Journal
CHEMISTRY-A EUROPEAN JOURNAL
Volume 11, Issue 24, Pages 7358-7365Publisher
WILEY-V C H VERLAG GMBH
DOI: 10.1002/chem.200500401
Keywords
manganese; silica; silsesquioxane; surface chemistry
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The reaction of [Mn(CH(2)tBu)(2)(tmeda)] (1) and a silica partially dehydroxylated at 700 degrees C (SiO2/700) yields a single surface species [( SiO)Mn(CH(2)tBu)(tmeda)] (2 a; tmeda = tetramethylethylendiamine), while a mixture of 2a and [( SiO)(2)Mn-(tmeda)] (2b) is obtained by using SiO2/200, SiO2/300, or SiO2/500 as evidenced by mass balance analysis, and IR and EPR spectroscopy. ne reaction of I and (c-C5H9)(7)Si7O12SiOH (3), a soluble silanol that is a molecular model for a silica support, generates the bis-siloxy complex 4, [{(c-C5H9)(7)Si7O12SiO}(2)Mn(tmeda)(2)], in a quantitative yield; compound 4 was characterized by single-crystal X-ray diffraction. These reactions exemplify the limitation of considering molecular silanol derivatives as straightforward and reliable homogeneous models for silica, and address the need for thorough characterization of surface species by the use of surface-science techniques. These studies show the possibility of preparing coordinatively and geometrically unique surface species that would be difficult to prepare by solution chemistry methods; insights into the chemical and physical properties of these surface species are also gained.
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