| Summary: | When synthesizing the versatile precursors (NMe<sub>4</sub>)[Ni(CF<sub>3</sub>)<sub>3</sub>(MeCN)] we recently encountered the problem that marked amounts of C<sub>2</sub>F<sub>5</sub> were incorporated instead of CF<sub>3</sub> under the chosen reaction conditions forming mixed-ligand nickelates [Ni(CF<sub>3</sub>)x(C<sub>2</sub>F<sub>5</sub>)y(MeCN)]<sup>−</sup> (x + y = 3). We studied the three products with y = 0, 1, or 2, using <sup>19</sup>F nuclear magnetic resonance (NMR) spectroscopy and single-crystal X-ray diffraction. We were able to trace the reaction mechanism and solve the problem by modifying the experimental conditions.
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