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We report herein a practical approach for regio‐selective B—H/C—H bond activation at azo‐substituted carboranes. The reaction proceeded through Iridium(III)‐induced selective B—H/C—H bond activations based on an azo directing group. Through this strategy, a series of mononuclear, trinuclear and tetranuclear cyclometalated iridium complexes containing Cp*Ir—B or Cp*Ir—C bonds were successfully isolated...
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