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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...
Autores principales: | , |
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Formato: | Online Artículo Texto |
Lenguaje: | English |
Publicado: |
International Union of Crystallography
2023
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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 |
Sumario: | 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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