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Abstract
By reacting NH4VO3 and mpa (mpa = 4-methoxypicolinamide) in the presence of H2O2, a bis-peroxovanadium [NH4][VO(O2)2(mpa)]·H2O (1) was obtained and characterized by X-ray single-crystal diffraction. Structural analyses demonstrate that 1 belongs to the monoclinic space group P21/c and consists of a bis-peroxovanadium [VO(O2)2(mpa)]−, one NH4+ counterion and one free lattice water. Adjacent [VO(O2)2(mpa)]− anions construct a 3D supramolecular framework through intra- and intermolecular hydrogen bonding interactions. The compositions of 1 in solution are investigated by using multinuclear (1H, 13C, and 51V) magnetic resonance, COSY, HSQC, HMBC, and variable temperature NMR in a 0.15 mol L−1 NaCl/D2O solution that mimics the physiological conditions. Comparing the results of single-crystal X-ray and NMR experiments, the VV ion in the undissociated [VO(O2)2(mpa)]− in solution displays a similar seven-coordinate distorted pentagonal bipyramidal geometry with the solid-state crystal. The catalytic activity of the 1 in the oxidative bromination for phenol/aniline-like compounds to mimic bromoperoxidases reactivity was also studied.
Graphical Abstract
Disclosure statement
No potential conflict of interest was reported by the authors.
