Synthesis and Crystal and Molecular Structures of the N,N-Dimethylethanol-aminogallane and N,N-Dimethylethanolaminogallium Dimethyl Dimers

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Abstract
Crystals of the N,N-dimethylethanolaminogallane dimer 1a are monoclinic, a = 8.540(1), b = 7.0433(7), c = 12.227(6) Å, β = 92.94(3)°, Z = 2, space group P21/c and crystals of the N,N-dimethylethanolaminogallium dimethyl dimer 1b are orthorhombic, a = 15.608(3), b = 11.655(2), c = 10.266(2) Å, Z = 4, space group Pccn. Both structures were determined by Patterson and Fourier syntheses and were refined by full-matrix least-squares procedures to final R values of 0.039 and 0.053 for 1062 and 1155 reflections with 1 ≥ 3σ(I) respectively. Both structures feature well-separated centrosymmetric dimeric units occurring via the formation of four-membered Ga2O2 rings. The five-coordinate gallium atoms have distorted trigonal bipyramidal geometry. Steric interactions between methyl groups in 1b are believed responsible for the lengthening of the axial Ga—N distance from 2.279(3) in 1a to 2.471(4) Å in 1b. Other bond distances are: for 1a; Ga—O (axial), 2.053(3), Ga—O, 1.911(3), Ga—H, 1.50(7) and 1.73(5), O—C, 1.369(5), N—C, 1.466 – 1.485(6), C—C, 1.512(7), and mean C—H, 1.05; for 1b; Ga—O (axial), 2.078(3), Ga—O, 1.913(3), Ga—C, 1.936(6) and 1.948(7), O—C, 1.382(7), N—C, 1.452–1.482(7−8), C—C, 1.516(9), and mean C—H, 1.01 Å.

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