Mixing of metallocyclic trimers and tetramers in an exact 1 : 1.5 stoichiometry provided new supramolecular triangles in quantitative yields. Characterization of the new hetero-nuclear metallomacrocycles was achieved by (1)H, 2D-COSY, 2D-NOESY, and (13)C NMR spectroscopy, along with ESI and TWIM mass spectrometry. Gradient tandem MS (gMS(2)) provided insight into the stabilities of the binuclear structures.
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