Synthesis, Spectral Studies, and Structural Characterization of a New Organosilanetriol, Its Amine Complexes, and a Surface Lewis Basic Cubic Aluminosilicate

Synthesis, Spectral Studies, and Structural Characterization of a New Organosilanetriol, Its Amine Complexes, and a Surface Lewis Basic Cubic Aluminosilicate

The new trichlorosilane 2,6-Et2C6H3N(SiMe3)SiCl3 (2) on controlled hydrolysis yields 2,6-Et2C6H3N(SiMe3)Si(OH)3 (3). X-ray diffraction analysis of 3 reveals a rare structure type of aggregation where eight molecules of the silanetriol form an octameric cage through intermolecular O−H···O hydrogen bo...

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Veröffentlicht in:Organometallics 2005-04, Vol.24 (9), p.2124-2128
Hauptverfasser: Prabusankar, Ganesan, Murugavel, Ramaswamy, Butcher, Ray J.
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creator Prabusankar, Ganesan
Murugavel, Ramaswamy
Butcher, Ray J.
description The new trichlorosilane 2,6-Et2C6H3N(SiMe3)SiCl3 (2) on controlled hydrolysis yields 2,6-Et2C6H3N(SiMe3)Si(OH)3 (3). X-ray diffraction analysis of 3 reveals a rare structure type of aggregation where eight molecules of the silanetriol form an octameric cage through intermolecular O−H···O hydrogen bonding. Reaction of 3 with piperazine (PIP), 4,4‘-bipyridine (BPY), and 1,4-diazabicyclo[2,2,2]octane (DABCO) yields [{2,6-Et2C6H3N(SiMe3)Si(OH)3}·{PIP}] (4), [{2,6-Et2C6H3N(SiMe3)Si(OH)3}·{BPY}] (5), and [{2,6-Et2C6H3N(SiMe3)Si(OH)3}·{DABCO}] (6), respectively. Treatment of 6 with HAl i Bu2 affords the cubic aluminosiloxane [2,6-Et2C6H3N(SiMe3)SiO3Al(DABCO)]4·1,4-dioxane (7). The aluminum centers on the cubic core are coordinated by DABCO molecules in a monodentate fashion.
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X-ray diffraction analysis of 3 reveals a rare structure type of aggregation where eight molecules of the silanetriol form an octameric cage through intermolecular O−H···O hydrogen bonding. Reaction of 3 with piperazine (PIP), 4,4‘-bipyridine (BPY), and 1,4-diazabicyclo[2,2,2]octane (DABCO) yields [{2,6-Et2C6H3N(SiMe3)Si(OH)3}·{PIP}] (4), [{2,6-Et2C6H3N(SiMe3)Si(OH)3}·{BPY}] (5), and [{2,6-Et2C6H3N(SiMe3)Si(OH)3}·{DABCO}] (6), respectively. Treatment of 6 with HAl i Bu2 affords the cubic aluminosiloxane [2,6-Et2C6H3N(SiMe3)SiO3Al(DABCO)]4·1,4-dioxane (7). 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X-ray diffraction analysis of 3 reveals a rare structure type of aggregation where eight molecules of the silanetriol form an octameric cage through intermolecular O−H···O hydrogen bonding. Reaction of 3 with piperazine (PIP), 4,4‘-bipyridine (BPY), and 1,4-diazabicyclo[2,2,2]octane (DABCO) yields [{2,6-Et2C6H3N(SiMe3)Si(OH)3}·{PIP}] (4), [{2,6-Et2C6H3N(SiMe3)Si(OH)3}·{BPY}] (5), and [{2,6-Et2C6H3N(SiMe3)Si(OH)3}·{DABCO}] (6), respectively. Treatment of 6 with HAl i Bu2 affords the cubic aluminosiloxane [2,6-Et2C6H3N(SiMe3)SiO3Al(DABCO)]4·1,4-dioxane (7). 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