Crystal structure of 1,1′-(pentane-1,5-diyl)bis(3-methyl-1H-imidazol-3-ium)bis(hexafluorophosphate), C₁₃H₂₂F₁₂N₄P₂

Abstract

CCDC no.: 1841197The crystal structure is shown in the figure. Tables 1 and 2 contain details on crystal structure and measurement conditions and a list of the atoms including atomic coordinates and displacement parameters. Source of materials 1-Methylimidazole (8.21 g, 0.1 mol) was dissolved in methylbenzene (20 mL), 1,5-dibromopentane (11.35 g, 0.05 mol) was quickly added under stirring. The mixture first reacted at 90°C for 10 min, and then heated to 110°C for 7-10 hours. After the reaction has completed (monitored by TLC), a white solid was produced. The resulting suspension was filtered, crushed and washed with hexane, ethylacetate and diethyl ether three times respectively. Then the intermediate (C5M-Br)(0.5 g, 0.00127 mol), potassium hexafluorophosphate (0.6 g, 0.0029 mol) was dissolved in deionized water (20 mL). The mixture stirred well for 12 h at 85°C and then cooled slowly. Colorless crystals were produced and filtered. They were washed with deionized water many times until silver bromide precipitation occurs anymore. The product (0.1 g) was dissolved in ethanol: water (2:1) solution and (7 mL), then the mixture reacted in the microwave synthesizer at 100°C for 2 min. Crystals suitable for X-ray analysis were obtained after cooled slowly.