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The synthetic approaches to [AgIII(CF3)3(NCCH3)] (2) from either [AgIII(CF3)3Cl]- (3⋅Cl) or [AgIII(CF3)4]- (1), originally reported by Eujen and Naumann, are herein reinvestigated owing to major inconsistencies. Naumann's method provides 2 from 1 and HBF4, yet accompanied by its s-triazinyl derivative [AgIII(CF3)3(C6H9N3)] (2'), which is formed in situ through nitrile cyclotrimerization enabled by AgIII/H+. In turn, chloride abstraction from 3·Cl using AgNO3 leads to [AgIII(CF3)3(ONO2)]- (5) instead of 2, as evidenced by NMR spectroscopy, Sc-XRD and EA.
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