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Synthesis and crystallographic characterization of di-phenyl-amide rare-earth metal complexes

Authors :
Chad T, Palumbo
Christopher M, Kotyk
Joseph W, Ziller
William J, Evans
Source :
Acta Crystallographica Section E: Crystallographic Communications
Publication Year :
2020

Abstract

Crystallographic characterization of complexes of the smaller rare-earth elements Y, Dy, and Er with the NPh2 ligand reveals monometallic, bimetallic, and tetra­metallic structures.<br />Studies of the coordination chemistry between the di­phenyl­amide 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(di­phenyl­amido-κN)bis­(tetrahydro­furan-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)-di­phenyl­amido]­bis­[bis­(di­phenyl­amido-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 tetra­metallic ErIII bridging oxide hydrolysis product, bis­(μ-di­phenyl­amido-κ2 N:N)bis­[μ-1κN:2(η6)-di­phenyl­amido]­tetra­kis­(di­phenyl­amido-κN)di-μ3-oxido-tetra­erbium(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.

Details

ISSN :
20569890
Volume :
76
Issue :
Pt 9
Database :
OpenAIRE
Journal :
Acta crystallographica. Section E, Crystallographic communications
Accession number :
edsair.pmid..........40ea767d8787fdcd8168cf3612109b9e