Structures of rhenium(I) complexes with 3-hydroxyflavone and benzhydroxamic acid as O,O′-bidentate ligands and confirmation of π-stacking by solid-state NMR spectroscopy
| Autor: | Renier Koen, Marietjie Schutte-Smith, Roger Alberto, Leo Kirsten, Hendrik G. Visser, Andreas Roodt, Linette Twigge |
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| Přispěvatelé: | University of Zurich, Schutte-Smith, Marietjie |
| Jazyk: | angličtina |
| Rok vydání: | 2019 |
| Předmět: |
10120 Department of Chemistry
Denticity 3104 Condensed Matter Physics 010405 organic chemistry 1604 Inorganic Chemistry Synthon chemistry.chemical_element Nuclear magnetic resonance spectroscopy Crystal structure Rhenium Carbon-13 NMR 010402 general chemistry Condensed Matter Physics 01 natural sciences 0104 chemical sciences Inorganic Chemistry Crystallography chemistry Solid-state nuclear magnetic resonance 540 Chemistry Materials Chemistry Magic angle spinning Physical and Theoretical Chemistry 1606 Physical and Theoretical Chemistry 2505 Materials Chemistry |
| Popis: | The synthesis and crystal structures of two new rhenium(I) complexes obtained utilizing benzhydroxamic acid (BHAH) and 3-hydroxyflavone (2-phenylchromen-4-one, FlavH) as bidentate ligands, namely tetraethylammonium fac-(benzhydroxamato-κ2 O,O′)bromidotricarbonylrhenate(I), (C8H20N)[ReBr(C7H6NO2)(CO)3], 1, and fac-aquatricarbonyl(4-oxo-2-phenylchromen-3-olato-κ2 O,O′)rhenium(I)–3-hydroxyflavone (1/1), [Re(C15H9O3)(CO)3(H2O)]·C15H10O3, 3, are reported. Furthermore, the crystal structure of free 3-hydroxyflavone, C15H10O3, 4, was redetermined at 100 K in order to compare the packing trends and solid-state NMR spectroscopy with that of the solvate flavone molecule in 3. The compounds were characterized in solution by 1H and 13C NMR spectroscopy, and in the solid state by 13C NMR spectroscopy using the cross-polarization magic angle spinning (CP/MAS) technique. Compounds 1 and 3 both crystallize in the triclinic space group P\overline{1} with one molecule in the asymmetric unit, while 4 crystallizes in the orthorhombic space group P212121. Molecules of 1 and 3 generate one-dimensional chains formed through intermolecular interactions. A comparison of the coordinated 3-hydroxyflavone ligand with the uncoordinated solvate molecule and free molecule 4 shows that the last two are virtually completely planar due to hydrogen-bonding interactions, as opposed to the former, which is able to rotate more freely. The differences between the solid- and solution-state 13C NMR spectra of 3 and 4 are ascribed to inter- and intramolecular interactions. The study also investigated the potential labelling of both bidentate ligands with the corresponding fac-99mTc-tricarbonyl synthon. All attempts were unsuccessful and reasons for this are provided. |
| Databáze: | OpenAIRE |
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