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Crystal structure of (2,11-diaza[3.3](2,6)pyridinophane-κ (4) N,N′,N′′,N′′′)(1,6,7,12-tetraazaperylene-κ (2) N (1),N (12))ruthenium(II) bis(hexafluoridophosphate) acetonitrile 1.422-solvate
In the title compound, [Ru(C(14)H(16)N(4))(C(16)H(8)N(4))](PF(6))(2)·1.422CH(3)CN, discrete dimers of complex cations, [Ru(L–N(4)H(2))tape](2+) are formed {L–N(4)H(2) = 2,11-diaza[3.3](2,6)pyridinophane; tape = 1,6,7,12-tetraazaperylene}, held together by π–π stacking interactions via the tape...
Autores principales: | , , , , |
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Formato: | Online Artículo Texto |
Lenguaje: | English |
Publicado: |
International Union of Crystallography
2014
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Materias: | |
Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC4257199/ https://www.ncbi.nlm.nih.gov/pubmed/25484670 http://dx.doi.org/10.1107/S1600536814021060 |
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author | Brietzke, Thomas Rottke, Falko Otto Kelling, Alexandra Schilde, Uwe Holdt, Hans-Jürgen |
author_facet | Brietzke, Thomas Rottke, Falko Otto Kelling, Alexandra Schilde, Uwe Holdt, Hans-Jürgen |
author_sort | Brietzke, Thomas |
collection | PubMed |
description | In the title compound, [Ru(C(14)H(16)N(4))(C(16)H(8)N(4))](PF(6))(2)·1.422CH(3)CN, discrete dimers of complex cations, [Ru(L–N(4)H(2))tape](2+) are formed {L–N(4)H(2) = 2,11-diaza[3.3](2,6)pyridinophane; tape = 1,6,7,12-tetraazaperylene}, held together by π–π stacking interactions via the tape ligand moieties with a centroid–centroid distance of 3.49 (2) Å, assisted by hydrogen bonds between the non-coordinating tape ligand α,α′-diimine unit and the amine proton of a 2,11-diaza[3.3](2,6)-pyridinophane ligand of the opposite complex cation. The combination of these interactions leads to an unusual nearly face-to-face π–π stacking mode. Additional weak C—H⋯N, C—H⋯F, N—H⋯F and P—F⋯π-ring (tape, py) (with F⋯centroid distances of 2.925–3.984 Å) interactions are found, leading to a three-dimensional architecture. The Ru(II) atom is coordinated in a distorted octahedral geometry, particularly manifested by the N(amine)—Ru—N(amine) angle of 153.79 (10)°. The counter-charge is provided by two hexafluoridophosphate anions and the asymmetric unit is completed by acetonitrile solvent molecules of crystallization. Disorder was observed for both the hexafluoridophosphate anions as well as the acetonitrile solvate molecules, with occupancies for the major moieties of 0.801 (6) for one of the PF(6) anions, and a shared occupancy of 0.9215 (17) for the second PF(6) anion and a partially occupied acetonitrile molecule. A second CH(3)CN molecule is fully occupied, but 1:1 disordered across a crystallographic inversion center. |
format | Online Article Text |
id | pubmed-4257199 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2014 |
publisher | International Union of Crystallography |
record_format | MEDLINE/PubMed |
