]. To a solution of 1 2+ [TfO -]2 (30 mg, 0.033 mmol) in CDCl3 (0.5 mL) was added 1-adamantyl isocyanide (9.8 mg, 0.066 mmol) at room temperature and the resulting solution stirred for 5 minutes. Volatiles were removed in vacuo. The residue was dissolved in Et2O (2 mL) and sonicated for 5 minutes, resulting in the formation of white precipitates. The suspension was filtered, and the solids washed with Et2O (2 × 0.5 mL). The solids were then dried under vacuum to yield 5 + [TfO -] (15 mg, 58% yield) as an off-white powder. Single crystals suitable for X-ray crystallography were obtained by slow evaporation from a concentrated chloroform solution at room temperature. Preparation of 8. To a solution of C6F5Br (0.01 mL, 0.079 mmol) in THF (0.5 mL) was added Mg dust (6 mg, 0.25 mmol) and sonicated for an hour. The resulting suspension was filtered into another flask containing [( Me CAACN)2CH + ][TfO -] (30 mg, 0.039 mmol) and stirred for 5 minutes. Volatiles were removed in vacuo. To the solids were added C6D6 (0.5 mL) and filtered. The yield (40% yield) of 8 was determined by H NMR using C6Me6 as internal standard. All spectroscopic data match literature values .