146842-48-0Relevant articles and documents
Synthesis and characterization of the monomeric aluminum monoamides (t-Bu)2AlN(R)R′ (R and R′ = bulky aryl, alkyl, or silyl groups)
Petrie, Mark A.,Ruhlandt-Senge, Karin,Power, Philip P.
, p. 1135 - 1141 (2008/10/08)
The synthesis and characterization of the compounds (t-Bu)2AlNR2 (R = Mes, 1, and SiPh3, 2) and (t-Bu)2AlN(R′)SiPh3 (R′ = 2,6-i-Pr2C6H3 (Dipp), 3, and 1-adamantyl (1-Ad), 4) are described. They were characterized by X-ray crystallography and 1H NMR and IR spectroscopy. In the crystal phase, the structures of 1-4 are monomeric with essentially trigonal planar coordinations at aluminum and nitrogen and Al-N bond lengths that range from 1.82 to 1.89 ?. The variation in the Al-N bond lengths are a consequence of the steric interactions between the large groups at aluminum and nitrogen, different change separations across the Al-N bond, and, in some instances, weak Al-N π-bonding. The structural data together with VT 1H NMR studies of these and related compounds indicate that a decrease in the size of these groups affords considerably shorter Al-N distances and, in some cases, barriers to rotation around the Al-N bond that have a maximum value of ca. 9-10 kcal mol-1. The synthesis and characterization of [(t-Bu)2Al{N(H)CPh3}2(Li)], 5, are also described. Crystal data with Mo Kα (λ = 0.710 69 ?) at 130 K: 1, C26H40AlN, a = 9.965(3) ?, b = 13.746(5) ?, c = 17.700(6) ?, orthorhombic, space group Pca21, Z = 4, R = 0.069; 2, C44H48AlNSi2, a = 12.623(4) ?, b = 16.880(3) ?, c = 18.600(2) ?, α = 93.45(1)°, β = 100.25(2)°, γ = 99.46(2)°, triclinic, space group P1, Z = 4, R = 0.051; 3, C38H50AlNSi, a = 10.413(4) ?, b = 10.585(6) ?, c = 18.281(6) ?, α = 97.75(4)°, β = 96.41(3)°, γ = 118.97(2)°, triclinic, space group P1, Z = 2, R = 0.050; 4, C36H48AlNSi, a= 10.372(3) ?, b= 17.957(8) ?, c = 19.184(8) ?, α = 113.87(3)°, β = 99.23(3)°, γ = 96.71(3)°, triclinic, space group P1, Z = 4, R = 0.045; 5, C46H50AlLiN2, a = 37.78(2) ?, b = 10.635(4) ?, c = 19.237(7) ?, β = 98.19(3)°, monoclinic, space group C2/c, Z = 8, R = 0.056.
