The crystalline lithium primary amide derived from tertbutylamine, [ [ ButN(H)Li), 1, is structurally characterised by an X-ray diffraction study and shown to be a novel octameric (n = 8) ladder conformation, the cyclic, 'double-crown' nature of which implies molecules of this design could direct the synthesis of heterobimetallic (i.e. lithium and another metal) imide cage constructions.
Abstract. K[C6HIsNSi2].CvHs, Mr=291.62, monoclinic, C2/c, a= 13.213 (5), b= 17.077 (4), c= 15.796 (4) A, fl= 95.66 (2) °, V= 3546.8 (1.2) A 3, Z =8, D x= l.09gcm -3, 2(MoKa)=0.71069A, /t= 4.08 cm -1, F(000) = 1264, T,,,173 K. Final R = 0.045 for 2062 unique observed reflections. The compound was found to be a dimeric aggregate, the core of which consists of a nearly planar K--N-K--N four-membered ring. The crystallization solvent, toluene, co-crystallizes with the dimer but is not coordinated. Bond lengths and angles are in agreement with those of the monomeric dioxane-solvated compound.
[reaction: see text] Three different N-silyl-protected allylamines, i.e., N-TMS, N-TBDMS, and N-TIPS allylamine, were lihtiated by reaction with excess n-butyllithium. Crystallization of the resulting dianions and X-ray structure determination yields three uniquely different aggregates.
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