Substitution Reactions of Aluminum Organoamide Complexes [Al(&mgr;-NR(2))(n)Cl(3-n)](2) (R = Et, (i)Pr; n </= 3) with LiNR'R" (R' = R" = (i)Pr, Et; R' = H, R" = (i)Pr): Crystal Structure of [Al(&mgr;-NEt(2))(N(i)Pr(2))X](2) (X = Cl, H) and AlCl(3)(N(i)PrH(2))(2){Al(NH(3))(NH(2))[Al(N(i)PrH)(N(i)Pr)Cl](2)}(2).
As part of our ongoing study of different substituents of Al(2)N(2) ring systems, the synthesis, structural characterization, and spectroscopic studies on several amido derivatives of four-coordinated aluminum are described. The compounds Al(2)(NEt(2))(2)(N(i)Pr(2))(2)Cl(2), 1, Al(2)((N(i)Pr(2))(4)Cl(2), 2, Al((N(i)Pr(2))(3), 3, Al(NEt(2))(3), 4, {Al(N(i)PrH)(3)}(3), 5, Al(2)(NEt(2))(2)(N(i)Pr(2))(2)H(2), 6, and AlCl(3)(N(i)PrH(2))(2){Al(NH(3))(NH(2))[Al(N(i)PrH)(N(i)Pr)Cl](2)}(2), 7, were synthesized by substitution reactions and characterized by mass spectra, IR spectra, elemental analysis, and (1)H, (13)C, and (27)Al NMR data. The structures of three compounds, viz., 1, 6, and 7, have been determined by single-crystal X-ray diffraction analysis. Crystal data with Mo Kalpha (1 and 7, lambda = 0.710 73 Å) or Cu Kalpha (6, lambda = 1.541 78 Å) radiation: (1) Al(2)N(4)C(20)H(48)Cl(2), a = 7.747(2) Å, b = 9.648(2) Å, c = 10.110(3) Å, alpha = 102.91(2) degrees, beta = 83.54(2) degrees, gamma = 110.19(2) degrees, triclinic, space group P&onemacr;, Z = 1, R = 0.053 for 1789 (I > 3sigma(I)) reflections; (6) Al(2)N(4)C(20)H(50), a = 15.088(2) Å, b = 14.506(3) Å, c = 12.439(3) Å, orthorhombic, space group Cmca (No. 64), Z = 4, R = 0.045 for 701 (I > 3sigma(I)) reflections; (7) Al(7)N(14)C(30)H(86)Cl(7), a = 29.914(9) Å, b = 10.197(3) Å, c = 20.525(5) Å, beta = 90.99(4) degrees, monoclinic, space group C2/c, Z = 4, R = 0.042 for 2472 (I > 2sigma(I)) reflections.
Chang
Chung-Cheng
CC
Department of Chemistry, National Sun Yat-Sen University, Kaohsiung, Taiwan, ROC, and Department of Chemistry, National Taiwan University, Taipei, Taiwan, ROC.
Li
Mung-Dar
MD
Chiang
Michael Y.
MY
Peng
Shie-Ming
SM
Wang
Yu
Y
Lee
Gene-Hsiang
GH