Solid-state synthesis of various tris-cyclometalated iridium(iii) complexesa,b.
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Conditions: for the first step: 1 (0.20 mmol), 2 (0.42 mmol), 2-methoxyethan-1-ol (0.20 μL mg−1) in a stainless-steel milling jar (1.5 mL) with a stainless-steel ball (5 mm). Crude yields are shown. For the second step: 3 (0.05 mmol), AgOTf (0.10 mmol), 2 (0.25 mmol), 2-methoxyethan-1-ol (0.20 μL mg−1) in a stainless-steel milling jar (1.5 mL) with a stainless-steel ball (5 mm). Isolated yields are shown.
DMF (0.50 μL mg−1) was used in a 5 mL jar with a 10 mm ball.