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A new type of rigid ligand, 4,5-di(4'-carboxyphenyl)phthalic acid, was synthesized by using rigid polycarboxylate ligands. The ligand is expected to be stable under water splitting conditions. Based on H4L and two N donors, 4,4'-bipyridine (4,4'-bpy) and (E)-1,2-di(pyridin-4-yl)diazene (called nitre), two metal(II) complexes were obtained: [Co4L2(4,4'-bpy)(H2O)6]·3.5 H2O (1) and [Co3L(nitrene)(H2O)4]·DMF (2; DMF = dimethylformamide). Their cyclic voltammograms (CV), Tafel plots, electrochemical impedance spectroscopy (EIS), controlled potential electrolysis (CPE) experiments, powder XRD (PXRD) data after CPE, thermal stability and UV/Vis absorption spectra are also presented. A mixture of CoSO4·7H2O (0.1mmol, 0.028g), L (0.05mmol, 0.020g), (E)-1,2-di(pyridin-4-yl)diazene (0.05 mmol, 0.010 g), water (6mL), ethanol (2mL), NH3·H2O (0.4mL) and DMF (0.1mL) was sealed in a polytetrafluoroethylene autoclave and heated at 120±8℃ for 3 days, followed by slow cooling to room temperature. The resulting red flaky crystals were separated by filtration (yield, based on Co, about 38%). Infrared: v˜ = 3268(s), 3077(w), 2976(w), 1598(s), 1538(s), 1396(s), 1229(w), 1179(w), 1091(w), 1016(m), 921(w), 845(s), 786(w), 720(w), 676(m), 572(m), 458(w) cm-1.
A new type of rigid ligand, 4,5-di(4'-carboxyphenyl)phthalic acid, was synthesized by using rigid polycarboxylate ligands. The ligand is expected to be stable under water splitting conditions. Based on H4L and two N donors, 4,4'-bipyridine (4,4'-bpy) and (E)-1,2-di(pyridin-4-yl)diazene (called nitre), two metal(II) complexes were obtained: [Co4L2(4,4'-bpy)(H2O)6]·3.5 H2O (1) and [Co3L(nitrene)(H2O)4]·DMF (2; DMF = dimethylformamide). Their cyclic voltammograms (CV), Tafel plots, electrochemical impedance spectroscopy (EIS), controlled potential electrolysis (CPE) experiments, powder XRD (PXRD) data after CPE, thermal stability and UV/Vis absorption spectra are also presented.
A mixture of CoSO4·7H2O (0.1mmol, 0.028g), L (0.05mmol, 0.020g), (E)-1,2-di(pyridin-4-yl)diazene (0.05 mmol, 0.010 g), water (6mL), ethanol (2mL), NH3·H2O (0.4mL) and DMF (0.1mL) was sealed in a polytetrafluoroethylene autoclave and heated at 120±8℃ for 3 days, followed by slow cooling to room temperature. The resulting red flaky crystals were separated by filtration (yield, based on Co, about 38%). Infrared: v˜ = 3268(s), 3077(w), 2976(w), 1598(s), 1538(s), 1396(s), 1229(w), 1179(w), 1091(w), 1016(m), 921(w), 845(s), 786(w), 720(w), 676(m), 572(m), 458(w) cm-1.