Journal
CHEMISTRY-A EUROPEAN JOURNAL
Volume 22, Issue 42, Pages 14968-14978Publisher
WILEY-V C H VERLAG GMBH
DOI: 10.1002/chem.201602683
Keywords
alkali metals; amides; bases; magnesiates; metalation; structure elucidation
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Funding
- UK Engineering and Physical Science Research Council [EP/K001183/ 1]
- Royal Society
- Engineering and Physical Sciences Research Council [EP/L001497/1, EP/J001872/1, EP/K001183/1] Funding Source: researchfish
- EPSRC [EP/L001497/1, EP/J001872/1, EP/K001183/1] Funding Source: UKRI
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Bulky amido ligands are precious in s-block chemistry, since they can implant complementary strong basic and weak nucleophilic properties within compounds. Recent work has shown the pivotal importance of the base structure with enhancement of basicity and extraordinary regioselectivities possible for cyclic alkali metal magnesiates containing mixed n-butyl/amido ligand sets. This work advances alkali metal and alkali metal magnesiate chemistry of the bulky arylsilyl amido ligand [N(SiMe3)(Dipp)](-) (Dipp= 2,6-iPr(2)-C6H3). Infinite chain structures of the parent sodium and potassium amides are disclosed, adding to the few known crystallographically characterised unsolvated s-block metal amides. Solvation by N, N, N', N '', N ''-pentamethyldiethylenetriamine (PMDETA) or N, N, N', N'-tetramethylethylenediamine (TMEDA) gives molecular variants of the lithium and sodium amides; whereas for potassium, PMDETA gives a molecular structure, TMEDA affords a novel, hemi-solvated infinite chain. Crystal structures of the first magnesiate examples of this amide in [MMg{N(SiMe3)(Dipp)}(2)(mu-nBu)](infinity) (M= Na or K) are also revealed, though these breakdown to their homometallic components in donor solvents as revealed through NMR and DOSY studies.
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