Cargando…
Crystal structures of binuclear complexes of gadolinium(III) and dysprosium(III) with oxalate bridges and chelating N,N′-bis(2-oxidobenzyl)-N,N′-bis(pyridin-2-ylmethyl)ethylenediamine (bbpen(2−))
The reaction between mononuclear [Ln(bbpen)Cl] [Ln = Gd or Dy; H(2)bbpen = N,N′-bis(2-hydroxybenzyl)-N,N′-bis(pyridin-2-ylmethyl)ethylenediamine, C(28)H(30)N(4)O(2)] and potassium oxalate monohydrate in water/methanol produced the solvated centrosymmetric isostructural binuclear (μ-oxalato)b...
Autores principales: | , , , |
---|---|
Formato: | Online Artículo Texto |
Lenguaje: | English |
Publicado: |
International Union of Crystallography
2019
|
Materias: | |
Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC6509678/ https://www.ncbi.nlm.nih.gov/pubmed/31161048 http://dx.doi.org/10.1107/S2056989019002998 |
_version_ | 1783417290412261376 |
---|---|
author | Barbosa, Guilherme Augusto Santana, Francielli Sousa Nunes, Giovana Gioppo Soares, Jaísa Fernandes |
author_facet | Barbosa, Guilherme Augusto Santana, Francielli Sousa Nunes, Giovana Gioppo Soares, Jaísa Fernandes |
author_sort | Barbosa, Guilherme Augusto |
collection | PubMed |
description | The reaction between mononuclear [Ln(bbpen)Cl] [Ln = Gd or Dy; H(2)bbpen = N,N′-bis(2-hydroxybenzyl)-N,N′-bis(pyridin-2-ylmethyl)ethylenediamine, C(28)H(30)N(4)O(2)] and potassium oxalate monohydrate in water/methanol produced the solvated centrosymmetric isostructural binuclear (μ-oxalato)bis{[N,N′-bis(2-oxidobenzyl-κO)-N,N′-bis(pyridin-2-ylmethyl-κN)ethylenediamine-κ(2) N,N′]dilanthanide(III)}–methanol–water (1/4/4) complexes, [Ln (2)(C(28)H(28)N(4)O(2))(2)(C(2)O(4))]·4CH(3)OH·4H(2)O, with lanthanide(III) = gadolinium(III) (Ln = Gd) and dysprosium(III) (Ln = Dy), in high yields (ca 70%) directly from the reaction mixtures. In both complexes, the lanthanide ion is eight-coordinate and adopts a distorted square-antiprismatic coordination environment. The triclinic (P [Image: see text]) unit cell contains one dimeric unit together with four water and four methanol molecules; in the final structural model, two of each type of solvating molecule refine well. In each lanthanide(III) dimeric molecule, the medium-strength O⋯H—O hydrogen-bonding pattern involves four oxygen atoms, two of them from the phenolate groups that are ‘bridged’ by one water and one methanol molecule. These interactions seem to contribute to the stabilization of the relatively compact shape of the dimer. Electron densities associated with an additional water and methanol molecule were removed with the SQUEEZE procedure in PLATON [Spek (2015 ▸). Acta Cryst. C71, 9–18]. These two new compounds are of interest with respect to magnetic properties. |
format | Online Article Text |
id | pubmed-6509678 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2019 |
publisher | International Union of Crystallography |
record_format | MEDLINE/PubMed |
spelling | pubmed-65096782019-06-03 Crystal structures of binuclear complexes of gadolinium(III) and dysprosium(III) with oxalate bridges and chelating N,N′-bis(2-oxidobenzyl)-N,N′-bis(pyridin-2-ylmethyl)ethylenediamine (bbpen(2−)) Barbosa, Guilherme Augusto Santana, Francielli Sousa Nunes, Giovana Gioppo Soares, Jaísa Fernandes Acta Crystallogr E Crystallogr Commun Research Communications The reaction between mononuclear [Ln(bbpen)Cl] [Ln = Gd or Dy; H(2)bbpen = N,N′-bis(2-hydroxybenzyl)-N,N′-bis(pyridin-2-ylmethyl)ethylenediamine, C(28)H(30)N(4)O(2)] and potassium oxalate monohydrate in water/methanol produced the solvated centrosymmetric isostructural binuclear (μ-oxalato)bis{[N,N′-bis(2-oxidobenzyl-κO)-N,N′-bis(pyridin-2-ylmethyl-κN)ethylenediamine-κ(2) N,N′]dilanthanide(III)}–methanol–water (1/4/4) complexes, [Ln (2)(C(28)H(28)N(4)O(2))(2)(C(2)O(4))]·4CH(3)OH·4H(2)O, with