Inorganic Chemistry, Vol.36, No.9, 1955-1960, 1997
Substitution-Reactions of Aluminum Organoamide Complexes (Al(Mu-Nr2)(N)Cl3-N)(2) (R=et, Pr-I N-Less-Than-or-Equal-to-3) with Linr’r" (R’=r"=pr-I, Et - R’=h, R"=pr-I) - Crystal-Structure of (Al(Mu-Net2)((Npr2)-Pr-I)X)(2) (X=cl,H) and AlCl3((Nprh2)-Pr-I)(2)(Al(NH3)(NH2)(Al((Nprh)-Pr-I)((NPR)-Pr-I)Cl)(2))(2)
As part of our ongoing study of different substituents of Al2N2 ring systems, the synthesis, structural characterization, and spectroscopic studies on several amido derivatives of four-coordinated aluminum are described. The compounds Al-2(NEt2)(2)((NPr2)-Pr-i)(2)Cl-2, 1, Al-2(((NPr2)-Pr-i)(4)Cl-2, 2, Al(((NPr2)-Pr-i)(3), 3, Al(NEt2)(3), 4, {Al((NPrH)-Pr-i)(3)}(3), 5, Al-2(NEt2)(2)((NPr2)-Pr-i)(2)H-2, 6, and AlCl3((NPrH2)-Pr-i)(2){Al(NH3)(NH2)[Al((NPrH)-Pr-i)((NPr)-Pr-i)Cl](2)}(2), 7, were synthesized by substitution reactions and characterized by mass spectra, IR spectra, elemental analysis, and H-1, C-13, and Al-27 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 K alpha (1 and 7, lambda = 0.710 73 Angstrom) or Cu K alpha (6, lambda = 1.541 78 Angstrom) radiation : (1) Al2N4C20H48Cl2, a = 7.747(2) Angstrom, b = 9.648(2) Angstrom, c = 10.110(3) Angstrom, alpha = 102.91(2)degrees, beta = 83.54(2)degrees, gamma = 110.19(2)degrees, triclinic, space group P (1) over bar, Z = 1, R = 0.053 for 1789 (I > 3 sigma(I)) reflections; (6) Al2N4C20H50, a = 15.088(2) Angstrom, b = 14.506(3) Angstrom, c = 12.439(3) Angstrom, orthorhombic, space group Cmca (No. 64), Z = 4, R = 0.045 for 701 (I > 3 sigma(I)) reflections; (7) Al7N14C30H86Cl7, a = 29.914(9) Angstrom, b = 10.197(3) Angstrom, c = 20.525(5) Angstrom, beta = 90.99(4)degrees, monoclinic, space group C2/c, Z = 4, R = 0.042 for 2472 (I > 2 sigma(I)) reflections.