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Crystal structure, synthesis and thermal properties of bis(4-benzoylpyridine-?N)bis(isothiocyanato-?N)bis(methanol-?N)iron(II).

ABSTRACT: In the crystal structure of the title compound, [Fe(NCS)2(C12H9NO)2(CH4O)2], the FeII cations are octahedrally coordinated by two N atoms of 4-benzoylpyridine ligands, two N atoms of two terminal isothiocyanate anions and two methanol molecules into discrete complexes that are located on centres of inversion. These complexes are linked via intermolecular O—H?O hydrogen bonds between the methanol O—H H atoms and the carbonyl O atoms of the 4-benzoylpyridine ligands, forming layers parallel to (101). Powder X-ray diffraction proved that a pure sample was obtained but that this compound is unstable and transforms into an unknown crystalline phase within several weeks. However, the solvent molecules can be removed by heating in a thermobalance, which for the aged sample as well as the title compound leads to the formation of a compound with the composition Fe(NCS)2(4-benzoylpyridine)2, which exhibits a powder pattern that is similar to that of Mn(NCS)2(4-benzoylpyridine)2.

SUBMITTER: Wellm C

PROVIDER: S-EPMC7001824 | biostudies-literature | 2020 Feb

REPOSITORIES: biostudies-literature

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Project description:Reaction of FeCl2·4H2O with KSCN and 3-cyano-pyridine (pyridine-3-carbo-nitrile) in ethanol accidentally leads to the formation of single crystals of Fe(NCS)(Cl)(3-cyano-pyridine)4 or [FeCl(NCS)(C6H4N2)4]. The asymmetric unit of this compound consists of one FeII cation, one chloride and one thio-cyanate anion that are located on a fourfold rotation axis as well as of one 3-cyano-pyridine coligand in a general position. The FeII cations are sixfold coordinated by one chloride anion and one terminally N-bonding thio-cyanate anion in trans-positions and four 3-cyano-pyridine coligands that coordinate via the pyridine N atom to the FeII cations. The complexes are arranged in columns with the chloride anions, with the thio-cyanate anions always oriented in the same direction, which shows the non-centrosymmetry of this structure. No pronounced inter-molecular inter-actions are observed between the complexes. Initially, FeCl2 and KSCN were reacted in a 1:2 ratio, which lead to a sample that contains the title compound as the major phase together with a small amount of an unknown crystalline phase, as proven by powder X-ray diffraction (PXRD). If FeCl2 and KSCN is reacted in a 1:1 ratio, the title compound is obtained as a nearly pure phase. IR investigations reveal that the CN stretching vibration for the thio-cyanate anion is observed at 2074 cm-1, and that of the cyano group at 2238 cm-1, which also proves that the anionic ligands are only terminally bonded and that the cyano group is not involved in the metal coordination. Measurements with thermogravimetry and differential thermoanalysis reveal that the title compound decomposes at 169°C when heated at a rate of 4°C min-1 and that the 3-cyano-pyridine ligands are emitted in two separate poorly resolved steps. After the first step, an inter-mediate compound with the composition Fe(NCS)(Cl)(3-cyano-pyridine)2 of unknown structure is formed, for which the CN stretching vibration of the thio-cyanate anion is observed at 2025 cm-1, whereas the CN stretching vibration of the cyano group remain constant. This strongly indicates that the FeII cations are linked by μ-1,3-bridg-ing thio-cyanate anions into chains or layers.

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Crystal structure, synthesis and thermal properties of bis(4-benzoylpyridine-?N)bis(isothiocyanato-?N)bis(methanol-?N)iron(II).

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Crystal structure, synthesis and thermal properties of bis­(4-benzoyl­pyridine-?N)bis­(iso­thio­cyanato-?N)bis­(methanol-?N)iron(II).

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OmicsDI is part of the ELIXIR infrastructure

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Crystal structure, synthesis and thermal properties of bis(4-benzoylpyridine-?N)bis(isothiocyanato-?N)bis(methanol-?N)iron(II).