Sodium β-Diketonate Glyme Adducts as Precursors for Fluoride Phases: Synthesis, Characterization and Functional Validation

Very few sodium complexes are available as precursors for the syntheses of sodium-based nanostructured materials. Herein, the diglyme, triglyme, and tetraglyme (CH<sub>3</sub>O(CH<sub>2</sub>CH<sub>2</sub>O)<sub>n</sub>CH<sub>3</sub>, <i...

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Bibliographic Details
Main Authors: Nishant Peddagopu, Anna L. Pellegrino, Carmela Bonaccorso, Patrizia Rossi, Paola Paoli, Graziella Malandrino
Format: Article
Language:English
Published: MDPI AG 2022-09-01
Series:Molecules
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Online Access:https://www.mdpi.com/1420-3049/27/19/6282
Description
Summary:Very few sodium complexes are available as precursors for the syntheses of sodium-based nanostructured materials. Herein, the diglyme, triglyme, and tetraglyme (CH<sub>3</sub>O(CH<sub>2</sub>CH<sub>2</sub>O)<sub>n</sub>CH<sub>3</sub>, <i>n</i> = 2–4) adducts of sodium hexafluoroacetylacetonate were synthesized in a single-step reaction and characterized by IR spectroscopy, <sup>1</sup>H, and <sup>13</sup>C NMR. Single-crystal X-ray diffraction studies provide evidence of the formation of the ionic oligomeric structure [Na<sub>4</sub>(hfa)<sub>6</sub>]<sup>2−</sup>•2[Na(diglyme<sub>2</sub>]<sup>+</sup> when the diglyme is coordinated, while a mononuclear seven-coordinated complex Na(hfa)•tetraglyme is formed with the tetraglyme. Reaction with the monoglyme (CH<sub>3</sub>OCH<sub>2</sub>CH<sub>2</sub>OCH<sub>3</sub>) does not occur, and the unadducted polymeric structure [Na(hfa)]<sub>n</sub> forms, while the triglyme gives rise to a liquid adduct, Na(hfa)•triglyme•H<sub>2</sub>O. Thermal analysis data reveal great potentialities for their applications as precursors in metalorganic chemical vapor deposition (MOCVD) and sol-gel processes. As a proof-of-concept, the Na(hfa)•tetraglyme adduct was successfully applied to both the low-pressure MOCVD and the sol-gel/spin-coating synthesis of NaF films.
ISSN:1420-3049