Group 8 Metallomacrocycles – Synthesis, Characterization, and Stability

Abstract The one‐step synthesis of the first homoleptic <tpy–Os II –tpy> metallomacrocycle is reported. Characterization of the Os II complex, along with its Fe II and Ru II analogues, was accomplished by NMR spectroscopy, ESI‐MS, TWIM‐MS, gradient tandem‐MS, CV, luminescence and UV/Vis spectroscopy. Center‐of‐mass collision energies, derived from gradient tandem‐MS, reveal that the <tpy–Ru II –tpy>‐based structures are more stable than those of <tpy–Os II –tpy>.