In this work,we report the preparation,isolation,and characterization of a family of double-decker silses-quioxane architectures starting from the previously reported DDSQ-Me_(2)H_(2)precursor,a mixture of cis and tra...In this work,we report the preparation,isolation,and characterization of a family of double-decker silses-quioxane architectures starting from the previously reported DDSQ-Me_(2)H_(2)precursor,a mixture of cis and trans isomers.Using such a starting material results in a subsequent mixture of isomers when hydrosilyl-ation reactions using DDSQ-Me_(2)H_(2)and hydroxyalkyl-substituted alkenes catalyzed by Karstedt catalyst are performed.We describe a procedure to sequentially crystallize the two isomers from one another,affording a protocol potentially applicable to other closely related derivatives.The ability to access pure cis and trans isomers of double-decker silsesquioxanes may result in the preparation of new materials and polymers with well-defined properties.All resulting silsesquioxanes were characterized by multinuclear(^(1)H,^(13)C,and^(29)Si)NMR spectroscopy,FT-IR,and HR-MS.Additionally,we report five crystal structures of geometrical isomers,including two cis forms described in the literature for the first time.This is a break-through in itself and sets a new strategy for obtaining such exiting organosilicon-based systems.展开更多
基金supported by the National Science Centre,Poland(Grant No.2020/39/B/ST4/00910).
文摘In this work,we report the preparation,isolation,and characterization of a family of double-decker silses-quioxane architectures starting from the previously reported DDSQ-Me_(2)H_(2)precursor,a mixture of cis and trans isomers.Using such a starting material results in a subsequent mixture of isomers when hydrosilyl-ation reactions using DDSQ-Me_(2)H_(2)and hydroxyalkyl-substituted alkenes catalyzed by Karstedt catalyst are performed.We describe a procedure to sequentially crystallize the two isomers from one another,affording a protocol potentially applicable to other closely related derivatives.The ability to access pure cis and trans isomers of double-decker silsesquioxanes may result in the preparation of new materials and polymers with well-defined properties.All resulting silsesquioxanes were characterized by multinuclear(^(1)H,^(13)C,and^(29)Si)NMR spectroscopy,FT-IR,and HR-MS.Additionally,we report five crystal structures of geometrical isomers,including two cis forms described in the literature for the first time.This is a break-through in itself and sets a new strategy for obtaining such exiting organosilicon-based systems.
