Photochromic ligand, Re (I) rectangular supramolecular complex, preparation method and application thereof
A photochromic and complex technology, which is applied in the fields of color-changing fluorescent materials, chemical instruments and methods, compounds of Group 7/17 elements of the periodic table, etc., can solve the problems of no ultraviolet photochromic properties, no optical properties, etc., To achieve the effect of easy separation and purification, simple operation
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[0047] The third embodiment of the present invention provides a Re(I) rectangular supramolecular complex, the chemical structure of which is shown in 1.
[0048]
[0049] Experiments show that the Re(I) rectangular supramolecular complex formed by the above photochromic ligand still has the photochromic properties under ultraviolet irradiation.
[0050] In one or more examples of this embodiment, the single crystal molecular formula of the Re(I) rectangular supramolecular complex is: C 40 H 22 Cl 4 N 2 O 6 Re 2 S 2 , The chemical formula is [Re 2 (CO) 6 (C 34 H 22 Cl 2 N 2 S 2 )(μ 2 -Cl) 2 , Crystalline in the monoclinic system, belongs to the C2 / m space group.
[0051] In this series of embodiments, the single crystal contains four Re (I) centers with the same environment, the entire molecule is a rectangular frame, the metal Re (I) centers are located at 4 vertices, and the two short sides are respectively composed of 4 μ 2 -Chlorine bridged, the two long sides are respectively comp...
Embodiment 1
[0061] 1. Preparation of photochromic ligand L
[0062] The preparation of intermediates S1 and S2 follows the literature method.
[0063] Preparation of intermediate S3
[0064] Intermediate S2 (4.0g, 10mmol) was dissolved in thionyl chloride (25ml, 95.2g, 0.8mol) and heated to reflux for 4 hours. This reaction should be equipped with a drying tube to prevent moisture from entering the reaction system. After the reaction was completed, the unreacted thionyl chloride was distilled off, and then a dichloromethane solution (30ml) dissolved in 2-chloro-5-methylthiophene (2.3ml, 21mmol) was added. The reaction solution was cooled to 0°C with an ice water bath, and 3.3 g of anhydrous aluminum trichloride (25 mmol) was added in several portions. Stirring was continued at 0°C for 30 min, then warmed to room temperature and stirring continued overnight. After the reaction is over, ice water is added to the reaction system to remove excess aluminum trichloride. The organic phase was separ...
Embodiment 2
[0080] The ligand L prepared in Example 1 was dissolved in methanol to prepare a concentration of 1.65×10 -5 M methanol solution, under 298K, using 313nm ultraviolet light, the methanol solution before and after the light is measured by ultraviolet-visible absorption spectrum and fluorescence emission spectrum, the results are as follows Figure 7 As shown in the left picture, before and after illumination, the absorption wavelength of ligand L has a red shift, and a new absorption band appears in the visible range of 500-600nm, which is consistent with the color change of the solution before and after illumination. As shown in the right figure, the fluorescence emission spectrum of ligand L is quenched by ultraviolet light. It shows that the structure of ligand L has changed before and after UV irradiation, and the open loop state changes to the closed loop state.
[0081] The Re(I) rectangular supramolecular complex solution DMF prepared in Example 1 was prepared into a DMF solu...
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