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1H NMR spectroscopic titration of the cyclam–marimastat conjugate 12 (0.02 m) with Zn(ClO4)2 (1 m) in [D7]DMF. a) 0.0 equiv; b) 1.0 equiv, 25 °C, 5 min; c) 1.0 equiv, 80 °C, 5 min; d) 1.0 equiv, 80 °C, 1 h; e) 2.0 equiv, 80 °C, 1 h; f) 3.0 equiv, 80 °C, 1 h. S=nondeuterated solvent residual peaks.
