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Preparation and characterization of a number of CoIII and CrIII complexes containing one heterocyclic ligand was reported. The complexes [(NH3)5ML](ClO4)3 (M˭Co, Cr, L=phthalazine, 1‐methylphthalazine, pyridazine, 3‐methylpyridazine) were prepared by reaction of triflato complex [(NH3)5MOSO2CF3] (CF3SO3)2 with the appropriate ligand in sulfolane. These complexes were recrystallized in warm water by addition of NaClO4 and characterized by 1H and 13C NMR spectroscopy and elemental analysis. NOE and DESERT experiments were carried out in order to characterize the position of coordination.
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