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Crystal structure of bis{μ(2)-2,2′-[(4,10-dimethyl-1,4,7,10-tetraazacyclododecane-1,7-diyl)bis(methylene)]bis(4-oxo-4H-pyran-3-olato)}dicobaltcalcium bis(perchlorate) 1.36-hydrate
The title compound, [CaCo(2)(C(22)H(30)N(4)O(6))(2)](ClO(4))(2)·1.36H(2)O or {Ca[Co(H(–2) L1)](2)}·2ClO(4)·1.36H(2)O {where L1 is 4,10-bis[(3-hydroxy-4-pyron-2-yl)methyl]-1,7-dimethyl-1,4,7,10-tetraazacyclododecane}, is a trinuclear complex whose asymmetric unit comprises a quarter of the {Ca[...
Autores principales: | , , , , , |
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Formato: | Online Artículo Texto |
Lenguaje: | English |
Publicado: |
International Union of Crystallography
2017
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Materias: | |
Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5730261/ https://www.ncbi.nlm.nih.gov/pubmed/29250424 http://dx.doi.org/10.1107/S2056989017016693 |
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author | Rossi, Patrizia Macedi, Eleonora Paoli, Paola Giorgi, Luca Formica, Mauro Fusi, Vieri |
author_facet | Rossi, Patrizia Macedi, Eleonora Paoli, Paola Giorgi, Luca Formica, Mauro Fusi, Vieri |
author_sort | Rossi, Patrizia |
collection | PubMed |
description | The title compound, [CaCo(2)(C(22)H(30)N(4)O(6))(2)](ClO(4))(2)·1.36H(2)O or {Ca[Co(H(–2) L1)](2)}·2ClO(4)·1.36H(2)O {where L1 is 4,10-bis[(3-hydroxy-4-pyron-2-yl)methyl]-1,7-dimethyl-1,4,7,10-tetraazacyclododecane}, is a trinuclear complex whose asymmetric unit comprises a quarter of the {Ca[Co(H(–2) L1)](2)}(2+) trinuclear complex, half of a perchlorate ion and 0.34-water molecules. In the neutral [Co(H(–2) L1)] moiety, the cobalt ion is hexacoordinated in a trigonal–prismatic fashion by the surrounding N(4)O(2) donor set. A Ca(2+) cation holds together two neutral [Co(H(–2) L1)] moieties and is octacoordinated in a distorted trigonal–dodecahedral fashion by the surrounding O atoms belonging to the deprotonated oxide and carbonyl groups of two [Co(H(–2) L1)] units. The coordination of the Co(II) cation preorganizes L1 and an electron-rich area forms, which is able to host hard metal ions. The comparison between the present structure and the previously published ones suggests a high versatility of this ligand; indeed, hard metal ions with different nature and dimensions lead to complexes having different stoichiometry (mono- and dinuclear monomers and trinuclear dimers) or even a polymeric structure. The heterotrinuclear Co(II)–Ca(II)–Co(II) complexes are connected in three dimensions via weak C—H⋯O hydrogen bonds, which are also responsible for the interactions with the perchlorate anions and the lattice water molecules. The perchlorate anion is disordered about a twofold rotation axis and was refined giving the two positions a fixed occupancy factor of 0.5. The crystal studied was refined as a two-component inversion twin [BASF parameter = 0.14 (4)]. |
format | Online Article Text |
id | pubmed-5730261 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2017 |
publisher | International Union of Crystallography |
record_format | MEDLINE/PubMed |
