallography Materials Chemistry Molecule [CHIM.COOR]Chemical Sciences/Coordination chemistry 0210 nano-technology ComputingMilieux_MISCELLANEOUS |
| Zdroj: | New Journal of Chemistry New Journal of Chemistry, Royal Society of Chemistry, 2019, 43 (33), pp.13282-13293. ⟨10.1039/c9nj01152h⟩ |
| ISSN: | 1144-0546 1369-9261 |
| DOI: | 10.1039/c9nj01152h⟩ |
| Popis: | Attempts to prepare a supramolecular M4L2 box involving two tetra-bipyridyl calix[4]arene units and four copper(I) cations afforded, in fact, complex 2 for which, in the solid state, X-ray diffraction analysis showed that the stoichiometry is indeed M4L2, with the two calixarene subunits associated in a “hand-to-hand” mode by complexation via two adjacent bipyridine units to two copper(I) cations, and each group of two residual, adjacent, bipyridine arms is complexed to one copper(I) centre. Mass spectrometry, UV spectroscopy and preliminary 1H-NMR analysis are in preliminary accordance with a monocalixarenic right/left handed M2L structure. Nevertheless, some particularities of the NMR spectrum related to Ar-CH2-Ar and O-CH2bpy resonance signals, the possible generation of the M2L species during the mass spectrometry experiment and the lack of sensitivity of the UV-visible titration caused us to proceed to deeper investigations, looking for other associations, notably the M4L2 “hand-to-hand” systems. This involved 1D and 2D-NMR spectroscopies, among them 1H–15N HMBC, for the reconstruction of the molecule, but also the measurement of self-diffusion coefficients by NMR and electrochemistry. The 2D-NMR analysis and NMR self-diffusion evaluation were in accordance with the M2L structure, but the electrochemical self-diffusion experiment indicated a M4L2 structure. |
| Databáze: | OpenAIRE |
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