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The reactivity of 2,6‐bis(diazaboryl)pyridine (dab2py) with the metal alkyls MeLi, Et2Zn and n‐Bu2Mg is reported. In all reactions, the alkylation of one boron atom of dab2py was observed to yield a new type of anionic pyridine ligand, which forms the respective adducts with [Li(OEt2)]+, [ZnEt]+ or [Mg(n‐Bu)]+. The alkylation of the boron atom results in a tetrahedral geometry, which allows for both amine nitrogen atoms to participate in the coordination. The products are highly soluble in all common solvents including alkanes. The reactivity is compared with the one already reported for unsubstituted pyridine, which is alkylated at the 2‐position by treatment with MeLi. The reaction of these metal alkyls with the popular terdentate 2,6‐diiminopyridine ligand (DIMPY) were previously reported to yield N‐alkylated anionic ligands, which subsequently undergo alkyl‐migration or deprotonation reactions. Single crystal XRD was performed on the products obtained from the reaction with MeLi and Et2Zn. Attempts to grow crystals for the respective magnesium alkyl complex in a dry ice box yielded a dinuclear complex bridged by two valerate groups instead. [ABSTRACT FROM AUTHOR]

In this work, we present our improved protocols for the single batch syntheses of approximately 32 g of [NHMe3][CB11H12] and 10 g of Na[CHB11F11] as well as salt metathesis reactions, granting access to useful starting materials to introduce the [CHB11F11]− anion. This includes the trityl cation [Ph3C]+ and the bis‐1,2‐difluorobenzene‐silver(I)‐complex [Ag(odfb)2]+, as well as some applications of the shown compounds. The described methodology allows the synthesis of large amounts of both the [CB11H12]− and the [CHB11F11]− anion and therefore making them accessible for further reactions. To facilitate the reproducibility, we present video tutorials of the synthetic steps towards Na[CHB11F11]. [ABSTRACT FROM AUTHOR]

The article in Chemistry - Methods discusses the synthesis of salts of the parent carbaborate ion [CB11H12]− and its undecafluorinated form [CHB11F11]−, along with useful starting materials. Ingo Krossing and co‐workers provide detailed synthetic protocols for the large-scale synthesis of these compounds, including instructive videos for reproducibility. The authors also explore the chemical properties of [CHB11F11]− and synthesize its trityl and silver salts for various reactions. More information can be found in the Research Article by I. Krossing and co‐workers. [Extracted from the article]