Computation of magnetic shielding to simultaneously validate a crystal structure and assign a solid-state NMR spectrum

Autor:	Stewart J. Clark, Paul Hodgkinson, Andrei S. Batsanov, Robin K. Harris, Dominik B. Jochym, David C. Apperley
Rok vydání:	2012
Předmět:	Carbon-13 NMR satellite Chemistry Chemical shift Organic Chemistry Fluorine-19 NMR Nuclear magnetic resonance crystallography Carbon-13 NMR Analytical Chemistry Inorganic Chemistry Crystallography Solid-state nuclear magnetic resonance Heteronuclear molecule Molecule Spectroscopy
Zdroj:	Journal of Molecular Structure. 1015:192-201
ISSN:	0022-2860
DOI:	10.1016/j.molstruc.2011.10.024
Popis:	The validity of the structure of diterbutaline sulphate diacetic acid solvate in the Cambridge Crystallographic Database (code ZIYXAG) was checked using 13C solid-state NMR together with shielding computations and was found to be in error as far as the geometry of one acetic acid molecule is concerned. A new X-ray diffraction study confirmed the existence of an error and showed there was disorder in the molecule in question. Techniques of NMR crystallography were used to further understand the situation. Two-dimensional (13C, 1H) heteronuclear correlation experiments enabled the 1H chemical shifts to be determined, including those of the hydrogen-bonded protons. NMR was also used to monitor partial desolvation and the 13C spectrum of a new solvate, diterbutaline sulphate monoacetic acid, is reported. Heteronuclear correlation experiments on this new compound allowed most of its proton chemical shifts to be determined and showed that it had one hydrogen bond stronger than any of those in the diacetic acid solvate.
Databáze:	OpenAIRE
Externí odkaz:	https://explore.openaire.eu/search/publication?articleId=doi_________::525dee5308e7d026094f6bb5fbbc19d9 https://doi.org/10.1016/j.molstruc.2011.10.024 Zobrazit plný text záznamu Full Text from ScienceDirect