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<p>Methylaluminoxane (MAO) is a key activator for olefin polymerization catalysts, making its chemistry of ongoing interest. Neutral donors such as octamethyltrisiloxane (OMTS) are effective abstractors of the dimethylaluminum cation, [Me<sub>2</sub>Al]<sup>+</sup>, from methylaluminoxane (MAO), and this process can be readily investigated using electrospray ionization mass spectrometry (ESI-MS) in fluorobenzene (PhF) solution. Complementary studies employing 1D and 2D <sup>1</sup>H NMRdoi:10.26434/chemrxiv.7701710.v1 fatcat:f2iepbzwmba63fokimcuvlnh5i