Abstract
Immobilized decamethylzirconocene methyl cation on a silica support was generated by treatment of Cp*2ZrMe2 with tethered borate activator [(SiO2)x(Al(iBu)n(OC6H4B(C6F5)3)2–n][R2R′NH] (NEt: R = R′ = Et or NPh: R = Me; R′ = Ph). The concentration of [Cp*2ZrMe]+ on the support was quantified using a newly developed and straightforward method that involves trapping and releasing the active species by subsequent treatment with vinyl methyl thioethers (CH2CH(CH2)nSMe, n = 1, 2) and ammonium bromide, [Bu4N]Br, followed by quantification using simple 1H NMR spectroscopic tools. Reaction of [Cp*2ZrMe]+ with the trapping agent results in formation of stable metallacycle [Cp*2Zr(CH2CHMe(CH2)nSMe)]+ (n = 1, 2); ion exchange in Cp*2Zr(Br)(CH2CHMe(CH2)nSMe) (n = 1,2). This affords a measure for the number of ionic species that were initially present on the support. In this particular case, full conversion of the decamethyl zirconocene precursor to the corresponding cation, [Cp*2ZrMe]+, was observed. Whereas trapping w...
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