spelling | pubmed-42571992014-12-05 Crystal structure of (2,11-diaza[3.3](2,6)pyridinophane-κ (4) N,N′,N′′,N′′′)(1,6,7,12-tetraazaperylene-κ (2) N (1),N (12))ruthenium(II) bis(hexafluoridophosphate) acetonitrile 1.422-solvate Brietzke, Thomas Rottke, Falko Otto Kelling, Alexandra Schilde, Uwe Holdt, Hans-Jürgen Acta Crystallogr Sect E Struct Rep Online Research Communications In the title compound, [Ru(C(14)H(16)N(4))(C(16)H(8)N(4))](PF(6))(2)·1.422CH(3)CN, discrete dimers of complex cations, [Ru(L–N(4)H(2))tape](2+) are formed {L–N(4)H(2) = 2,11-diaza[3.3](2,6)pyridinophane; tape = 1,6,7,12-tetraazaperylene}, held together by π–π stacking interactions via the tape ligand moieties with a centroid–centroid distance of 3.49 (2) Å, assisted by hydrogen bonds between the non-coordinating tape ligand α,α′-diimine unit and the amine proton of a 2,11-diaza[3.3](2,6)-pyridinophane ligand of the opposite complex cation. The combination of these interactions leads to an unusual nearly face-to-face π–π stacking mode. Additional weak C—H⋯N, C—H⋯F, N—H⋯F and P—F⋯π-ring (tape, py) (with F⋯centroid distances of 2.925–3.984 Å) interactions are found, leading to a three-dimensional architecture. The Ru(II) atom is coordinated in a distorted octahedral geometry, particularly manifested by the N(amine)—Ru—N(amine) angle of 153.79 (10)°. The counter-charge is provided by two hexafluoridophosphate anions and the asymmetric unit is completed by acetonitrile solvent molecules of crystallization. Disorder was observed for both the hexafluoridophosphate anions as well as the acetonitrile solvate molecules, with occupancies for the major moieties of 0.801 (6) for one of the PF(6) anions, and a shared occupancy of 0.9215 (17) for the second PF(6) anion and a partially occupied acetonitrile molecule. A second CH(3)CN molecule is fully occupied, but 1:1 disordered across a crystallographic inversion center. International Union of Crystallography 2014-09-30 /pmc/articles/PMC4257199/ /pubmed/25484670 http://dx.doi.org/10.1107/S1600536814021060 Text en © Brietzke et al. 2014 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 Brietzke, Thomas Rottke, Falko Otto Kelling, Alexandra Schilde, Uwe Holdt, Hans-Jürgen Crystal structure of (2,11-diaza[3.3](2,6)pyridinophane-κ (4) N,N′,N′′,N′′′)(1,6,7,12-tetraazaperylene-κ (2) N (1),N (12))ruthenium(II) bis(hexafluoridophosphate) acetonitrile 1.422-solvate |
title | Crystal structure of (2,11-diaza[3.3](2,6)pyridinophane-κ
(4)
N,N′,N′′,N′′′)(1,6,7,12-tetraazaperylene-κ
(2)
N
(1),N
(12))ruthenium(II) bis(hexafluoridophosphate) acetonitrile 1.422-solvate |
title_full | Crystal structure of (2,11-diaza[3.3](2,6)pyridinophane-κ
(4)
N,N′,N′′,N′′′)(1,6,7,12-tetraazaperylene-κ
(2)
N
(1),N
(12))ruthenium(II) bis(hexafluoridophosphate) acetonitrile 1.422-solvate |
title_fullStr | Crystal structure of (2,11-diaza[3.3](2,6)pyridinophane-κ
(4)
N,N′,N′′,N′′′)(1,6,7,12-tetraazaperylene-κ
(2)
N
(1),N
(12))ruthenium(II) bis(hexafluoridophosphate) acetonitrile 1.422-solvate |
title_full_unstemmed | Crystal structure of (2,11-diaza[3.3](2,6)pyridinophane-κ
(4)
N,N′,N′′,N′′′)(1,6,7,12-tetraazaperylene-κ
(2)
N
(1),N
(12))ruthenium(II) bis(hexafluoridophosphate) acetonitrile 1.422-solvate |
title_short | Crystal structure of (2,11-diaza[3.3](2,6)pyridinophane-κ
(4)
N,N′,N′′,N′′′)(1,6,7,12-tetraazaperylene-κ
(2)
N
(1),N
(12))ruthenium(II) bis(hexafluoridophosphate) acetonitrile 1.422-solvate |
title_sort | crystal structure of (2,11-diaza[3.3](2,6)pyridinophane-κ
(4)
n,n′,n′′,n′′′)(1,6,7,12-tetraazaperylene-κ
(2)
n
(1),n
(12))ruthenium(ii) bis(hexafluoridophosphate) acetonitrile 1.422-solvate |
topic | Research Communications |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC4257199/ https://www.ncbi.nlm.nih.gov/pubmed/25484670 http://dx.doi.org/10.1107/S1600536814021060 |
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