A kind of tetranuclear iron cluster compound and its synthesis method and application
A synthesis method and cluster compound technology are applied in the field of tetranuclear iron cluster compound and its synthesis, which can solve unseen problems and achieve the effects of low cost, good repeatability and simple synthesis method.
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Embodiment 1
[0031] Take ligand 2-methyl-8-hydroxyquinoline (0.063g, 0.4mmol) and FeCl 3 ·6H 2 O (0.027g, 0.1mmol) was placed in a Pyrex tube, 6mL of acetonitrile was added, and after stirring for 30 minutes, 2mL of methanol was added to mix well, and after stirring for 1 hour, 3 drops of triethylamine were added (the pH of the solution after stirring was 8.0), The Pyrex tube was evacuated and the other end was capped. Put the sealed Pyrex tube at 100°C for 72 hours, take it out, let it cool down to room temperature naturally, then filter the feed solution, and let the filtrate stand for natural volatilization. After 10 days, black blocky crystals are precipitated. Yield: 71%. Elemental analysis results: experimental value, C: 46.61%, H: 3.19%, N: 5.43%; theoretical value, C: 46.65%, H: 3.13%, N: 5.44%.
[0032] The product obtained in Example 1 is characterized:
[0033] 1) Crystal structure analysis:
[0034]The black bulk crystal with perfect surface structure is measured by Agilen...
Embodiment 2
[0052] Repeat Example 1, the difference is:
[0053] 1) FeCl 3 ·6H 2 The amount of O was changed to 0.02mmol, that is, 0.054g;
[0054] 2) Change the mixed solvent to consist of 1.5mL methanol and 3.0mL acetonitrile; and add acetonitrile and methanol in the mixed solvent to the Pyrex tube at the same time;
[0055] 3) Adjust the pH value of the solution to 7.5.
[0056] The Pyrex tube was taken out and naturally cooled to room temperature, the feed liquid was filtered, and the filtrate was left to evaporate naturally. After 15 days, black blocky crystals were precipitated at the bottom of the Pyrex tube. Yield 63%.
[0057] The obtained product was characterized by single crystal structure, and the product was determined to be the target product [Fe 4 (μ 2 -O) 2 Cl 4 (C 10 h 8 ON) 4 ]. Characterization of the magnetic properties of the product shows that the product obtained at room temperature χ M T is 6.75cm 3 Kmol -1 , much smaller than the theoretical value ...
Embodiment 3
[0059] Repeat Example 1, the difference is:
[0060] 1) Change the mixed solvent to consist of 1.5mL methanol and 1.5mL acetonitrile;
[0061] 2) adjust the pH value of the solution to 8.5;
[0062] 3) Change the reaction temperature to 60°C and the reaction time to 80h.
[0063] The Pyrex tube was taken out and naturally cooled to room temperature, the feed liquid was filtered, and the filtrate was left to evaporate naturally. After 15 days, black blocky crystals were precipitated at the bottom of the Pyrex tube. Yield 65%.
[0064] The obtained product was characterized by single crystal structure, and the product was determined to be the target product [Fe 4 (μ 2 -O) 2 Cl 4 (C 10 h 8 ON) 4 ]. Characterization of the magnetic properties of the product shows that the product obtained at room temperature χ M T is 6.75cm 3 Kmol -1 , much smaller than the theoretical value of four pure spin iron ions. With decreasing temperature, χ M The T value also decreases slo...
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