lanthanide(III) = gadolinium(III) (Ln = Gd) and dysprosium(III) (Ln = Dy), in high yields (ca 70%) directly from the reaction mixtures. In both complexes, the lanthanide ion is eight-coordinate and adopts a distorted square-antiprismatic coordination environment. The triclinic (P [Image: see text]) unit cell contains one dimeric unit together with four water and four methanol molecules; in the final structural model, two of each type of solvating molecule refine well. In each lanthanide(III) dimeric molecule, the medium-strength O⋯H—O hydrogen-bonding pattern involves four oxygen atoms, two of them from the phenolate groups that are ‘bridged’ by one water and one methanol molecule. These interactions seem to contribute to the stabilization of the relatively compact shape of the dimer. Electron densities associated with an additional water and methanol molecule were removed with the SQUEEZE procedure in PLATON [Spek (2015 ▸). Acta Cryst. C71, 9–18]. These two new compounds are of interest with respect to magnetic properties. International Union of Crystallography 2019-03-05 /pmc/articles/PMC6509678/ /pubmed/31161048 http://dx.doi.org/10.1107/S2056989019002998 Text en © Barbosa et al. 2019 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 Barbosa, Guilherme Augusto Santana, Francielli Sousa Nunes, Giovana Gioppo Soares, Jaísa Fernandes Crystal structures of binuclear complexes of gadolinium(III) and dysprosium(III) with oxalate bridges and chelating N,N′-bis(2-oxidobenzyl)-N,N′-bis(pyridin-2-ylmethyl)ethylenediamine (bbpen(2−)) |
title | Crystal structures of binuclear complexes of gadolinium(III) and dysprosium(III) with oxalate bridges and chelating N,N′-bis(2-oxidobenzyl)-N,N′-bis(pyridin-2-ylmethyl)ethylenediamine (bbpen(2−)) |
title_full | Crystal structures of binuclear complexes of gadolinium(III) and dysprosium(III) with oxalate bridges and chelating N,N′-bis(2-oxidobenzyl)-N,N′-bis(pyridin-2-ylmethyl)ethylenediamine (bbpen(2−)) |
title_fullStr | Crystal structures of binuclear complexes of gadolinium(III) and dysprosium(III) with oxalate bridges and chelating N,N′-bis(2-oxidobenzyl)-N,N′-bis(pyridin-2-ylmethyl)ethylenediamine (bbpen(2−)) |
title_full_unstemmed | Crystal structures of binuclear complexes of gadolinium(III) and dysprosium(III) with oxalate bridges and chelating N,N′-bis(2-oxidobenzyl)-N,N′-bis(pyridin-2-ylmethyl)ethylenediamine (bbpen(2−)) |
title_short | Crystal structures of binuclear complexes of gadolinium(III) and dysprosium(III) with oxalate bridges and chelating N,N′-bis(2-oxidobenzyl)-N,N′-bis(pyridin-2-ylmethyl)ethylenediamine (bbpen(2−)) |
title_sort | crystal structures of binuclear complexes of gadolinium(iii) and dysprosium(iii) with oxalate bridges and chelating n,n′-bis(2-oxidobenzyl)-n,n′-bis(pyridin-2-ylmethyl)ethylenediamine (bbpen(2−)) |
topic | Research Communications |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC6509678/ https://www.ncbi.nlm.nih.gov/pubmed/31161048 http://dx.doi.org/10.1107/S2056989019002998 |
work_keys_str_mv | AT barbosaguilhermeaugusto crystalstructuresofbinuclearcomplexesofgadoliniumiiianddysprosiumiiiwithoxalatebridgesandchelatingnnbis2oxidobenzylnnbispyridin2ylmethylethylenediaminebbpen2 AT santanafranciellisousa crystalstructuresofbinuclearcomplexesofgadoliniumiiianddysprosiumiiiwithoxalatebridgesandchelatingnnbis2oxidobenzylnnbispyridin2ylmethylethylenediaminebbpen2 AT nunesgiovanagioppo crystalstructuresofbinuclearcomplexesofgadoliniumiiianddysprosiumiiiwithoxalatebridgesandchelatingnnbis2oxidobenzylnnbispyridin2ylmethylethylenediaminebbpen2 AT soaresjaisafernandes crystalstructuresofbinuclearcomplexesofgadoliniumiiianddysprosiumiiiwithoxalatebridgesandchelatingnnbis2oxidobenzylnnbispyridin2ylmethylethylenediaminebbpen2 |