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Crystal structure of imidazo[1,5-a]pyridinium-based hybrid salt (C(13)H(12)N(3))(2)[MnCl(4)]
A new organic–inorganic hybrid salt [L](2)[MnCl(4)] (I) where L (+) is the 2-methyl-3-(pyridin-2-yl)imidazo[1,5-a]pyridinium cation, is built of discrete organic cations and tetrachloridomanganate(II) anions. The L (+) cation was formed in situ in the oxidative cyclocondensation of 2-pyridinecar...
Autores principales: | , , , , , |
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Formato: | Online Artículo Texto |
Lenguaje: | English |
Publicado: |
International Union of Crystallography
2020
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Materias: | |
Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7057380/ https://www.ncbi.nlm.nih.gov/pubmed/32148866 http://dx.doi.org/10.1107/S2056989020001425 |
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author | Vassilyeva, Olga Yu. Buvaylo, Elena A. Kokozay, Vladimir N. Petrusenko, Svitlana R. Melnyk, Andrii K. Skelton, Brian W. |
author_facet | Vassilyeva, Olga Yu. Buvaylo, Elena A. Kokozay, Vladimir N. Petrusenko, Svitlana R. Melnyk, Andrii K. Skelton, Brian W. |
author_sort | Vassilyeva, Olga Yu. |
collection | PubMed |
description | A new organic–inorganic hybrid salt [L](2)[MnCl(4)] (I) where L (+) is the 2-methyl-3-(pyridin-2-yl)imidazo[1,5-a]pyridinium cation, is built of discrete organic cations and tetrachloridomanganate(II) anions. The L (+) cation was formed in situ in the oxidative cyclocondensation of 2-pyridinecarbaldehyde and CH(3)NH(2)·HCl in methanol. The structure was refined as a two-component twin using PLATON (Spek, 2020 ▸) to de-twin the data. The twin law (−1 0 0 0 − 1 0 0.5 0 1) was applied in the refinement where the twin component fraction refined to 0.155 (1). The compound crystallizes in the space group P2(1)/c with two crystallographically non-equivalent cations in the asymmetric unit, which possess similar structural conformations. The fused pyridinium and imidazolium rings of the cations are virtually coplanar [dihedral angles are 0.89 (18) and 0.78 (17)°]; the pendant pyridyl rings are twisted by 36.83 (14) and 36.14 (13)° with respect to the planes of the remaining atoms of the cations. The tetrahedral MnCl(4) (2–) anion is slightly distorted with the Mn—Cl distances falling in the range 2.3469 (10)–2.3941 (9) Å. The distortion value of 0.044 relative to the ideal tetrahedron was obtained by continuous shape measurement (CShM) analysis. In the crystal, the cations and anions form separate stacks propagating along the a-axis direction. The organic cations display weak π–π stacking. The anions, which are stacked identically one above the other, demonstrate loose packing; the minimum Mn⋯Mn separation in the cation stack is approximately 7.49 Å. The investigation of the fluorescent properties of a powdered sample of (I) showed no emission. X-band EPR data for (I) at 293 and 77 K revealed broad fine structure signals, indicating moderate zero-field splitting. |
format | Online Article Text |
id | pubmed-7057380 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2020 |
publisher | International Union of Crystallography |
record_format | MEDLINE/PubMed |
spelling | pubmed-70573802020-03-06 Crystal structure of imidazo[1,5-a]pyridinium-based hybrid salt (C(13)H(12)N(3))(2)[MnCl(4)] Vassilyeva, Olga Yu. Buvaylo, Elena A. Kokozay, Vladimir N. Petrusenko, Svitlana R. Melnyk, Andrii K. Skelton, Brian W. Acta Crystallogr E Crystallogr Commun Research Communications A new organic–inorganic hybrid salt [L](2)[MnCl(4)] (I) where L (+) is the 2-methyl-3-(pyridin-2-yl)imidazo[1,5-a]pyridinium cation, is built of discrete organic cations and tetrachloridomanganate(II) anions. The L (+) cation was formed in situ in the oxidative cyclocondensation of 2-pyridinecarbaldehyde and CH(3)NH(2)·HCl in methanol. The structure was refined as a two-component twin using PLATON (Spek, 2020 ▸) to de-twin the data. The twin law (−1 0 0 0 − 1 0 0.5 0 1) was applied in the refinement where the twin component fraction refined to 0.155 (1). The compound crystallizes in the space group P2(1)/c with two crystallographically non-equivalent cations in the asymmetric unit, which possess similar structural conformations. The fused pyridinium and imidazolium rings of the cations are virtually coplanar [dihedral angles are 0.89 (18) and 0.78 (17)°]; the pendant pyridyl rings are twisted by 36.83 (14) and 36.14 (13)° with respect to the planes of the remaining atoms of the cations. The tetrahedral MnCl(4) (2–) anion is slightly distorted with the Mn—Cl distances falling in the range 2.3469 (10)–2.3941 (9) Å. The distortion value of 0.044 relative to the ideal tetrahedron was obtained by continuous shape measurement (CShM) analysis. In the crystal, the cations and anions form separate stacks propagating along the a-axis direction. The organic cations display weak π–π stacking. The anions, which are stacked identically one above the other, demonstrate loose packing; the minimum Mn⋯Mn separation in the cation stack is approximately 7.49 Å. The investigation of the fluorescent properties of a powdered sample of (I) showed no emission. X-band EPR data for (I) at 293 and 77 K revealed broad fine structure signals, indicating moderate zero-field splitting. International Union of Crystallography 2020-02-06 /pmc/articles/PMC7057380/ /pubmed/32148866 http://dx.doi.org/10.1107/S2056989020001425 Text en © Vassilyeva et al. 2020 http://creativecommons.org/licenses/by/4.0/ 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/4.0/ |
spellingShingle | Research Communications Vassilyeva, Olga Yu. Buvaylo, Elena A. Kokozay, Vladimir N. Petrusenko, Svitlana R. Melnyk, Andrii K. Skelton, Brian W. Crystal structure of imidazo[1,5-a]pyridinium-based hybrid salt (C(13)H(12)N(3))(2)[MnCl(4)] |
title | Crystal structure of imidazo[1,5-a]pyridinium-based hybrid salt (C(13)H(12)N(3))(2)[MnCl(4)] |
title_full | Crystal structure of imidazo[1,5-a]pyridinium-based hybrid salt (C(13)H(12)N(3))(2)[MnCl(4)] |
title_fullStr | Crystal structure of imidazo[1,5-a]pyridinium-based hybrid salt (C(13)H(12)N(3))(2)[MnCl(4)] |
title_full_unstemmed | Crystal structure of imidazo[1,5-a]pyridinium-based hybrid salt (C(13)H(12)N(3))(2)[MnCl(4)] |
title_short | Crystal structure of imidazo[1,5-a]pyridinium-based hybrid salt (C(13)H(12)N(3))(2)[MnCl(4)] |
title_sort | crystal structure of imidazo[1,5-a]pyridinium-based hybrid salt (c(13)h(12)n(3))(2)[mncl(4)] |
topic | Research Communications |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7057380/ https://www.ncbi.nlm.nih.gov/pubmed/32148866 http://dx.doi.org/10.1107/S2056989020001425 |
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