Structural Refinement of Carbimazole by NMR Crystallography
| Autor: | Giovanni Barcaro, Francesca Martini, Andrea Scarperi, Aleksandra Pajzderska, Marco Geppi, Elisa Carignani |
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| Jazyk: | angličtina |
| Rok vydání: | 2021 |
| Předmět: |
Diffraction
CP-MAS Materials science structure optimization Pharmaceutical Science 1H-1H DQSQ 02 engineering and technology Crystal structure pharmaceuticals 010402 general chemistry Energy minimization DFT calculations 01 natural sciences Article Analytical Chemistry QD241-441 TheoryofComputation_ANALYSISOFALGORITHMSANDPROBLEMCOMPLEXITY Drug Discovery medicine Physical and Theoretical Chemistry solid state NMR 1H CRAMPS 1H-13C 2D-HETCOR crystalline drugs isotropic chemical shift Organic Chemistry Isotropy 021001 nanoscience & nanotechnology 0104 chemical sciences Characterization (materials science) Crystallography Carbimazole Solid-state nuclear magnetic resonance Chemistry (miscellaneous) Molecular Medicine 0210 nano-technology Two-dimensional nuclear magnetic resonance spectroscopy medicine.drug |
| Zdroj: | Molecules Volume 26 Issue 15 Molecules, Vol 26, Iss 4577, p 4577 (2021) |
| ISSN: | 1420-3049 |
| DOI: | 10.3390/molecules26154577 |
| Popis: | The characterization of the three-dimensional structure of solids is of major importance, especially in the pharmaceutical field. In the present work, NMR crystallography methods are applied with the aim to refine the crystal structure of carbimazole, an active pharmaceutical ingredient used for the treatment of hyperthyroidism and Grave’s disease. Starting from previously reported X-ray diffraction data, two refined structures were obtained by geometry optimization methods. Experimental 1H and 13C isotropic chemical shift measured by the suitable 1H and 13C high-resolution solid state NMR techniques were compared with DFT-GIPAW calculated values, allowing the quality of the obtained structure to be experimentally checked. The refined structure was further validated through the analysis of 1H-1H and 1H-13C 2D NMR correlation experiments. The final structure differs from that previously obtained from X-ray diffraction data mostly for the position of hydrogen atoms. |
| Databáze: | OpenAIRE |
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