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Phase Behavior and Proton Conductivity in Crown Ether-Based Supramolecular Sodium Hydrogen Sulfate Complexes
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DOI：10.1021/acs.cgd.5c01467.png)
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Abstract
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This study deals with the preparation and solid-state characterization, as well as structural and phase transition features of supramolecular complexes composed of sodium hydrogen sulfate (NaHSO4) and two crown ether ligands, namely, 15-crown-5 and benzo-15-crown-5. Single crystals for each compound were grown, and their structures were elucidated via single-crystal X-ray diffraction (XRD) analysis, which highlighted the following compositions: [15-crown-5·Na]HSO4 (1) and [benzo-15-crown-5·Na]HSO4 (2). Microcalorimetric analyses, hot-stage microscopy, and variable-temperature powder X-ray diffraction were employed to analyze thermal stability and phase transition behaviors. Variable-temperature 1H T1 solid-state NMR measurements were also used to monitor proton dynamics and to determine activation energies associated with motion across phase transitions. Formation of supramolecular complexes is crucial for inducing solid–solid transitions, leading to superprotonic phases, namely, crystalline solids exhibiting an enhanced ability to conduct protons, as demonstrated through electrochemical impedance spectroscopy measurement.
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