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Ion pairs of 1,10-phenanthrolin-5,6-dione radical anion [M ·  ⊖ Me ⊕n ] · ⊕(n−1)  with Me ⊕n  = Mg ⊕⊕ , Ca ⊕⊕ , Sr ⊕⊕ , Zn ⊕⊕ , Cd ⊕⊕ , Pb ⊕⊕  and La ⊕⊕⊕  are advantageously prepared in aprotic DMF solution containing appropriate metal salts Me ⊕n X ⊖  by using the ‘mild’ single-electron reducing agent tetra(n-butyl)ammonium-boranate R 4 N ⊕ BH 4  ⊖  . For comparison, the ‘naked’ radical anion with the largely interaction-free [K ⊕ (2.2.2)-cryptand] ⊕  counter cation is chosen, which is formed on reduction with potassium in THF solution of (2.2.2)-cryptand. Addition of excess Na ⊕ [B(C 6 H 5 ) 4 ] ⊖  to the reduction solution only yields a solvent-separated ion pair (M ·  ⊖ )DMF ··· (Na ⊕ )DMF, whereas in the presence of multiply charged counter cations Me ⊕n  the respective contact ion pair radical cations [M ·  ⊖ Me ⊕n ] ·  ⊕(n−1)  are formed. Their g values decrease with increasing nuclear charge of Me ⊕n  and their metal-s-spin densities increase with the effective counter cation charge n ⊕ /r Me ⊕n. The ESR /ENDOR data recorded suggest Me ⊕n  complexation by the  δ⊖ OC -CO δ⊖  chelate tongs and the ion pair stability, which is modified by the dielectric properties of the solvent used, may be rationalized by the Coulombic attraction between the radical anion M ·  ⊖  and the counter cations Me ⊕n .

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Elektronentransfer und Ionenpaar-Bildung, 27 [1, 2] Darstellung von Semichinon-Ionenpaaren durch Reduktion von Chinonen mit Tetraalkylammonium-boranat in aprotischen Lösungen: 1,10-Phenanthrolin-5,6-dion / Electron Transfer and Ion Pairing, 27 [1, 2] Preparation of Semiquinone Ion Pairs by Reduction of Quinones Using Tetraalkylammonium Boranate in Aprotic Salt Solutions: 1,10-Phenanthrolin-5,6-dione