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Crystal structure of tetrakis(μ(3)-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)tetrakis[aquacopper(II)]: a redetermination at 200 K
The crystal structure of the tetranuclear title compound, [Cu(4)(C(12)H(15)NO(5))(4)(H(2)O)(4)], has been previously reported by Back, Oliveira, Canabarro & Iglesias [Z. Anorg. Allg. Chem. (2015), 641, 941–947], based on room-temperature data. In the previously published structure, no standard...
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Formato: | Online Artículo Texto |
Lenguaje: | English |
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International Union of Crystallography
2015
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Materias: | |
Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC4647398/ https://www.ncbi.nlm.nih.gov/pubmed/26594407 http://dx.doi.org/10.1107/S2056989015017314 |
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author | Buvaylo, Elena A. Vassilyeva, Olga Yu. Skelton, Brian W. |
author_facet | Buvaylo, Elena A. Vassilyeva, Olga Yu. Skelton, Brian W. |
author_sort | Buvaylo, Elena A. |
collection | PubMed |
description | The crystal structure of the tetranuclear title compound, [Cu(4)(C(12)H(15)NO(5))(4)(H(2)O)(4)], has been previously reported by Back, Oliveira, Canabarro & Iglesias [Z. Anorg. Allg. Chem. (2015), 641, 941–947], based on room-temperature data. In the previously published structure, no standard uncertainties are recorded for the deprotonated hydroxymethyl group and water molecule O atoms coordinating to the metal atom indicating that they were not refined; furthermore, the H atoms of some OH groups and water molecules have not been positioned accurately. Since the current structure was determined at a lower temperature, all atoms, including the H atoms of these hydroxy groups and the water molecule, have been determined more accurately resulting in improved standard uncertainties in the bond lengths and angles. Diffraction data were collected at 200 K, rather than the more usual 100 K, due to apparent disordering at lower temperatures. In addition, it is now possible to report intra- and intermolecular O—H⋯O interactions. In the title complex molecule, which has crystallographic -4 symmetry, the Cu(II) ions are coordinated by the tridentate Schiff base ligands and water molecules, forming a tetranuclear Cu(4)O(4) cubane-like core. The Cu(II) ion adopts a CuNO(5) elongated octahedral environment. The coordination environment of Cu(II) at 200 K displays a small contraction of the Cu—N/O bonds, compared with the room-temperature structure. In the crystal lattice, the neutral clusters are linked by intermolecular O—H⋯O hydrogen bonds into a one-dimensional hydrogen-bonding network propagating along the b axis. |
format | Online Article Text |
id | pubmed-4647398 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2015 |
publisher | International Union of Crystallography |
record_format | MEDLINE/PubMed |
spelling | pubmed-46473982015-11-20 Crystal structure of tetrakis(μ(3)-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)tetrakis[aquacopper(II)]: a redetermination at 200 K Buvaylo, Elena A. Vassilyeva, Olga Yu. Skelton, Brian W. Acta Crystallogr E Crystallogr Commun Research Communications The crystal structure of the tetranuclear title compound, [Cu(4)(C(12)H(15)NO(5))(4)(H(2)O)(4)], has been previously reported by Back, Oliveira, Canabarro & Iglesias [Z. Anorg. Allg. Chem. (2015), 641, 941–947], based on room-temperature data. In the previously published structure, no standard uncertainties are recorded for the deprotonated hydroxymethyl group and water molecule O atoms coordinating to the metal atom indicating that they were not refined; furthermore, the H atoms of some OH groups and water molecules have not been positioned accurately. Since the current structure was determined at a lower temperature, all atoms, including the H atoms of these hydroxy groups and the water molecule, have been determined more accurately resulting in improved standard uncertainties in the bond lengths and angles. Diffraction data were collected at 200 K, rather than the more usual 100 K, due to apparent disordering at lower temperatures. In addition, it is now possible to report intra- and intermolecular O—H⋯O interactions. In the title complex molecule, which has crystallographic -4 symmetry, the Cu(II) ions are coordinated by the tridentate Schiff base ligands and water molecules, forming a tetranuclear Cu(4)O(4) cubane-like core. The Cu(II) ion adopts a CuNO(5) elongated octahedral environment. The coordination environment of Cu(II) at 200 K displays a small contraction of the Cu—N/O bonds, compared with the room-temperature structure. In the crystal lattice, the neutral clusters are linked by intermolecular O—H⋯O hydrogen bonds into a one-dimensional hydrogen-bonding network propagating along the b axis. International Union of Crystallography 2015-09-26 /pmc/articles/PMC4647398/ /pubmed/26594407 http://dx.doi.org/10.1107/S2056989015017314 Text en © Buvaylo et al. 2015 http://creativecommons.org/licenses/by/2.0/uk/ This is an open-access article distributed under the terms of the Creative Commons Attribution Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited. |
spellingShingle | Research Communications Buvaylo, Elena A. Vassilyeva, Olga Yu. Skelton, Brian W. Crystal structure of tetrakis(μ(3)-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)tetrakis[aquacopper(II)]: a redetermination at 200 K |
title | Crystal structure of tetrakis(μ(3)-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)tetrakis[aquacopper(II)]: a redetermination at 200 K |
title_full | Crystal structure of tetrakis(μ(3)-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)tetrakis[aquacopper(II)]: a redetermination at 200 K |
title_fullStr | Crystal structure of tetrakis(μ(3)-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)tetrakis[aquacopper(II)]: a redetermination at 200 K |
title_full_unstemmed | Crystal structure of tetrakis(μ(3)-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)tetrakis[aquacopper(II)]: a redetermination at 200 K |
title_short | Crystal structure of tetrakis(μ(3)-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)tetrakis[aquacopper(II)]: a redetermination at 200 K |
title_sort | crystal structure of tetrakis(μ(3)-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)tetrakis[aquacopper(ii)]: a redetermination at 200 k |
topic | Research Communications |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC4647398/ https://www.ncbi.nlm.nih.gov/pubmed/26594407 http://dx.doi.org/10.1107/S2056989015017314 |
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