Synthesis and Advanced NMR Characterization of Ordered 3D Reticular Materials with PolySilicate Nodes and Hydrophobic OrganoSilicone Linkers

This work describes the synthesis of ordered 3D siloxane-silsesquioxane reticular materials with silicate D4R cubes (Si8O208−), harvested from a sacrificial tetrabutylammonium cyclosilicate hydrate (TBA-CySH) precursor, interlinked with octyl and dicyclopentyl (Cp2) hydrocarbon functionalities in a...

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Vydáno v:Molecules (Basel, Switzerland) Ročník 30; číslo 2; s. 228
Hlavní autoři: Jamoul, Jelle, Radhakrishnan, Sambhu, Houlleberghs, Maarten, Chandran, C. Vinod, Vits, Aline, Weckx, Pasquinel, Smet, Sam, Arenas Esteban, Daniel, Bals, Sara, Martens, Johan A., Breynaert, Eric
Médium: Journal Article
Jazyk:angličtina
Vydáno: Switzerland MDPI AG 01.01.2025
MDPI
Témata:
Crystal structure
cyclosilicate hydrate
Nuclear magnetic resonance spectroscopy
octyl-methyldichlorosilane
Polymer blends
Polymerization
POSiSils
reticular material synthesis
Silane
silicate-silicone hybrids
Silicates
Silicones
siloxane-silsesquioxane
Spectrum analysis
Water
Belgium
advanced multidimensional NMR characterization
siloxane-silsesquioxane
29Si NMR
octyl-methyldichlorosilane
reticular material synthesis
POSiSils
cyclosilicate hydrate
dicyclopentyldichlorosilane
silicate-silicone hybrids
ISSN:1420-3049, 1420-3049
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Shrnutí:This work describes the synthesis of ordered 3D siloxane-silsesquioxane reticular materials with silicate D4R cubes (Si8O208−), harvested from a sacrificial tetrabutylammonium cyclosilicate hydrate (TBA-CySH) precursor, interlinked with octyl and dicyclopentyl (Cp2) hydrocarbon functionalities in a one-step synthesis with organodichlorosilanes. Advanced solid-state NMR spectroscopy allowed us to unravel the molecular order of the nodes and their interconnection by the silicone linkers. In the case of octyl-methyl silicone linkers, changing the silane-to-silicate ratio in the synthesis allowed for tuning the length of the linker between the nodes. With dicyclopentyl linkers, the addition of dimethyldichlorosilane was essential to enable the formation of a reticular network. The resulting materials contained mixed, dimeric silicone linkers, i.e., Si8-O-Si(Me2)-O-Si(Cp2)-O-Si8.
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These authors contributed equally to this work.
ISSN:1420-3049
1420-3049
DOI:10.3390/molecules30020228