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 (Si<sub>8</sub>O<sub>20</sub><sup>8−</sup>), harvested from a sacrificial tetrabutylammonium cyclosilicate hydrate (TBA-CySH) precursor, interlinked...
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| Main Authors: | , , , , , , , , , , |
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| Format: | Article |
| Language: | English |
| Published: |
MDPI AG
2025-01-01
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| Series: | Molecules |
| Subjects: | |
| Online Access: | https://www.mdpi.com/1420-3049/30/2/228 |
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| Summary: | This work describes the synthesis of ordered 3D siloxane-silsesquioxane reticular materials with silicate D4R cubes (Si<sub>8</sub>O<sub>20</sub><sup>8−</sup>), harvested from a sacrificial tetrabutylammonium cyclosilicate hydrate (TBA-CySH) precursor, interlinked with octyl and dicyclopentyl (Cp<sub>2</sub>) 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., Si<sub>8</sub>-O-Si(Me<sub>2</sub>)-O-Si(Cp<sub>2</sub>)-O-Si<sub>8</sub>. |
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| ISSN: | 1420-3049 |