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Synthesis, crystal structure and properties of bis(isoselenocyanato-κN)tetrakis(pyridine-κN)nickel(II)
The reaction of nickel chloride hexahydrate with potassium selenocyanate and pyridine in water leads to the formation of crystals of the title complex, [Ni(NCSe)(2)(C(5)H(5)N)(4)], which were characterized by single-crystal X-ray diffraction. Its crystal structure consists of discrete complexes, l...
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Formato: | Online Artículo Texto |
Lenguaje: | English |
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International Union of Crystallography
2023
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Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9912460/ https://www.ncbi.nlm.nih.gov/pubmed/36793409 http://dx.doi.org/10.1107/S2056989023000245 |
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author | Näther, Christian Boeckmann, Jan |
author_facet | Näther, Christian Boeckmann, Jan |
author_sort | Näther, Christian |
collection | PubMed |
description | The reaction of nickel chloride hexahydrate with potassium selenocyanate and pyridine in water leads to the formation of crystals of the title complex, [Ni(NCSe)(2)(C(5)H(5)N)(4)], which were characterized by single-crystal X-ray diffraction. Its crystal structure consists of discrete complexes, located on centers of inversion, in which the Ni cations are sixfold coordinated by two terminal N-bonded selenocyanate anions and four pyridine ligands within a slightly distorted octahedral coordination. In the crystal, the complexes are connected by weak C—H⋯Se interactions. PXRD investigations revealed that a pure crystalline phase has formed. In the IR and Raman spectra, the C—N stretching vibrations are observed at 2083 and 2079 cm(−1), respectively, in agreement with the presence of only terminally bonded anionic ligands. Upon heating, one well-resolved mass loss is observed, in which two of the four pyridine ligands are removed, leading to a compound with the composition Ni(NCSe)(2)(C(5)H(5)N)(2). In this compound, the C—N stretching vibration is shifted to 2108 cm(−1) (Raman) and 2115 cm(−1) (IR), indicating the presence of μ-1,3-bridging anionic ligands. In its PXRD pattern, very broad reflections are observed, indicating for poor crystallinity and/or very small particle size. This crystalline phase is not isotypic to its Co and Fe analogs. |
format | Online Article Text |
id | pubmed-9912460 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2023 |
publisher | International Union of Crystallography |
record_format | MEDLINE/PubMed |
spelling | pubmed-99124602023-02-14 Synthesis, crystal structure and properties of bis(isoselenocyanato-κN)tetrakis(pyridine-κN)nickel(II) Näther, Christian Boeckmann, Jan Acta Crystallogr E Crystallogr Commun Research Communications The reaction of nickel chloride hexahydrate with potassium selenocyanate and pyridine in water leads to the formation of crystals of the title complex, [Ni(NCSe)(2)(C(5)H(5)N)(4)], which were characterized by single-crystal X-ray diffraction. Its crystal structure consists of discrete complexes, located on centers of inversion, in which the Ni cations are sixfold coordinated by two terminal N-bonded selenocyanate anions and four pyridine ligands within a slightly distorted octahedral coordination. In the crystal, the complexes are connected by weak C—H⋯Se interactions. PXRD investigations revealed that a pure crystalline phase has formed. In the IR and Raman spectra, the C—N stretching vibrations are observed at 2083 and 2079 cm(−1), respectively, in agreement with the presence of only terminally bonded anionic ligands. Upon heating, one well-resolved mass loss is observed, in which two of the four pyridine ligands are removed, leading to a compound with the composition Ni(NCSe)(2)(C(5)H(5)N)(2). In this compound, the C—N stretching vibration is shifted to 2108 cm(−1) (Raman) and 2115 cm(−1) (IR), indicating the presence of μ-1,3-bridging anionic ligands. In its PXRD pattern, very broad reflections are observed, indicating for poor crystallinity and/or very small particle size. This crystalline phase is not isotypic to its Co and Fe analogs. International Union of Crystallography 2023-01-12 /pmc/articles/PMC9912460/ /pubmed/36793409 http://dx.doi.org/10.1107/S2056989023000245 Text en © Näther and Boeckmann 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 Boeckmann, Jan Synthesis, crystal structure and properties of bis(isoselenocyanato-κN)tetrakis(pyridine-κN)nickel(II) |
title | Synthesis, crystal structure and properties of bis(isoselenocyanato-κN)tetrakis(pyridine-κN)nickel(II) |
title_full | Synthesis, crystal structure and properties of bis(isoselenocyanato-κN)tetrakis(pyridine-κN)nickel(II) |
title_fullStr | Synthesis, crystal structure and properties of bis(isoselenocyanato-κN)tetrakis(pyridine-κN)nickel(II) |
title_full_unstemmed | Synthesis, crystal structure and properties of bis(isoselenocyanato-κN)tetrakis(pyridine-κN)nickel(II) |
title_short | Synthesis, crystal structure and properties of bis(isoselenocyanato-κN)tetrakis(pyridine-κN)nickel(II) |
title_sort | synthesis, crystal structure and properties of bis(isoselenocyanato-κn)tetrakis(pyridine-κn)nickel(ii) |
topic | Research Communications |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9912460/ https://www.ncbi.nlm.nih.gov/pubmed/36793409 http://dx.doi.org/10.1107/S2056989023000245 |
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