Crystal structure of (2,6-diisopropyl-phenyl)-(6-(2,6-dimethyl-phenyl)-pyridin-2-yl)-amine-(2,6-diisopropyl-phenyl)-(6-(2,6-dimethyl-phenyl)- pyridin-2-yl)-amido-lithium, Li(C25H29N2)(C25H30N2)

Andrea Espiga Ayuso, Awal Noor, Torsten Irrgang, Germund Glatz, Rhett Kempe
2007 Zeitschrift für Kristallographie - New Crystal Structures  
C 50 H 59 LiN 4 ,monoclinic, P 12 1 / n 1(no. 14), a =10.7120(8) Å, b =19.470(2) Å, c =20.681(2) Å, b =94.178(7)°, V =4301.8 Å 3 , Z =4, R gt (F) =0.065, wR ref (F 2 ) =0.115, T =173 K. Source of material Toastirredy ellow solution of 0.474 g( 0.54 mmol) Ap 2 ZrCl 2 [1] (Ap=( 2,6-diisopropyl-phenyl)-(6-(2,6-dimethyl-phenyl)pyridin-2-yl)-amine)i n1 0m Lhexane wasadded 0.68 mL (1.08 mmol) of CH 3 Li(1.6 Min diethylether) at0°C.The mixture wasallowed to warm up to room temperature and wasstirred
more » ... re and wasstirred overnight. The resulting brown solutionwasfiltered and hexane wase vaporated completely. The solid materiall eft behind was dissolved in 10 mLof toluene and 0.086 mL(0.54 mmol) of 4tert-butylaniline wasadded atr oom temperature.The solution mixture washeated at130°Cfor 3days. After cooling to room temperature volume of the solvent wasreduced to ca.2mLand wasl ayered with pentane. Colorless crystals of the title compound were obtained overnight at-25°C. Experimental details The Hatom bonded to the Natom waslocated and refined due to its importance in the hydrogen bonding pattern. Other Hatoms were included atcalculated positions. Discussion The title compound, amonomeric three-coordinated lithium aminopyridinate, is anew member of the lithium amides of sterically demanding aminopyridines which we reported recently [2]. One ligand is deprotonated and coordinates the lithium atom by the N pyridine and N amido atoms. The small chelating angle of N1-Li-N2( 70.0(2)°) underlines the strained nature of the aminopyridinato coordination. The second,p rotonated ligand coordinates the lithium by the N pyridine atom ( d (N3-Li1) = 1.983(6) Å). The coordination of the lithium ion is approximately trigonal-planar(sum of angles=339.6°) with adeviation of Liout of the N1-N2-N3plane of 0.42 Å.The bond lengths for N1-Li1 (1.958(6) Å)and N2-Li1 (1.999(6) Å)are nearly equaland indicate adelocalized bonding mode. The amino Ha tom forms ani ntramolecularh ydrogen bond to the adjacent amido atom ( d (H4···N2) =2.058 Å).
doi:10.1524/ncrs.2007.0119 fatcat:3d2vd22lqvckvefpniazbdvimq