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Quadrupolar NMR crystallography guided crystal structure prediction (QNMRX-CSP).
- Source :
- CrystEngComm; 9/21/2024, Vol. 26 Issue 35, p4782-4803, 22p
- Publication Year :
- 2024
-
Abstract
- We describe a new quadrupolar NMR crystallography guided crystal structure prediction (QNMRX-CSP) protocol for the prediction and refinement of crystal structures, including its design, benchmarking, and application to seven organic HCl salts. Five HCl salts with a limited number of low-energy conformations were chosen as model systems for benchmarking: betaine HCl, glycine HCl, D -alanine HCl, guanidine HCl, and aminoguanidine HCl; two were chosen for blind tests: N,N′-dimethylglycine HCl and metformin HCl. The QNMRX-CSP protocol uses experimental <superscript>35</superscript>Cl solid-state NMR (SSNMR) spectra and X-ray diffraction (XRD) data in tandem with Monte Carlo simulated annealing and dispersion-corrected plane-wave density functional theory (DFT-D2*) calculations. The protocol comprises three modules: (i) the assignment of motion groups, (ii) a Monte Carlo simulated annealing algorithm for generating tens of thousands of candidate structures, and (iii) DFT-D2* geometry optimizations of structural models and concomitant computation of <superscript>35</superscript>Cl EFG tensors. Key benchmarked metrics are used for retaining the best candidate structures, including unit cell parameters, static lattice energies, and EFG distances (Γ<subscript>EFG</subscript>). The protocol is shown to generate structural models that are excellent matches with experimental crystal structures that have been DFT-D2* geometry optimized, as validated by crystallographic R-factors (R) and root-mean squared distances (RMSDs) of atomic positions that are well below 10% and 0.2 Å, respectively. Finally, consideration is given to the use of the QNMRX-CSP protocol as a standalone technique or in concert with other NMRX methods and Rietveld refinements, and possible applications employing other quadrupolar nuclei (i.e., <superscript>14</superscript>N and <superscript>17</superscript>O). [ABSTRACT FROM AUTHOR]
Details
- Language :
- English
- ISSN :
- 14668033
- Volume :
- 26
- Issue :
- 35
- Database :
- Complementary Index
- Journal :
- CrystEngComm
- Publication Type :
- Academic Journal
- Accession number :
- 179534083
- Full Text :
- https://doi.org/10.1039/d3ce01306e