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The hydridoirida‐β‐diketone [(IrH{(PPh2(o‐C6H4CO))2H})2(μ‐Cl)][BF4] (2) has been used as a homogeneous catalyst for the methanolysis of ammonia‐borane to release up to 3 equivalents of hydrogen in the presence of air. With catalyst loadings as low as 0.2 mol%, ammonia‐borane undergoes methanolysis within 6 min at 30 °C, with TOF50% of 320 molH2 ⋅ molIr−1 ⋅ min−1, or within 80 s at 60 °C, with an excellent...
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