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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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Autores principales: Näther, Christian, Boeckmann, Jan
Formato: Online Artículo Texto
Lenguaje:English
Publicado: International Union of Crystallography 2023
Materias:
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.
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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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