Description:
<jats:p>We report the synthesis and full characterization of a novel series of indole‐derived triazolium salts and their corresponding triazolylidene gold, palladium, rhodium, and iridium complexes. All new compounds were fully characterized by means of <jats:sup>1</jats:sup>H and <jats:sup>13</jats:sup>C NMR spectroscopy, elemental analyses, and in the case of triazoliums <jats:bold>1</jats:bold> and <jats:bold>2</jats:bold> and complexes <jats:bold>3</jats:bold>, <jats:bold>4</jats:bold>, and <jats:bold>9</jats:bold>, by single crystal X‐ray diffraction. Gold complexes demonstrated a good catalytic performance in the hydrohydrazination of terminal alkynes producing a series of substituted hydrazones in good yields under mild reaction conditions. Additionally, the iridium complex (<jats:bold>9</jats:bold>) performed well in the catalytic transfer hydrogenation of ketones and aldehydes using isopropanol as hydrogen source.</jats:p>