On the assignment of 19F MAS NMR spectra of fluoroaluminates using through-space spectral edition of 19F–27Al and 19F–19F connectivities

Literature Information

Publication Date 2008-12-09
DOI 10.1039/B812091A
Impact Factor 3.676
Authors

Christophe Legein, Jean-Yves Buzaré


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Abstract

Advantages and limitations of 19F–27Al and 19F–19F dipolar-based 2D NMR experiments for 19F MAS spectra assignments of fluoroaluminates are presented. In β-BaAlF5, combination of 2D MAS 19F–27Al CP-HETCOR and 19F–19F DQ-SQ NMR correlation experiments allows complete unambiguous assignment of the ten poorly resolved resonances of same relative intensities of the 19F MAS NMR spectrum. The gain in resolution of the 19F MAS 2D spectrum compared to a 1D spectrum is evidenced, allowing distinction of the two shared-fluorine resonances of Ba3Al2F12. Limitations of the 19F MAS DQ-SQ NMR experiment are shown for Ba3Al2F12 and for α-CaAlF5. For β-BaAlF5 and Ba3Al2F12, final line assignments question those previously established from 19F isotropic chemical shift calculations, which demonstrate that such experiments are essential for correct line assignments and assessment of calculation results.

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Physical Chemistry Chemical Physics

Physical Chemistry Chemical Physics
CiteScore: 5.5
Self-citation Rate: 10.3%
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Physical Chemistry Chemical Physics (PCCP) is an international journal co-owned by 19 physical chemistry and physics societies from around the world. This journal publishes original, cutting-edge research in physical chemistry, chemical physics and biophysical chemistry. To be suitable for publication in PCCP, articles must include significant innovation and/or insight into physical chemistry; this is the most important criterion that reviewers and Editors will judge against when evaluating submissions. The journal has a broad scope and welcomes contributions spanning experiment, theory, computation and data science. Topical coverage includes spectroscopy, dynamics, kinetics, statistical mechanics, thermodynamics, electrochemistry, catalysis, surface science, quantum mechanics, quantum computing and machine learning. Interdisciplinary research areas such as polymers and soft matter, materials, nanoscience, energy, surfaces/interfaces, and biophysical chemistry are welcomed if they demonstrate significant innovation and/or insight into physical chemistry. Joined experimental/theoretical studies are particularly appreciated when complementary and based on up-to-date approaches.

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