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Synthesis, crystal structure and thermal decomposition pathway of bis(isoselenocyanato-κN)tetrakis(pyridine-κN)manganese(II)
The reaction of MnCl(2)·2H(2)O with KSeCN and pyridine in water leads to the formation of the title complex, [Mn(NCSe)(2)(C(5)H(5)N)(4)], which is isotypic to its Fe, Co, Ni, Zn and Cd analogues. In its crystal structure, discrete complexes are observed that are located on centres of inversion. The...
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Formato: | Online Artículo Texto |
Lenguaje: | English |
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International Union of Crystallography
2023
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Materias: | |
Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10162072/ https://www.ncbi.nlm.nih.gov/pubmed/37151823 http://dx.doi.org/10.1107/S2056989023003535 |
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author | Näther, Christian Mangelsen, Sebastian Boeckmann, Jan |
author_facet | Näther, Christian Mangelsen, Sebastian Boeckmann, Jan |
author_sort | Näther, Christian |
collection | PubMed |
description | The reaction of MnCl(2)·2H(2)O with KSeCN and pyridine in water leads to the formation of the title complex, [Mn(NCSe)(2)(C(5)H(5)N)(4)], which is isotypic to its Fe, Co, Ni, Zn and Cd analogues. In its crystal structure, discrete complexes are observed that are located on centres of inversion. The Mn cations are octahedrally coordinated by four pyridine coligands and two selenocyanate anions that coordinate via the N atom to the metal centres to generate trans-MnN(s)(2)N(p)(4) octahedra (s = selenocyanate and p = pyridine). In the extended structure, weak C—H⋯Se contacts are observed. Powder X-ray diffraction (PXRD) investigations prove that a pure sample was obtained and in the IR and Raman spectra, the C—N stretching vibrations are observed at 2058 and 2060 cm(−1), respectively, in agreement with the terminal coordination of the selenocyanate anions. Thermogravimetric investigations reveal that the pyridine coligands are removed in two separate steps. In the first mass loss, a compound with the composition Mn(NCSe)(2)(C(5)H(5)N)(2) is formed, whereas in the second mass loss, the remaining pyridine ligands are removed, which is superimposed with the decomposition of Mn(NCSe)(2) formed after ligand removal. In the intermediate compound Mn(NCSe)(2)(C(5)H(5)N)(2), the CN stretching vibration is observed at 2090 cm(−1) in the Raman and at 2099 cm(−1) in the IR spectra, indicating that the Mn cations are linked by μ-1,3-bridging anionic ligands. PXRD measurements show that a compound has formed that is of poor crystallinity. A comparison of the powder pattern with that calculated for the previously reported Cd(NCSe)(2)(C(5)H(5)N)(2) indicates that these compounds are isotypic, which was proven by a Pawley fit. |
format | Online Article Text |
id | pubmed-10162072 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2023 |
publisher | International Union of Crystallography |
record_format | MEDLINE/PubMed |
spelling | pubmed-101620722023-05-06 Synthesis, crystal structure and thermal decomposition pathway of bis(isoselenocyanato-κN)tetrakis(pyridine-κN)manganese(II) Näther, Christian Mangelsen, Sebastian Boeckmann, Jan Acta Crystallogr E Crystallogr Commun Research Communications The reaction of MnCl(2)·2H(2)O with KSeCN and pyridine in water leads to the formation of the title complex, [Mn(NCSe)(2)(C(5)H(5)N)(4)], which is isotypic to its Fe, Co, Ni, Zn and Cd analogues. In its crystal structure, discrete complexes are observed that are located on centres of inversion. The Mn cations are octahedrally coordinated by four pyridine coligands and two selenocyanate anions that coordinate via the N atom to the metal centres to generate trans-MnN(s)(2)N(p)(4) octahedra (s = selenocyanate and p = pyridine). In the extended structure, weak C—H⋯Se contacts are observed. Powder X-ray diffraction (PXRD) investigations prove that a pure sample was obtained and in the IR and Raman spectra, the C—N stretching vibrations are observed at 2058 and 2060 cm(−1), respectively, in agreement with the terminal coordination of the selenocyanate anions. Thermogravimetric investigations reveal that the pyridine coligands are removed in two separate steps. In the first mass loss, a compound with the composition Mn(NCSe)(2)(C(5)H(5)N)(2) is formed, whereas in the second mass loss, the remaining pyridine ligands are removed, which is superimposed with the decomposition of Mn(NCSe)(2) formed after ligand removal. In the intermediate compound Mn(NCSe)(2)(C(5)H(5)N)(2), the CN stretching vibration is observed at 2090 cm(−1) in the Raman and at 2099 cm(−1) in the IR spectra, indicating that the Mn cations are linked by μ-1,3-bridging anionic ligands. PXRD measurements show that a compound has formed that is of poor crystallinity. A comparison of the powder pattern with that calculated for the previously reported Cd(NCSe)(2)(C(5)H(5)N)(2) indicates that these compounds are isotypic, which was proven by a Pawley fit. International Union of Crystallography 2023-04-21 /pmc/articles/PMC10162072/ /pubmed/37151823 http://dx.doi.org/10.1107/S2056989023003535 Text en © Näther et al. 2023 https://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. |
spellingShingle | Research Communications Näther, Christian Mangelsen, Sebastian Boeckmann, Jan Synthesis, crystal structure and thermal decomposition pathway of bis(isoselenocyanato-κN)tetrakis(pyridine-κN)manganese(II) |
title | Synthesis, crystal structure and thermal decomposition pathway of bis(isoselenocyanato-κN)tetrakis(pyridine-κN)manganese(II) |
title_full | Synthesis, crystal structure and thermal decomposition pathway of bis(isoselenocyanato-κN)tetrakis(pyridine-κN)manganese(II) |
title_fullStr | Synthesis, crystal structure and thermal decomposition pathway of bis(isoselenocyanato-κN)tetrakis(pyridine-κN)manganese(II) |
title_full_unstemmed | Synthesis, crystal structure and thermal decomposition pathway of bis(isoselenocyanato-κN)tetrakis(pyridine-κN)manganese(II) |
title_short | Synthesis, crystal structure and thermal decomposition pathway of bis(isoselenocyanato-κN)tetrakis(pyridine-κN)manganese(II) |
title_sort | synthesis, crystal structure and thermal decomposition pathway of bis(isoselenocyanato-κn)tetrakis(pyridine-κn)manganese(ii) |
topic | Research Communications |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10162072/ https://www.ncbi.nlm.nih.gov/pubmed/37151823 http://dx.doi.org/10.1107/S2056989023003535 |
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