Three-dimensional coordination polymer nonlinear optical material and preparation method thereof
A technology of coordination polymer and nonlinear optics, which is applied in the field of three-dimensional coordination polymer nonlinear optical materials and its preparation, and achieves the effect of simple preparation process and high yield
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Embodiment 1
[0017] Take 2-(4-pyridyl)-1H-imidazole-4,5-dicarboxylic acid (0.5mmol), potassium thiocyanate (1mmol) and MnCl 2 4H 2 O (1mmol) was added to 6 ml of water, stirred for 20 minutes, then sealed in a 25 ml polytetrafluoroethylene reactor, kept at a constant temperature of 160°C for 3 days, cooled to room temperature, filtered, washed, and dried to obtain a yellow block crystals with a yield of 64%.
Embodiment 2
[0019] Take 2-(4-pyridyl)-1H-imidazole-4,5-dicarboxylic acid (0.5mmol), potassium thiocyanate (0.8mmol) and MnCl 2 4H 2 O (1 mmol) was added to 5 ml of water, stirred for 20 minutes, then sealed in a 25 ml polytetrafluoroethylene reactor, kept at a constant temperature of 170°C for 3 days, cooled to room temperature, filtered, washed, and dried to obtain a yellow block crystals with a yield of 27%.
Embodiment 3
[0021] Take 2-(4-pyridyl)-1H-imidazole-4,5-dicarboxylic acid (0.6mmol), potassium thiocyanate (1mmol) and MnCl 2 4H 2 O (1 mmol) was added to 7 ml of water, stirred for 20 minutes, then sealed in a 25 ml polytetrafluoroethylene reactor, kept at a constant temperature of 180°C for 3 days, cooled to room temperature, filtered, washed, and dried to obtain a yellow block crystals with a yield of 21%.
[0022] 1) Determination of crystal structure:
[0023] The above-prepared crystals were selected for structural analysis. At 296±2K on the BrukerApex-IICCD diffractometer, graphite monochromatized MoKα rays (λ=0.71073?), in the range of 2.35°<θ<25° Collect crystal diffraction point data, the crystal structure is solved by empirical method, the coordinates of all non-hydrogen atoms in the complex are corrected by the anisotropic temperature factor by the full matrix least square method, and the coordinates of all hydrogen atoms are found by the theoretical hydrogenation program . ...
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