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Electrospray‐ionization mass spectrometric studies of poly(methylaluminoxane) (MAO) in the presence of [Cp2ZrMe2], [Cp2ZrMe(Cl)], and [Cp2ZrCl2] in fluorobenzene (PhF) solution are reported. The results demonstrate that alkylation and ionization are separate events that occur at competitive rates in a polar solvent. Furthermore, there are significant differences in ion‐pair speciation that result...
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