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The syntheses and single crystal structures of five new tetracyanidoborate salts with N‐based cations are described. Three of these compounds contain cations with acidic H atoms. The H‐bond strength, expressed by D‐A distances is correlated with a shift of the CN stretching mode frequency in the IR spectra. Melting points are found between 59 °C and 214 °C, i. e. at the borderline between ionic liquids and molten salts. Isothermal annealing indicates slow decomposition. Solubility tests in polar solvents show a strong dependence on the cation.

A series of nine different known ionic liquids or low melting salts was synthesised and purified. They are composed of the [NTf2]– (bis(trifluoromethane)sulfonimide), [OTf]– (trifluoro‐methane‐sulfonate), or [B(CN)4]– (tetracyanidoborate) anion and [Ph4P]+ (tetraphenylphosphonium), [Ph3BzP]+ (triphenylbenzyl phosphonium), [nBu4P]+ (tetra‐nbutylphosphonium), [nBuPh3P]+ (tri‐phenyl‐nbutylphosphonium), [nBu4N]+ (tetra‐nbutylammonium), or the [PPN]+ (bis(triphenylphosphine)iminium) cation. Precise vapour pressure data and enthalpies of vaporisation were measured using the Quartz Crystal Microbalance (QCM) method and evaluated. Structure‐property relations are established using the obtained data as well as literature known data of ILs with alkyl‐substituted imidazolium cations. It turns out that ILs with the tetracyanidoborate anion have even higher values of the enthalpy of vaporisation than those with the common [NTf2]− or [OTf]− anion and therefore are even less volatile.

Novel silylated diols and polyols were prepared using a recently developed synthesis route with bifunctionalized silyl triflates. These silyl derivatives include two triflate functions, [a] 1302 Scheme 2. Preparation of the silyl-protected 1,2-cyclitols 12a-e. Reagents and conditions: a) TfOH, dichloromethane, -20°C, b) trans-cyclohexane-1,2-diol (7a) or cis-cyclohexane-1,2-diol (7b), Et 3 N, dichloromethane, -20°C to room temp.