NF3 and N(NO2)3 are known compounds, whereas the mixed fluoronitroamines, FN(NO2)2 and F2NNO2, have been unknown thus far. One of these, FN(NO2)2, has now been prepared and characterized by multinuclear NMR and Raman spectroscopy. FN(NO2)2 is the first known example of an inorganic fluoronitroamine. It is a thermally unstable, highly energetic material formed by the fluorination of the dinitramide anion using NF4(+) salts as the preferred fluorinating agent.
Oxalic acid forms in superacidic solutions HF/MF5 (M = As, Sb) its corresponding mono‐ and diprotonated salts [HOOCC(OH)2][MF6] and [(HO)2CC(OH)2][MF6]2 (M = As, Sb). The number of protonations is strongly dependent on the stoichiometric ratio of the Lewis acid with regard to oxalic acid. Mono‐ and diprotonated salts were characterized by vibrational spectroscopy and in the case of [HOOCC(OH)2][AsF6] (1) and [(HO)2CC(OH)2][SbF6]2 (4) by a single‐crystal X‐ray structure analysis. The salts crystallize in the monoclinic space groups P21/c and P21/n with eight, respectively four, formula units per unit cell. The vibrational spectra were compared to quantum chemical calculations of the cations [HOOCC(OH)2]+ and [(OH)2CC(OH)2]2+⋅4HF. In addition to this, an MEP analysis together with the NPA charges of [(OH)2CC(OH)2]2+, [(OH)2CC(OH)2]2+⋅6HF and oxalic acid were calculated to locate the positive charge. The protonation of oxalic acid does not lead to a remarkable change of the C‐C bond length, which is discussed for the entire series of the oxalic skeleton, starting with the dianion and ending with the tetrahydroxy dication.
The reactions of hydrogen cyanide, butyronitrile, cyclopropanecarbonitrile, pivalonitrile and benzonitrile with arsenic pentafluoride and antimony pentafluoride result in the formation of 1 : 1 Lewis adducts, while malononitrile yielded both 1 : 1 and 1 : 2 Lewis adducts.
The thermally unstable, primary perfluoroalcohols, CF OH, C F OH, and nC F OH, were conveniently prepared from the corresponding carbonyl compounds in anhydrous HF solution. Experimental values for the reaction enthalpies and entropies were derived from the temperature dependence of the R COF+HF⇄R CF OH (R =F, CF , CF CF ) equilibria by NMR spectroscopy. Electronic structure calculations of the gas-phase and solution reaction energies, gas-phase acidities and heats of formation were carried out at the G3MP2 level, showing that these compounds are strong acids. Protonation of these alcohols in HF/SbF produced the perfluoroalkyl oxonium salts R CF OH SbF .
We show that a new terpyridine ligand comprising a directly-connected methyldisulfide group (tpySSMe) can be used to prepare a modular series of metal bis(terpyidine) complexes, [M(tpySSMe)2](PF6)2 (M = Fe, Co,...
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