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Synthesis and crystal structures of tetrameric [2-(4,4-dimethyl-2-oxazolin-2-yl)anilido]sodium and tris[2-(4,4-dimethyl-2-oxazolin-2-yl)anilido]ytterbium(III)
Reaction of 2-(4,4-dimethyl-2-oxazolin-2-yl)aniline (H(2)-L1) with one equivalent of Na[N(SiMe(3))(2)] in toluene afforded pale-yellow crystals of tetrameric poly[bis[μ(3)-2-(4,4-dimethyl-2-oxazolin-2-yl)anilinido][μ(2)-2-(4,4-dimethyl-2-oxazolin-2-yl)aniline]tetrasodium(I)], [Na(4)(C(11)H(13)N(...
Autores principales: | , , |
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Formato: | Online Artículo Texto |
Lenguaje: | English |
Publicado: |
International Union of Crystallography
2020
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Materias: | |
Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7199245/ https://www.ncbi.nlm.nih.gov/pubmed/32431936 http://dx.doi.org/10.1107/S2056989020005034 |
Sumario: | Reaction of 2-(4,4-dimethyl-2-oxazolin-2-yl)aniline (H(2)-L1) with one equivalent of Na[N(SiMe(3))(2)] in toluene afforded pale-yellow crystals of tetrameric poly[bis[μ(3)-2-(4,4-dimethyl-2-oxazolin-2-yl)anilinido][μ(2)-2-(4,4-dimethyl-2-oxazolin-2-yl)aniline]tetrasodium(I)], [Na(4)(C(11)H(13)N(2)O)(4)](n) or [Na(4)(H-L1)(4)](n) (2), in excellent yield. Subsequent reaction of [Na(4)(H-L1)(4)](n) (2) with 1.33 equivalents of anhydrous YbCl(3) in a 50:50 mixture of toluene–THF afforded yellow crystals of tris[2-(4,4-dimethyl-2-oxazolin-2-yl)anilinido]ytterbium(III), [Yb(C(11)H(13)N(2)O)(3)] or Yb(H-L1)(3) (3) in moderate yield. Direct reaction of three equivalents of 2-(4′,4′-dimethyl-2′-oxazolinyl)aniline (H(2)-L1) with Yb[N(SiMe(3))(2)](3) in toluene resulted in elimination of hexamethyldisilazane, HN(SiMe(3))(2), and produced Yb(H-L1)(3) (3) in excellent yield. The structure of 2 consists of tetrameric Na(4)(H-L1)(4) subunits in which each Na(+) cation is bound to two H-L1 bridging bidentate ligands and these subunits are connected into a polymeric chain by two of the four oxazoline O atoms bridging to Na(+) cations in the adjacent tetramer. This results in two 4-coordinate and two 5-coordinate Na(+) cations within each tetrameric unit. The structure of 3 consists of a distorted octahedron where the bite angle of ligand L1 ranges between 74.72 (11) and 77.79 (11) degrees. The oxazoline (and anilide) N atoms occupy meridional sites such that for one ligand an anilide nitrogen is trans to an oxazoline nitrogen while for the other two oxazoline N atoms are trans to each other. This results in a significantly longer Yb—N(oxazoline) distance [2.468 (3) Å] for the bond trans to the anilide compared to those for the oxazoline N atoms trans to one another [2.376 (3), 2.390 (3) Å]. |
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