A new organic superconductor β-(meso-DMBEDT-TTF)2PF6

Shinya Kimura, Tomoko Maejima, Hideaki Suzuki, Ryoma Chiba, Hatsumi Mori, Tadashi Kawamoto, Takehiko Mori, Hiroshi Moriyama, Yutaka Nishio, Koji Kajita
2004 Chemical Communications  
General information. The reactions in scheme 1 and electrochemical crystallizations were carried out under a dry nitrogen atmosphere. Triethyl phosphite was distilled under reduced pressure in the presence of sodium and THF was freshly distilled under nitrogen over sodium and benzophenone. Chlorobenzene was washed with conc. H 2 SO 4 then with aq. NaHCO 3 and water, followed by drying with CaCl 2 , and distilled under nitrogen. Melting points were determined with a Yanaco MP micro melting point
more » ... apparatus. NMR spectra were obtained with a JEOL JNM-AL300 spectrometer. IR spectra were recorded on a HORIBA FT-730 spectrometer, and mass spectra on a JEOL JMS-AX500 spectrometer. Microanalyses were performed at Microanalytical Laboratory, The University of Tokyo. [1,4]dithiin-2-thione 3 (0.50 g, 2.0 mmol) and 4,5-bis(2-cyanoethylthio)-1,3-dithiol-2-one 4 (0.57 g, 2.0 mmol) in triethyl phosphate (6 cm 3 ) were heated at 110 °C under nitrogen for 3 h. After the mixture was cooled to room temperature, the solvent was removed in vacuo. The residue was purified by column chromatography (silica gel, dichloromethane-hexane) to afford 5 (0.54 g, 55%) as an orange solid. mp 109-111 o C; 1 H NMR (300 MHz, CDCl 3 ): δ = 1.39 (6H, d, J = 6.7 Hz), 2.73 (4H, t, J = 7.1 Hz), 3.08 (4H, t, J = 7.1 Hz), 3.60 (2H, m); MS 385 (M + -2CH 2 CH 2 CN); ν max /cm - meso-2-(4,5-Bis(2-cyanoethylthio)-1,3-dithiol-2-ylidene)-5,6-dihydro-5,6-dimethyl-1,3 -dithiolo[4,5-b][1,4]dithiin (5). meso
doi:10.1039/b409631b pmid:15514812 fatcat:nexn4ytllrczzplfickd5dd64q