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The controlled assembly of molecular building blocks enables the rational design of nanomaterials. In this study, two types of cage-type oligosiloxanes with double-three ring (D3R) structures are modified with dimethylsilanol groups to form supramolecular assemblies. One is the siloxane cage derived from Si(OEt)4 (denoted as the Q6 cage), and the other is the organosiloxane cage derived from (EtO)3Si-CH2-Si(OEt)3 (denoted as the T6 cage). The syntheses of the silanol-modified cages are performed in two steps: (i) dimethylsilylation of the corner Si-O- groups on the Q6 and T6 cages to introduce Si-H groups and (ii) subsequent oxidation of the Si-H groups to Si-OH groups. Dimethylsilylation of the cages is conducted at much lower temperatures (-94 and -78 °C for Q6 and T6 cages, respectively) than those used for conventional silylation, which is the key to suppressing the deterioration of the unstable D3R structure. The subsequent oxidation of the Si-H groups proceeds successfully, and the crystallization of these molecules is induced by the hydrogen bonds of the silanol groups. The crystal structure of the Q6 cage modified with dimethylsilanol groups can be regarded as a layered structure with tetrahydrofuran between the layers. In contrast, the T6 cage modified with dimethylsilanol groups assembled to form a more densely packed structure with no included solvent molecules. The differences between the crystal structures are discussed in terms of the shape of the cages. The insight into the effect of the shape of the cage on its assembly behavior will lead to the designable synthesis of crystalline siloxane-based materials.
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http://dx.doi.org/10.1039/c8dt04244f | DOI Listing |
Dalton Trans
February 2019
Department of Applied Chemistry, Faculty of Science and Engineering, Waseda University, 3-4-1 Okubo, Shinjuku-ku, Tokyo 169-8555, Japan.
The controlled assembly of molecular building blocks enables the rational design of nanomaterials. In this study, two types of cage-type oligosiloxanes with double-three ring (D3R) structures are modified with dimethylsilanol groups to form supramolecular assemblies. One is the siloxane cage derived from Si(OEt)4 (denoted as the Q6 cage), and the other is the organosiloxane cage derived from (EtO)3Si-CH2-Si(OEt)3 (denoted as the T6 cage).
View Article and Find Full Text PDFChemistry
November 2018
Department of Applied Chemistry, Faculty of Science and Engineering, Waseda University, 3-4-1 Okubo, Shinjuku-ku, Tokyo, 169-8555, Japan.
Controlled assembly of siloxane-based building blocks provides a rational approach toward designed architectures of silica-based porous materials. Here, a non-hydrothermal method to prepare microporous crystals from cage-type oligosiloxanes is reported. The crystals formation occurs through an ordered assembly assisted by hydrogen bonds and subsequent intermolecular connection by silylation.
View Article and Find Full Text PDFChem Commun (Camb)
July 2015
Department of Applied Chemistry, Faculty of Science and Engineering, Waseda University, 3-4-1 Ohkubo, Shinjuku-ku, Tokyo 169-8555, Japan.
A new class of ordered silica-based materials has been prepared by hydrogen bond-directed assembly of cage siloxanes modified with dimethylsilanol groups, providing a soft-chemical approach to crystalline silica materials with molecularly designed architectures.
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