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Crystal structures of two mononuclear complexes of terbium(III) nitrate with the tripodal alcohol 1,1,1-tris(hydroxymethyl)propane
Two new mononuclear cationic complexes in which the Tb(III) ion is bis-chelated by the tripodal alcohol 1,1,1-tris(hydroxymethyl)propane (H(3) L (Et), C(6)H(14)O(3)) were prepared from Tb(NO(3))(3)·5H(2)O and had their crystal and molecular structures solved by single-crystal X-ray diffraction...
Autores principales: | , , , , |
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Formato: | Online Artículo Texto |
Lenguaje: | English |
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International Union of Crystallography
2017
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Materias: | |
Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5290582/ https://www.ncbi.nlm.nih.gov/pubmed/28217359 http://dx.doi.org/10.1107/S2056989017001116 |
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author | Gregório, Thaiane Giese, Siddhartha O. K. Nunes, Giovana G. Soares, Jaísa F. Hughes, David L. |
author_facet | Gregório, Thaiane Giese, Siddhartha O. K. Nunes, Giovana G. Soares, Jaísa F. Hughes, David L. |
author_sort | Gregório, Thaiane |
collection | PubMed |
description | Two new mononuclear cationic complexes in which the Tb(III) ion is bis-chelated by the tripodal alcohol 1,1,1-tris(hydroxymethyl)propane (H(3) L (Et), C(6)H(14)O(3)) were prepared from Tb(NO(3))(3)·5H(2)O and had their crystal and molecular structures solved by single-crystal X-ray diffraction analysis after data collection at 100 K. Both products were isolated in reasonable yields from the same reaction mixture by using different crystallization conditions. The higher-symmetry complex dinitratobis[1,1,1-tris(hydroxymethyl)propane]terbium(III) nitrate dimethoxyethane hemisolvate, [Tb(NO(3))(2)(H(3) L (Et))(2)]NO(3)·0.5C(4)H(10)O(2), 1, in which the lanthanide ion is 10-coordinate and adopts an s-bicapped square-antiprismatic coordination geometry, contains two bidentate nitrate ions bound to the metal atom; another nitrate ion functions as a counter-ion and a half-molecule of dimethoxyethane (completed by a crystallographic twofold rotation axis) is also present. In product aquanitratobis[1,1,1-tris(hydroxymethyl)propane]terbium(III) dinitrate, [Tb(NO(3))(H(3) L (Et))(2)(H(2)O)](NO(3))(2), 2, one bidentate nitrate ion and one water molecule are bound to the nine-coordinate terbium(III) centre, while two free nitrate ions contribute to charge balance outside the tricapped trigonal-prismatic coordination polyhedron. No free water molecule was found in either of the crystal structures and, only in the case of 1, dimethoxyethane acts as a crystallizing solvent. In both molecular structures, the two tripodal ligands are bent to one side of the coordination sphere, leaving room for the anionic and water ligands. In complex 2, the methyl group of one of the H(3) L (Et) ligands is disordered over two alternative orientations. Strong hydrogen bonds, both intra- and intermolecular, are found in the crystal structures due to the number of different donor and acceptor groups present. |
format | Online Article Text |
id | pubmed-5290582 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2017 |
publisher | International Union of Crystallography |
record_format | MEDLINE/PubMed |
spelling | pubmed-52905822017-02-17 Crystal structures of two mononuclear complexes of terbium(III) nitrate with the tripodal alcohol 1,1,1-tris(hydroxymethyl)propane Gregório, Thaiane Giese, Siddhartha O. K. Nunes, Giovana G. Soares, Jaísa F. Hughes, David L. Acta Crystallogr E Crystallogr Commun Research Communications Two new mononuclear cationic complexes in which the Tb(III) ion is bis-chelated by the tripodal alcohol 1,1,1-tris(hydroxymethyl)propane (H(3) L (Et), C(6)H(14)O(3)) were prepared from Tb(NO(3))(3)·5H(2)O and had their crystal and molecular structures solved by single-crystal X-ray diffraction analysis after data collection at 100 K. Both products were isolated in reasonable yields from the same reaction mixture by using different crystallization conditions. The higher-symmetry complex dinitratobis[1,1,1-tris(hydroxymethyl)propane]terbium(III) nitrate dimethoxyethane hemisolvate, [Tb(NO(3))(2)(H(3) L (Et))(2)]NO(3)·0.5C(4)H(10)O(2), 1, in which the lanthanide ion is 10-coordinate and adopts an s-bicapped square-antiprismatic coordination geometry, contains two bidentate nitrate ions bound to the metal atom; another nitrate ion functions as a counter-ion and a half-molecule of dimethoxyethane (completed by a crystallographic twofold rotation axis) is also present. In product aquanitratobis[1,1,1-tris(hydroxymethyl)propane]terbium(III) dinitrate, [Tb(NO(3))(H(3) L (Et))(2)(H(2)O)](NO(3))(2), 2, one bidentate nitrate ion and one water molecule are bound to the nine-coordinate terbium(III) centre, while two free nitrate ions contribute to charge balance outside the tricapped trigonal-prismatic coordination polyhedron. No free water molecule was found in either of the crystal structures and, only in the case of 1, dimethoxyethane acts as a crystallizing solvent. In both molecular structures, the two tripodal ligands are bent to one side of the coordination sphere, leaving room for the anionic and water ligands. In complex 2, the methyl group of one of the H(3) L (Et) ligands is disordered over two alternative orientations. Strong hydrogen bonds, both intra- and intermolecular, are found in the crystal structures due to the number of different donor and acceptor groups present. International Union of Crystallography 2017-01-27 /pmc/articles/PMC5290582/ /pubmed/28217359 http://dx.doi.org/10.1107/S2056989017001116 Text en © Gregório et al. 2017 http://creativecommons.org/licenses/by/2.0/uk/ 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/2.0/uk/ |
spellingShingle | Research Communications Gregório, Thaiane Giese, Siddhartha O. K. Nunes, Giovana G. Soares, Jaísa F. Hughes, David L. Crystal structures of two mononuclear complexes of terbium(III) nitrate with the tripodal alcohol 1,1,1-tris(hydroxymethyl)propane |
title | Crystal structures of two mononuclear complexes of terbium(III) nitrate with the tripodal alcohol 1,1,1-tris(hydroxymethyl)propane |
title_full | Crystal structures of two mononuclear complexes of terbium(III) nitrate with the tripodal alcohol 1,1,1-tris(hydroxymethyl)propane |
title_fullStr | Crystal structures of two mononuclear complexes of terbium(III) nitrate with the tripodal alcohol 1,1,1-tris(hydroxymethyl)propane |
title_full_unstemmed | Crystal structures of two mononuclear complexes of terbium(III) nitrate with the tripodal alcohol 1,1,1-tris(hydroxymethyl)propane |
title_short | Crystal structures of two mononuclear complexes of terbium(III) nitrate with the tripodal alcohol 1,1,1-tris(hydroxymethyl)propane |
title_sort | crystal structures of two mononuclear complexes of terbium(iii) nitrate with the tripodal alcohol 1,1,1-tris(hydroxymethyl)propane |
topic | Research Communications |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5290582/ https://www.ncbi.nlm.nih.gov/pubmed/28217359 http://dx.doi.org/10.1107/S2056989017001116 |
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