Conference Agenda

Overview and details of the sessions of this conference. Please select a date or location to show only sessions at that day or location. Please select a single session for detailed view (with abstracts and downloads if available).

Please note that all times are shown in the time zone of the conference. The current conference time is: 1st Nov 2024, 12:55:54am CET

 
 
Session Overview
Session
Poster - 40 NMR: NMR crystallography
Time:
Thursday, 19/Aug/2021:
5:10pm - 6:10pm

Session Chair: David Bryce
Session Chair: Martin Dracinsky

 


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Presentations

Poster session abstracts

Radomír Kužel



Exploring zinc-terephthalate complexes through multi nuclear ssNMR and in-situ reaction monitoring by Raman spectroscopy

Cesar Leroy1, Thomas-Xavier Métro2, Danielle Laurencin1

1ICGM, Univ Montpellier, CNRS, ENSCM, Montpellier, France; 2IBMM, Univ Montpellier, CNRS, ENSCM, Montpellier, France

Mechanochemistry has shown impressive improvements in past decades for developing sophisticated materials such as pharmaceutical cocrystals, zeolite-based catalysts or metal-organic frameworks (MOFs). [1] The latter are elaborate porous materials exhibiting interesting applications in storage of fuels, capture of CO2, catalysis... [2] Being able to control the nature of MOFs synthesized under mechanochemical conditions thus appears as an important goal. In this context, recently, in-situ methods for mechano-synthesis, such as X-Ray diffraction under synchrotron beam or Raman spectroscopy, have emerged so that information about reaction rates and presence of intermediates are now becoming accessible. [3]

In this contribution, we have studied the formation of zinc-based MOFs using terephthalic acid as organic ligand. The observation of several intermediate phases was made possible by in-situ Raman spectroscopy during ball-milling synthesis (see Fig. 1 a)). Solid-state NMR spectroscopy was then used, along with FTIR, to obtain information about unknown structures observed during the synthetic route. 13C chemical shifts were proven to be sensitive to the binding mode of the dicarboxylic acids on the zinc atoms, in line with previous studies. [4] Chemical shift differences up to 5 ppm (Fig. 1 b)) helped to distinguish between monodentate and bridging binding modes. Moreover, further structural information could be obtained through the use of 17O NMR studies of enriched compounds.

[1] Friščić, T., Mottillo, C. & Titi, H. M. (2020). Angew. Chem. Int. Ed. 59, 1018-1029. [2] Furukawa, H., Cordova, K. E., O’Keeffe, M. & Yaghi, O. M. (2013). Science. 341, 1230444.[3] Kulla, H., Haferkamp, S., Akhmetova, I., Röllig, M., Maierhofer, C., Rademann, K. & Emmerling, F. (2018). Angew. Chem. Int. Ed. 57, 5930-5933. [4] Habib, H. A., Hoffmann, A., Höppe, H. A. & Janiak, C. (2009). Dalton. Trans. 10, 1742-1751.

External Resource:
Video Link


Solid - State NMR Crystallography Analysis of Lorlatinib, an Active Pharmaceutical Ingredient

Zainab Rehman

University of Warwick, Coventry, United Kingdom

A NMR crystallography study is presented for Lorlatinib, an active pharmaceutical ingredient (API) used in the treatment of lung cancer. Various one-dimensional and two-dimensional solid-state magic-angle spinning (MAS) NMR experiments have been performed that provide the 1H and 13C chemical shifts as well as the 14N shifts. A 1H(DQ)-1H(SQ) MAS NMR spectrum was obtained with BaBa recoupling that reveals proton-proton proximities interactions between the 1H nuclei that are typically within 3.5 Å of each other. A 14N-1H HMQC MAS NMR spectrum reveals that one of the NH21H resonances has a significantly low 1H chemical shift; this is interpreted in terms of differences in intermolecular hydrogen bonding. Enhanced resolution is observed in two-dimensional 1H-13C heteronuclear MAS NMR experiments at 1 GHz.

External Resource:
Video Link


 
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