Synthesis and crystallographic characterization of di-phenyl-amide rare-earth metal complexes Ln(NPh2)3(THF)2 and [(Ph2N)2 Ln(μ-NPh2)]2.

Studies of the coordination chemistry between the di-phenyl-amide ligand, NPh2, and the smaller rare-earth Ln III ions, Ln = Y, Dy, and Er, led to the structural characterization by single-crystal X-ray diffraction crystallography of both solvated and unsolvated complexes, namely, tris-(di-phenyl-amido-κN)bis-(tetrahydro-furan-κO)yttrium(III), Y(NPh2)3(THF)2 or [Y(C12H10N)3(C4H8O)2], 1-Y, and the erbium(III) (Er), 1-Er, analogue, and bis-[μ-1κN:2(η6)-di-phenyl-amido]-bis-[bis-(di-phenyl-amido-κN)yttrium(III)], [(Ph2N)2Y(μ-NPh2)]2 or [Y2(C12H10N)6], 2-Y, and the dysprosium(III) (Dy), 2-Dy, analogue. The THF ligands of 1-Er are modeled with disorder across two positions with occupancies of 0.627 (12):0.323 (12) and 0.633 (7):0.367 (7). Also structurally characterized was the tetra-metallic ErIII bridging oxide hydrolysis product, bis-(μ-di-phenyl-amido-κ2 N:N)bis-[μ-1κN:2(η6)-di-phenyl-amido]-tetra-kis-(di-phenyl-amido-κN)di-μ3-oxido-tetra-erbium(III) benzene disolvate, {[(Ph2N)Er(μ-NPh2)]4(μ-O)2}·(C6H6)2 or [Er4(C12H10N)8O2]·2C6H6, 3-Er. The 3-Er structure was refined as a three-component twin with occupancies 0.7375:0.2010:0.0615. © Palumbo et al. 2020.