Крикун, С.С.Крикун0000-0001-8274-0608Левков, Ігор ВікторовичІгор ВікторовичЛевков0000-0002-1110-9023Єгорова, Тетяна ВолодимирівнаТетяна ВолодимирівнаЄгорова0000-0002-2408-6991Войтенко, Зоя ВсеволодівнаЗоя ВсеволодівнаВойтенко2026-03-312026-03-312018Крикун, С., Левков, І., Єгорова, Т., & Войтенко, З. (2018). Синтез окисненої форми дитієно-ТТФ методом електрокристалізації. Вісник київського національного університету імені Тараса Шевченка. Хімія, 1(55), 57-60. https://doi.org/10.17721/1728-2209.2018.1(55).14УДК 547.759.410.17721/1728-2209.2018.1(55).14https://ir.library.knu.ua/handle/15071834/13895General principles of the electrocrystallization technique in application to organic molecules are shown, as some historical background. Based on this, we were able to rationalize main variables in the experiment which are needed in order to get crystals of the oxidized form, that are suitable for further applications such as for example single crystal x-ray diffraction analysis or conductivity measurements. The biggest impact comes from such factors as choice of solvent and supporting electrolyte, which influence directly the solubility of both the starting compound and its oxidized form. Purity of all components is also paramount. In order to avoid formation of by-products, experiment is usually performed in a sealed U-shaped electrochemical cell with a glass filter between the anodic and cathodic compartments and under inert atmosphere such as argon or nitrogen. Other parameters considered here, such as temperature of the solution and intensity of the current, help to fine-tune the result, but have less impact on whether the crystallization will occur at all. It is also critical to maintain both parameters at constant values in order to obtain high quality single crystals. Galvanostatic oxidation mode is more favourable comparing to the potentiostatic as it allows steady rate of oxidation by providing fixed intensity of the electrical current and subsequently more stable rate of crystal grows, although potentiostatic mode or alternating current can be used to grow bigger amounts when quality of the single crystal is less important. Further we used this approach to electrocrystalize previously obtained by our group dithieno-TTF, based on the exTTF scaffold. According to the literature cyclic voltammetry data, dithieno-TTF undergoes reversible single-wave two electron oxidation to form bis-cation similar to classic exTTF, but in our case only radical-cation salt was obtained in a form of shiny, dark-red, needle-like single crystals. This could be attributed to its extremely low solubility and corresponding formation of the kinetic product, which correlate well with relatively fast crystallization just within 3 days. Another possibility is a comproportionation reaction involving the starting neutral molecule and oxidized dication.Показано ефективну методику для отримання кристалів окисненої форми, проаналізовано вплив розчинників, температури та електроліту, що підтримує на перебіг процесу. Показано, що сполука дитієно-ТТФ крис-талізується у формі солі катіон-радикала, на відміну від очікуваного дикатіона.ukелектрокристалізаціятетратіофульваленТТФelectrocrystallizationtetrathiafulvaleneTTFСтаття