Di-μ-chlorobis[(1,2,5,6-η)-1,5-cyclooctadiene]diiridium
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![Di-μ-chlorobis[(1,2,5,6-η)-1,5-cyclooctadiene]diiridium structure](https://file.echemi.com/fileManage/upload/canonicalSmiles/20220812/081be16fa8a241efa20bf029cb6467f4.png "Di-μ-chlorobis[(1,2,5,6-η)-1,5-cyclooctadiene]diiridium")
Di-μ-chlorobis[(1,2,5,6-η)-1,5-cyclooctadiene]diiridium
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CAS No:
12112-67-3
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Formula:
C16H24Cl2Ir2
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Chemical Name:
Di-μ-chlorobis[(1,2,5,6-η)-1,5-cyclooctadiene]diiridium
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Synonyms:
Iridium,di-μ-chlorobis[(1,2,5,6-η)-1,5-cyclooctadiene]di-;Iridium,di-μ-chlorobis(1,5-cyclooctadiene)di-;Iridium,dichlorobis(cyclooctadiene)di-;1,5-Cyclooctadiene,iridium complex;Di-μ-chlorobis[(1,2,5,6-η)-1,5-cyclooctadiene]diiridium;Di-μ-Chlorobis(π-1,5-cyclooctadiene)diiridium;μ,μ-Dichlorobis(1,5-cyclooctadiene)diiridium;Di-μ-Chlorobis(1,5-cyclooctadiene)diiridium;Dichlorobis(cyclooctadiene)diiridium;Chloro(1,5-cyclooctadiene)iridium dimer;5-Chlorobis(1,5-cyclooctadiene)diiridium;Dichlorobis(1,5-cyclooctadiene)diiridium;Cyclooctadieneiridium chloride dimer;(1,5-Cyclooctadiene)iridium chloride dimer;Dichlorobis(η4-1,5-cyclooctadiene)diiridium;(1,5-Cyclooctadiene)chloroiridium dimer;Bis(chloro(1,5-cyclooctadiene)iridium);Di-μ-chlorobis(η4-1,5-cyclooctadiene)diiridium;Bis(μ-chloro)bis(1,5-cyclooctadiene)diiridium;Bis((μ-chloro)(1,5-cyclooctadiene)iridium);(η4-1,5-Cyclooctadiene)iridium chloride dimer;Di-μ-chlorobis(η4-1,5-cyclooctadiene)diiridium(I);Chloro(cyclooctadiene)iridium dimer;Bis(chloro(cyclooctadiene)iridium);NSC 326162;Di-μ2-chlorobis(1,5-cyclooctadiene)diiridium;Bis(1,5-cyclooctadiene)diiridium(I) dichloride;Di-μ-chlorobis[(1,5-cyclooctadiene)iridium];Bis[μ-chloro(η4-1,5-cyclooctadiene)iridium];69004-75-7
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CAS No:
Di-μ-chlorobis[(1,2,5,6-η)-1,5-cyclooctadiene]diiridium Basic Attributes
671.7
672.051331
235-170-1
28439000
Characteristics
6.72460
red to orange Powder
200-202 °C
153.5ºC at 760 mmHg
31.7ºC
insoluble
2-8°C
4.25mmHg at 25°C
Di-μ-chlorobis[(1,2,5,6-η)-1,5-cyclooctadiene]diiridium Use and Manufacturing
At room temperature (25 ° C)The lg content of 98percent of iridium chloride monohydrate (3. lmmol) and 5 g of deoxygenated water (obtained by bubbling argon lOmin) were charged into a reaction vessel filled with argon, The argon was replaced three times under reduced pressure and the temperature was raised to 80 ° C, 1.38 g of an aqueous acetaldehyde solution (acetaldehyde 12.5 mmol) having a mass content of 40percent1.4 g of 1, 5-cyclooctadiene (12.7 mm) in a mass of 98percent, refluxed at 80 ° C for 6 h, the resulting mixture was cooled to room temperature and transferred to an ice-water bath (0 ° C ) Lh, followed by suction (2 ° C), washed with water (lg water, lg cold methanol) and dried (room temperature 25 ° C, 6 h) to give 0.77 g of a red solid. The yield was 74percent.The red solid was analyzed by NMR and the melting point of the red solid was determined. The solid is 1, 5-cyclooctadiene Iridium chloride dimer, and the 1H-NMR spectrum of the prepared 1, 5-cyclooctadiene Iridium chloride dimer is shown in Fig. Shows the 13C-NMR spectrum of the prepared 1, 5-cyclooctadiene chloride iridium dimerAt room temperature (25 ° C), lgMass content of 98percentIridium tetrachloride monohydrate(2. Smmol) and 7 g of deoxygenated water (obtained by bubbling in argon) were charged into argon-filled reaction vials and argon was purged three times under reduced pressure. The temperature was raised to 75 ° C and 0.918 mass of 98percent (8.S.), 0.978 mass of 98percent 1, 5-cyclooctadiene (8. Smmol), refluxed at 75 ° C for 8 h, the resulting mixture was cooled to room temperature, Transfer to ice water (0 ° C) lh, followed by suction (2 ° C), water (lg water, lg cold methanol leaching) and drying (room temperature) to give red solid . The yield was 78percent. The red solid was analyzed by NMR and the melting point of the red solid was determined.The solid was determined to be 1, 5-cyclooctadiene chloride iridium dimer.Weigh 7.5g (21.3mmol) iridium trichloride hydrate, and add into a 500 ml three-necked flask. Repeatedly pumping the vacuum nitrogen, to ensure that high-purity nitrogen atmosphere. Use injector to measure successively taking 150 ml anhydrous ethanol, 3.93 ml 1, 5-cyclooctadiene (COD) and add it into the reactor. Stirring at room temperature condition the solid dissolves. Afterwards, the reactor is transferred to the oil bath pan, adjusting the reaction temperature to 130 °C, and keep the reaction temperature heating reflux reaction, the color of the solution in the reaction process by the dark brown gradually into a brick red, in the reaction process has the red crystal in the inner wall of the flask, After reacting for 4 hours, stop the reaction, natural cooling to room temperature, oxygen-free under the operation of filtering the reaction solution, then the injector for each injection 105 ml ice-cold absolute ethanol and washing the bottle for solid, repeating the above-mentioned washing process 3 times will be red solid after vacuum drying, weighing 6.85g, yield 95.8percent.A 100 mL two-necked round-bottomed flask was charged with 2.0g (5.67 mmol) of hydrated iridium trichloride(IrCl3.3H2O), 34.0 mL of ethyl alcohol, 17.0 mL of water and 6.0 mL of cyclooctadiene. A slow stream of nitrogenwas passed through the system, and the solution is stirred well at room temperature for a few minutes by means ofmagnetic stirring bar. The solution was refluxed at 100oC for 24 h. During this time it changes from dark red to yellowand iridium(I)-catalyst precipitates from the solution. The mixture was allowed to cool to room temperature and[Ir(cyclooctadiene)Cl]2 was collected quickly by filtration and washed quickly with ice-cold methanol to remove thelast traces of unreacted cyclooctene. After drying in vacuum at room temperature for 4 h, the yield of C was 33.4percent(668.1 mg). mp: >200 oC (decomp.).
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Di-μ-chlorobis[(1,2,5,6-η)-1,5-cyclooctadiene]diiridium
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