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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Veröffentlicht in:	Molecules (Basel, Switzerland) Jg. 30; H. 2; S. 228
Hauptverfasser:	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
Format:	Journal Article
Sprache:	Englisch
Veröffentlicht:	Switzerland MDPI AG 01.01.2025 MDPI
Schlagworte:	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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Abstract	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.
AbstractList	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. This work describes the synthesis of ordered 3D siloxane-silsesquioxane reticular materials with silicate D4R cubes (Si[sub.8]O[sub.20] [sup.8−]), harvested from a sacrificial tetrabutylammonium cyclosilicate hydrate (TBA-CySH) precursor, interlinked with octyl and dicyclopentyl (Cp[sub.2]) 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]-O-Si(Me[sub.2])-O-Si(Cp[sub.2])-O-Si[sub.8]. 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.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. This work describes the synthesis of ordered 3D siloxane-silsesquioxane reticular materials with silicate D4R cubes (Si O ), harvested from a sacrificial tetrabutylammonium cyclosilicate hydrate (TBA-CySH) precursor, interlinked with octyl and dicyclopentyl (Cp ) 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 -O-Si(Me )-O-Si(Cp )-O-Si .
Audience	Academic
Author	Smet, Sam Breynaert, Eric Radhakrishnan, Sambhu Martens, Johan A. Weckx, Pasquinel Jamoul, Jelle Chandran, C. Vinod Arenas Esteban, Daniel Houlleberghs, Maarten Vits, Aline Bals, Sara
AuthorAffiliation	2 NMRCoRe—NMR/X-Ray Platform for Convergence Research, KU Leuven, Celestijnenlaan 200F Box 2461, 3001 Heverlee, Belgium 3 Electron Microscopy for Materials Science (EMAT), University of Antwerp, Groenenborgerlaan 171, 2020 Antwerp, Belgium 1 Centre for Surface Chemistry and Catalysis—Characterization and Application Team (COK-KAT), KU Leuven, Celestijnenlaan 200F Box 2461, 3001 Heverlee, Belgium
AuthorAffiliation_xml	– name: 3 Electron Microscopy for Materials Science (EMAT), University of Antwerp, Groenenborgerlaan 171, 2020 Antwerp, Belgium – name: 2 NMRCoRe—NMR/X-Ray Platform for Convergence Research, KU Leuven, Celestijnenlaan 200F Box 2461, 3001 Heverlee, Belgium – name: 1 Centre for Surface Chemistry and Catalysis—Characterization and Application Team (COK-KAT), KU Leuven, Celestijnenlaan 200F Box 2461, 3001 Heverlee, Belgium
Author_xml	– sequence: 1 givenname: Jelle orcidid: 0000-0002-8466-6664 surname: Jamoul fullname: Jamoul, Jelle – sequence: 2 givenname: Sambhu orcidid: 0000-0002-0274-2759 surname: Radhakrishnan fullname: Radhakrishnan, Sambhu – sequence: 3 givenname: Maarten orcidid: 0000-0002-8456-0886 surname: Houlleberghs fullname: Houlleberghs, Maarten – sequence: 4 givenname: C. Vinod orcidid: 0000-0003-4074-8833 surname: Chandran fullname: Chandran, C. Vinod – sequence: 5 givenname: Aline surname: Vits fullname: Vits, Aline – sequence: 6 givenname: Pasquinel orcidid: 0000-0001-8796-8265 surname: Weckx fullname: Weckx, Pasquinel – sequence: 7 givenname: Sam surname: Smet fullname: Smet, Sam – sequence: 8 givenname: Daniel surname: Arenas Esteban fullname: Arenas Esteban, Daniel – sequence: 9 givenname: Sara surname: Bals fullname: Bals, Sara – sequence: 10 givenname: Johan A. orcidid: 0000-0002-9292-2357 surname: Martens fullname: Martens, Johan A. – sequence: 11 givenname: Eric orcidid: 0000-0003-3499-0455 surname: Breynaert fullname: Breynaert, Eric
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Keywords	advanced multidimensional NMR characterization siloxane-silsesquioxane 29Si NMR octyl-methyldichlorosilane reticular material synthesis POSiSils cyclosilicate hydrate dicyclopentyldichlorosilane silicate-silicone hybrids
Language	English
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Snippet	This work describes the synthesis of ordered 3D siloxane-silsesquioxane reticular materials with silicate D4R cubes (Si8O208−), harvested from a sacrificial... This work describes the synthesis of ordered 3D siloxane-silsesquioxane reticular materials with silicate D4R cubes (Si O ), harvested from a sacrificial... This work describes the synthesis of ordered 3D siloxane-silsesquioxane reticular materials with silicate D4R cubes (Si[sub.8]O[sub.20] [sup.8−]), harvested... This work describes the synthesis of ordered 3D siloxane-silsesquioxane reticular materials with silicate D4R cubes (Si8O208-), harvested from a sacrificial...
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SubjectTerms	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
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Title	Synthesis and Advanced NMR Characterization of Ordered 3D Reticular Materials with PolySilicate Nodes and Hydrophobic OrganoSilicone Linkers
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