Crystal structure of tetrakis(μ3-2-{[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, [Cu4(C12H15NO5)4(H2O)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 a...
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| Format: | Article |
| Language: | English |
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International Union of Crystallography
2015-10-01
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| Series: | Acta Crystallographica Section E: Crystallographic Communications |
| Subjects: | |
| Online Access: | http://scripts.iucr.org/cgi-bin/paper?S2056989015017314 |
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| author | Elena A. Buvaylo Olga Yu. Vassilyeva Brian W. Skelton |
| author_facet | Elena A. Buvaylo Olga Yu. Vassilyeva Brian W. Skelton |
| author_sort | Elena A. Buvaylo |
| collection | DOAJ |
| description | The crystal structure of the tetranuclear title compound, [Cu4(C12H15NO5)4(H2O)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 CuII ions are coordinated by the tridentate Schiff base ligands and water molecules, forming a tetranuclear Cu4O4 cubane-like core. The CuII ion adopts a CuNO5 elongated octahedral environment. The coordination environment of CuII 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. |
| first_indexed | 2024-12-20T23:01:03Z |
| format | Article |
| id | doaj.art-643e9f52b13c425aa156284fe3941ac8 |
| institution | Directory Open Access Journal |
| issn | 2056-9890 |
| language | English |
| last_indexed | 2024-12-20T23:01:03Z |
| publishDate | 2015-10-01 |
| publisher | International Union of Crystallography |
| record_format | Article |
| series | Acta Crystallographica Section E: Crystallographic Communications |
| spelling | doaj.art-643e9f52b13c425aa156284fe3941ac82022-12-21T19:23:59ZengInternational Union of CrystallographyActa Crystallographica Section E: Crystallographic Communications2056-98902015-10-0171101203120610.1107/S2056989015017314sj5474Crystal structure of tetrakis(μ3-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)tetrakis[aquacopper(II)]: a redetermination at 200 KElena A. Buvaylo0Olga Yu. Vassilyeva1Brian W. Skelton2Department of Inorganic Chemistry, Taras Shevchenko National University of Kyiv, 64/13 Volodymyrska Street, Kyiv 01601, UkraineDepartment of Inorganic Chemistry, Taras Shevchenko National University of Kyiv, 64/13 Volodymyrska Street, Kyiv 01601, UkraineCentre for Microscopy, Characterisation and Analysis, M313, University of Western Australia, Perth, WA 6009, AustraliaThe crystal structure of the tetranuclear title compound, [Cu4(C12H15NO5)4(H2O)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 CuII ions are coordinated by the tridentate Schiff base ligands and water molecules, forming a tetranuclear Cu4O4 cubane-like core. The CuII ion adopts a CuNO5 elongated octahedral environment. The coordination environment of CuII 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.http://scripts.iucr.org/cgi-bin/paper?S2056989015017314crystal structureCuII cubane-type complexSchiff base ligando-vanillintris(hydroxymethyl)aminomethanehydrogen bonding |
| spellingShingle | Elena A. Buvaylo Olga Yu. Vassilyeva Brian W. Skelton Crystal structure of tetrakis(μ3-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)tetrakis[aquacopper(II)]: a redetermination at 200 K Acta Crystallographica Section E: Crystallographic Communications crystal structure CuII cubane-type complex Schiff base ligand o-vanillin tris(hydroxymethyl)aminomethane hydrogen bonding |
| title | Crystal structure of tetrakis(μ3-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)tetrakis[aquacopper(II)]: a redetermination at 200 K |
| title_full | Crystal structure of tetrakis(μ3-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)tetrakis[aquacopper(II)]: a redetermination at 200 K |
| title_fullStr | Crystal structure of tetrakis(μ3-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)tetrakis[aquacopper(II)]: a redetermination at 200 K |
| title_full_unstemmed | Crystal structure of tetrakis(μ3-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)tetrakis[aquacopper(II)]: a redetermination at 200 K |
| title_short | Crystal structure of tetrakis(μ3-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)tetrakis[aquacopper(II)]: a redetermination at 200 K |
| title_sort | crystal structure of tetrakis μ3 2 1 1 bis hydroxymethyl 2 oxidoethyl iminomethyl 6 methoxyphenolato tetrakis aquacopper ii a redetermination at 200 k |
| topic | crystal structure CuII cubane-type complex Schiff base ligand o-vanillin tris(hydroxymethyl)aminomethane hydrogen bonding |
| url | http://scripts.iucr.org/cgi-bin/paper?S2056989015017314 |
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