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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 |
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International Union of Crystallography
2020
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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 |
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author | Gajecki, Leah Twamley, Brendan Berg, David J. |
author_facet | Gajecki, Leah Twamley, Brendan Berg, David J. |
author_sort | Gajecki, Leah |
collection | PubMed |
description | 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]. |
format | Online Article Text |
id | pubmed-7199245 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2020 |
publisher | International Union of Crystallography |
record_format | MEDLINE/PubMed |
spelling | pubmed-71992452020-05-19 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) Gajecki, Leah Twamley, Brendan Berg, David J. Acta Crystallogr E Crystallogr Commun Research Communications 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]. International Union of Crystallography 2020-04-21 /pmc/articles/PMC7199245/ /pubmed/32431936 http://dx.doi.org/10.1107/S2056989020005034 Text en © Gajecki et al. 2020 http://creativecommons.org/licenses/by/4.0/ This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.http://creativecommons.org/licenses/by/4.0/ |
spellingShingle | Research Communications Gajecki, Leah Twamley, Brendan Berg, David J. 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) |
title | 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) |
title_full | 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) |
title_fullStr | 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) |
title_full_unstemmed | 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) |
title_short | 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) |
title_sort | 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) |
topic | Research Communications |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7199245/ https://www.ncbi.nlm.nih.gov/pubmed/32431936 http://dx.doi.org/10.1107/S2056989020005034 |
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