Rare-earth organic coordination polymer taking 4,4'-bipyridyl as template, and preparation method and application thereof
A coordination polymer, rare earth organic technology, applied in the direction of organic compound/hydride/coordination complex catalysts, compounds containing elements of Group 3/13 of the periodic table, organic chemistry, etc., can solve the problem of rare earth coordination polymers. Less synthesis and other problems, to achieve the effect of easy large-scale industrial production, high yield and novel structure
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Embodiment 1
[0049] {(bpy)[Pr(ip) 1.5 (H 2 O) 4 ]} n Synthesis
[0050] Pr(NO 3 ) 3 ·6H 2 O (0.5mmol, 218mg), isophthalic acid (0.5mmol, 83mg), 4,4'-bipyridine (0.5mmol, 78mg) were dissolved in 15ml of distilled water, stirred evenly, and the pH of the reaction system was adjusted with triethylamine Value = 7-8, then added to the reaction kettle, heated up, reacted at 120°C for 72 hours, gradually lowered the temperature, cooled to room temperature, filtered, washed with water, dried to obtain blocky green crystals. The resulting crystals were monochromated with graphite molybdenum target MoKα rays on the Rigaku RAXIS-RAPID single crystal X-ray diffractometer of Japan Rigaku Corporation. Diffraction data were collected at 293(2)K in ω-scan mode. The initial structure of the crystal was solved by the direct method using the SHELX-97 program, and then the coordinates of all non-hydrogen atoms were obtained by the difference Fourier synthesis method and the least square method, and a...
Embodiment 2
[0054] {(bpy)[Nd(ip) 1.5 (H 2 O) 4 ]} n Synthesis
[0055] Nd(OH) 3 (0.25mmol, 49mg), isophthalic acid (3.75mmol, 623mg), 4,4'-bipyridine (3.75mmol, 585mg) were dissolved in 25ml of distilled water and 25ml of methanol, stirred evenly, and adjusted the pH of the reaction system with hydrochloric acid Value = 6-7, then added to the reaction kettle, heated up, reacted at 80°C for 240 hours, gradually lowered the temperature, cooled to room temperature, filtered, washed with water, dried to obtain blocky purple crystals. The resulting crystals were monochromated with graphite molybdenum target MoKα rays on the Rigaku RAXIS-RAPID single crystal X-ray diffractometer of Japan Rigaku Corporation. Diffraction data were collected at 293(2)K in ω-scan mode. The initial structure of the crystal was solved by the direct method using the SHELX-97 program, and then the coordinates of all non-hydrogen atoms were obtained by the difference Fourier synthesis method and the least square ...
Embodiment 3
[0059] {(bpy)[Sm(ip) 1.5 (H 2 O) 4 ]} n Synthesis
[0060] SmCl 3 ·6H 2 O (0.5mmol, 182mg), isophthalic acid (2.0mmol, 332mg), 4,4'-bipyridine (1.0mmol, 156mg) were dissolved in 10ml of distilled water and 5ml of ethanol, stirred evenly, and adjusted with sodium hydroxide solution The pH value of the reaction system is 8-9, then added to the reaction kettle, heated up, and reacted at 140°C for 24 hours, then gradually lowered the temperature, cooled to room temperature, filtered, washed with water, and dried to obtain blocky yellow crystals. The resulting crystals were monochromated with graphite molybdenum target MoKα rays on the RigakuRAXIS-RAPID single crystal X-ray diffractometer of Japan Rigaku Corporation. Diffraction data were collected at 293(2K in ω scan mode. The initial structure of the crystal was solved by the direct method using the SHELX-97 program, and then the coordinates of all non-hydrogen atoms were obtained by the difference Fourier synthesis method...
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