ANIONIC AND NEUTRAL ALUMINUM BIS(N,N'-DI-TERT-BUTYLETHYLENEDIAMIDE) COMPLEXES - [AL([N(T-BU)CH2](2))(2)](-) AND [AL([N(T-BU)CH2](2))(2)]

Citation
Mg. Gardiner et al., ANIONIC AND NEUTRAL ALUMINUM BIS(N,N'-DI-TERT-BUTYLETHYLENEDIAMIDE) COMPLEXES - [AL([N(T-BU)CH2](2))(2)](-) AND [AL([N(T-BU)CH2](2))(2)], Inorganic chemistry, 36(13), 1997, pp. 2795-2803
Citations number
37
Categorie Soggetti
Chemistry Inorganic & Nuclear
Journal title
ISSN journal
00201669
Volume
36
Issue
13
Year of publication
1997
Pages
2795 - 2803
Database
ISI
SICI code
0020-1669(1997)36:13<2795:AANABC>2.0.ZU;2-G
Abstract
The reaction of the aluminum triamide [{HN(t-Bu)CH2CH2N-t-Bu)Al(N(t-Bu )CH2)(2)] (1) with n-BuLi in hexane and diethyl ether gives the monome ric solvent-free lithium aluminum tetraamide [Li(N(t-Bu)CH2CH2N-t-Bu)( 2)Al] (2), and the diethyl ether adduct [Et2O . Li(N(t-Bu)CH2CH2N-t-Bu )(2)Al] (3), respectively. The reaction of the diethyl ether adduct 3 with 2 equiv of the chelating nitrogen Lewis bases TMEDA (=N,N,N',N'-t etramethylethylenediamine) and t-Bu(2)DAB (=N,N'-di-tert-butyl-1,4-dia zabutadiene) in diethyl ether affords the ionic complex [Li(TMEDA)(2)] [Al{[N(t-Bu)CH2](2)}(2)] (4) and a mixture of;the paramagnetic species [Li(t-BuDAB)(2)] and [Al ([N(t-Bu)CH2](2)}(2)], which cocrystallize 5 , respectively. The reaction of the diethyl ether adduct 3 with 0.5 eq uiv of HgCl2 yields the neutral paramagnetic species [AI([N(t-Bu)CH2]( 2)}(2)] (6). Crystals of 2 are triclinic, of space group <P(1)over bar > (No. 2), with a = 15.894(5) Angstrom, b = 15.473(5) Angstrom, c = 9. 975(3) Angstrom, a 93.74(2)degrees, beta = 91.97(2)degrees, gamma = 10 2.07(3)degrees, and Z = 4. Crystals of 3 are monoclinic, of space grou p C2/c (No. 15), with a = 15.835(5) Angstrom, b = 12.054(3) Angstrom, c = 16.456(5) Angstrom, beta = 111.56(3)degrees, and Z = 4. Crystals o f 4 are orthorhombic, of space group Pbca (No. 61), with a = 19.349(4) Angstrom, b = 22.227(7) Angstrom, c = 19070(3) Angstrom, and Z = 8. C rystals of 5 are orthorhombic, of space group Pmmn (No. 59), with a = 13.874(4) Angstrom, b = 13.473(6) Angstrom, c = 12.717(3) Angstrom, an d Z = 2. Crystals of 6 are monoclinic, of space group C2/c (No. 15), w ith a = 16.721(4) Angstrom, b = 9.454(4) Angstrom, c 16.460(8) Angstro m, beta = 113.27(3), and Z = 4.