The present invention relates to a process for forming a composition comprising oligomeric alkylaluminoxane, e.g., preferably methylaluminoxane, and moieties having the structure-OC(R)3, where R is, for example, methyl, which comprises initially treating a composition comprising trialkylaluminum with a reagent containing a carbon-oxygen double bond, such as, carbon dioxide, followed by hydrolysis of the resulting composition with water. Another embodiment of the invention a composition comprising oligomeric methylaluminoxane and greater than 10 mole % of moieties of the structure -OC(R)3, where R is methyl, which, when such composition is hydrolyzed, there is an evolution of hydrolysis products of methane and at least one C2 or higher alkane, such as t-butane.
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