Synthesis and Structural Characterization of Monomeric and Dimeric Aluminum Amides

Abstract

The synthesis and structural characterization of a trialkylaluminum amine adduct, Me₃AlNH₂tBu (l), four dimeric aluminum primary amides, [Me₂AlNHⁱBu]₂ (2), [ⁱBu₂AlNHPh]₂(3), [ⁱBu₂AlNH(2,6-ⁱPr₂)Ph]₂ (4), [(Me₃Si)₂AlNHPh]₂ (5) and a monomeric aluminium amide, Mes₂AlN(SiMe₃)₂ (6) are reported. Compounds 2_5 contribute to the relatively small number of structurally characterized primary amido complexes of aluminium. Compound 6 is one of a few examples of a monomeric, three-coordinate dialk 1 aliminum amide. Crystal data: (1): Monoclinic, P2₁, a = 6.405(1), b = 10.742(1), c = 8.421(1)Å, β= 109.42(1)°, V = 546.41(12), Z = 2, with 671 refl. with F > 4.0 σF, R = 0.0451; (2): Monoclinic, P2₁/n, p = 6.798(1), b = 12.273(1), c = 10.900(1) Å β = 96.25(2)°, V = 904.0(2), Z = 4, with 867 refl. with F > 4.0 σF, R = 0.0568; (3): Triclinic, P-1, a = 9.393(1), b = 9.479(1), c = 10.891(1) Å, α = 67.22(1), β = 68.10(1), γ = 61.57(1)°, V = 764.66(13), Z = 2, with 1602 refl. with F > 4.0 σF, R = 0.0464; (4): Monoclinic, P2₁/n, a = 10.798(2), b = 19.375(2), c = 20.119(2) Å, β = 92.93(1)°, V = 4203.6(1), Z = 4, with 2316 refl. with F > 4.0 σF, R = 0.0723; (5): Triclinic, P-1, a = 8.823(2), b = 9.830(4), c = 11.498(4) Å, α = 105.16(3), β = 110.56(2), γ = 96.43(2)°, V = 878.7(5), Z = 2, with 1341 refl. with F > 4.0 σF, R = 0.0593; (6): T riclinic, P-1, a = 8.146(2), b = 12.798(2), c = 13.912(3) Å, α = 110.68(1), β = 94.71(1), γ = 91.71(1) °V= 1349.6(5), Z = 2, with 1730 refl. with F > 6.0 σF, R = 0.0593.