| Summary: | Novel hexafluoroisopropylboranes (CF<sub>3</sub>)(CF<sub>2</sub>H)CFBH<sub>2</sub>·<i>L</i> and -borate anions [(CF<sub>3</sub>)(CF<sub>2</sub>H)CFBH<sub>2</sub><i>X</i>]<sup>−</sup> with Lewis basic heterocyclic ligands <i>L</i> and the anionic substituents <i>X</i> = F<sup>−</sup> and CN<sup>−</sup> were obtained. The syntheses were accomplished by substitution reactions of the dimethyl sulfide adduct (CF<sub>3</sub>)(CF<sub>2</sub>H)CFBH<sub>2</sub>·SMe<sub>2</sub>, which was synthesized on a large scale. The hexafluoroisopropylboranes and -borates were characterized by NMR and vibrational spectroscopy, elemental analysis, and single-crystal X-ray diffraction. In addition, the thermal and electrochemical stabilities were investigated by DSC measurements and cyclic voltammetry and selected experimental data and trends are compared with theoretical ones.
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