spelling | pubmed-57302612017-12-15 Crystal structure of bis{μ(2)-2,2′-[(4,10-dimethyl-1,4,7,10-tetraazacyclododecane-1,7-diyl)bis(methylene)]bis(4-oxo-4H-pyran-3-olato)}dicobaltcalcium bis(perchlorate) 1.36-hydrate Rossi, Patrizia Macedi, Eleonora Paoli, Paola Giorgi, Luca Formica, Mauro Fusi, Vieri Acta Crystallogr E Crystallogr Commun Research Communications The title compound, [CaCo(2)(C(22)H(30)N(4)O(6))(2)](ClO(4))(2)·1.36H(2)O or {Ca[Co(H(–2) L1)](2)}·2ClO(4)·1.36H(2)O {where L1 is 4,10-bis[(3-hydroxy-4-pyron-2-yl)methyl]-1,7-dimethyl-1,4,7,10-tetraazacyclododecane}, is a trinuclear complex whose asymmetric unit comprises a quarter of the {Ca[Co(H(–2) L1)](2)}(2+) trinuclear complex, half of a perchlorate ion and 0.34-water molecules. In the neutral [Co(H(–2) L1)] moiety, the cobalt ion is hexacoordinated in a trigonal–prismatic fashion by the surrounding N(4)O(2) donor set. A Ca(2+) cation holds together two neutral [Co(H(–2) L1)] moieties and is octacoordinated in a distorted trigonal–dodecahedral fashion by the surrounding O atoms belonging to the deprotonated oxide and carbonyl groups of two [Co(H(–2) L1)] units. The coordination of the Co(II) cation preorganizes L1 and an electron-rich area forms, which is able to host hard metal ions. The comparison between the present structure and the previously published ones suggests a high versatility of this ligand; indeed, hard metal ions with different nature and dimensions lead to complexes having different stoichiometry (mono- and dinuclear monomers and trinuclear dimers) or even a polymeric structure. The heterotrinuclear Co(II)–Ca(II)–Co(II) complexes are connected in three dimensions via weak C—H⋯O hydrogen bonds, which are also responsible for the interactions with the perchlorate anions and the lattice water molecules. The perchlorate anion is disordered about a twofold rotation axis and was refined giving the two positions a fixed occupancy factor of 0.5. The crystal studied was refined as a two-component inversion twin [BASF parameter = 0.14 (4)]. International Union of Crystallography 2017-11-28 /pmc/articles/PMC5730261/ /pubmed/29250424 http://dx.doi.org/10.1107/S2056989017016693 Text en © Rossi 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 Rossi, Patrizia Macedi, Eleonora Paoli, Paola Giorgi, Luca Formica, Mauro Fusi, Vieri Crystal structure of bis{μ(2)-2,2′-[(4,10-dimethyl-1,4,7,10-tetraazacyclododecane-1,7-diyl)bis(methylene)]bis(4-oxo-4H-pyran-3-olato)}dicobaltcalcium bis(perchlorate) 1.36-hydrate |
title | Crystal structure of bis{μ(2)-2,2′-[(4,10-dimethyl-1,4,7,10-tetraazacyclododecane-1,7-diyl)bis(methylene)]bis(4-oxo-4H-pyran-3-olato)}dicobaltcalcium bis(perchlorate) 1.36-hydrate |
title_full | Crystal structure of bis{μ(2)-2,2′-[(4,10-dimethyl-1,4,7,10-tetraazacyclododecane-1,7-diyl)bis(methylene)]bis(4-oxo-4H-pyran-3-olato)}dicobaltcalcium bis(perchlorate) 1.36-hydrate |
title_fullStr | Crystal structure of bis{μ(2)-2,2′-[(4,10-dimethyl-1,4,7,10-tetraazacyclododecane-1,7-diyl)bis(methylene)]bis(4-oxo-4H-pyran-3-olato)}dicobaltcalcium bis(perchlorate) 1.36-hydrate |
title_full_unstemmed | Crystal structure of bis{μ(2)-2,2′-[(4,10-dimethyl-1,4,7,10-tetraazacyclododecane-1,7-diyl)bis(methylene)]bis(4-oxo-4H-pyran-3-olato)}dicobaltcalcium bis(perchlorate) 1.36-hydrate |
title_short | Crystal structure of bis{μ(2)-2,2′-[(4,10-dimethyl-1,4,7,10-tetraazacyclododecane-1,7-diyl)bis(methylene)]bis(4-oxo-4H-pyran-3-olato)}dicobaltcalcium bis(perchlorate) 1.36-hydrate |
title_sort | crystal structure of bis{μ(2)-2,2′-[(4,10-dimethyl-1,4,7,10-tetraazacyclododecane-1,7-diyl)bis(methylene)]bis(4-oxo-4h-pyran-3-olato)}dicobaltcalcium bis(perchlorate) 1.36-hydrate |
topic | Research Communications |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5730261/ https://www.ncbi.nlm.nih.gov/pubmed/29250424 http://dx.doi.org/10.1107/S2056989017016693 |
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