Synthesis, crystal structure and properties of tetrakis(pyridine-3-carbonitrile)dithiocyanatoiron(II) and of diaquabis(pyridine-3-carbonitrile)dithiocyanatoiron(II) pyridine-3-carbonitrile monosolvate

The reaction of iron thiocyanate with 3-cyanopyridine (C6H4N2) leads to the formation of two compounds with the composition [Fe(NCS)2(C6H4N2)4] (1) and [Fe(NCS)2(C6H4N2)2(H2O)2]·2C6H4N2 (2). The asymmetric unit of 1 consists of one iron cation, two thiocyanate anions and four 3-cyanopyridine ligands...

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Main Authors: Christian Näther, Asmus Müller-Meinhard, Inke Jess
Format: Article
Language:English
Published: International Union of Crystallography 2023-11-01
Series:Acta Crystallographica Section E: Crystallographic Communications
Subjects:
Online Access:http://scripts.iucr.org/cgi-bin/paper?S205698902300909X
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author Christian Näther
Asmus Müller-Meinhard
Inke Jess
author_facet Christian Näther
Asmus Müller-Meinhard
Inke Jess
author_sort Christian Näther
collection DOAJ
description The reaction of iron thiocyanate with 3-cyanopyridine (C6H4N2) leads to the formation of two compounds with the composition [Fe(NCS)2(C6H4N2)4] (1) and [Fe(NCS)2(C6H4N2)2(H2O)2]·2C6H4N2 (2). The asymmetric unit of 1 consists of one iron cation, two thiocyanate anions and four 3-cyanopyridine ligands in general positions. The iron cation is octahedrally coordinated by two N-bonded thiocyanate anions and four 3-cyanopyridine ligands. The complexes are arranged in columns along the crystallographic c-axis direction and are linked by weak C—H...N interactions. In 2, the asymmetric unit consists of one iron cation on a center of inversion as well as one thiocyanate anion, one 3-cyanopyridine ligand, one water ligand and one 3-cyanopyridine solvate molecule in general positions. The iron cation is octahedrally coordinated by two N-bonded thiocyanate anions, two cyanopyridine ligands and two water ligands. O—H...N and C—H...S hydrogen bonding is observed between the water ligands and the solvent 3-cyanopyridine molecules. In the crystal structure, alternating layers of the iron complexes and the solvated 3-cyanopyridine molecules are observed. Powder X-ray (PXRD) investigations reveal that both compounds were obtained as pure phases and from IR spectroscopic measurements conclusions on the coordination mode of the thiocanate anions and the cyanogroup were made. Thermogravimetric (TG) and differential thermoanalysis (DTA) of 1 indicate the formation of a compound with the composition {[Fe(NCS)2]3(C6H4N2)4}n that is isotypic to the corresponding Cd compound already reported in the literature. TG/DTA of 2 show several mass losses. The first mass loss corresponds to the removal of the two water ligands leading to the formation of 1, which transforms into {[Fe(NCS)2]3(C6H4N2)4}n, upon further heating.
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spelling doaj.art-cd83ef7cbb6f4cf393e21e46e42a1d492023-11-06T14:46:42ZengInternational Union of CrystallographyActa Crystallographica Section E: Crystallographic Communications2056-98902023-11-0179111093109910.1107/S205698902300909Xhb8079Synthesis, crystal structure and properties of tetrakis(pyridine-3-carbonitrile)dithiocyanatoiron(II) and of diaquabis(pyridine-3-carbonitrile)dithiocyanatoiron(II) pyridine-3-carbonitrile monosolvateChristian Näther0Asmus Müller-Meinhard1Inke Jess2Institut für Anorganische Chemie, Universität Kiel, Max-Eyth.-Str. 2, 24118 Kiel, GermanyInstitut für Anorganische Chemie, Universität Kiel, Max-Eyth.-Str. 2, 24118 Kiel, GermanyInstitut für Anorganische Chemie, Universität Kiel, Max-Eyth.-Str. 2, 24118 Kiel, GermanyThe reaction of iron thiocyanate with 3-cyanopyridine (C6H4N2) leads to the formation of two compounds with the composition [Fe(NCS)2(C6H4N2)4] (1) and [Fe(NCS)2(C6H4N2)2(H2O)2]·2C6H4N2 (2). The asymmetric unit of 1 consists of one iron cation, two thiocyanate anions and four 3-cyanopyridine ligands in general positions. The iron cation is octahedrally coordinated by two N-bonded thiocyanate anions and four 3-cyanopyridine ligands. The complexes are arranged in columns along the crystallographic c-axis direction and are linked by weak C—H...N interactions. In 2, the asymmetric unit consists of one iron cation on a center of inversion as well as one thiocyanate anion, one 3-cyanopyridine ligand, one water ligand and one 3-cyanopyridine solvate molecule in general positions. The iron cation is octahedrally coordinated by two N-bonded thiocyanate anions, two cyanopyridine ligands and two water ligands. O—H...N and C—H...S hydrogen bonding is observed between the water ligands and the solvent 3-cyanopyridine molecules. In the crystal structure, alternating layers of the iron complexes and the solvated 3-cyanopyridine molecules are observed. Powder X-ray (PXRD) investigations reveal that both compounds were obtained as pure phases and from IR spectroscopic measurements conclusions on the coordination mode of the thiocanate anions and the cyanogroup were made. Thermogravimetric (TG) and differential thermoanalysis (DTA) of 1 indicate the formation of a compound with the composition {[Fe(NCS)2]3(C6H4N2)4}n that is isotypic to the corresponding Cd compound already reported in the literature. TG/DTA of 2 show several mass losses. The first mass loss corresponds to the removal of the two water ligands leading to the formation of 1, which transforms into {[Fe(NCS)2]3(C6H4N2)4}n, upon further heating.http://scripts.iucr.org/cgi-bin/paper?S205698902300909Xcrystal structureiron thiocyanate3-cyanopyridinethermal propertiesir spectrum
spellingShingle Christian Näther
Asmus Müller-Meinhard
Inke Jess
Synthesis, crystal structure and properties of tetrakis(pyridine-3-carbonitrile)dithiocyanatoiron(II) and of diaquabis(pyridine-3-carbonitrile)dithiocyanatoiron(II) pyridine-3-carbonitrile monosolvate
Acta Crystallographica Section E: Crystallographic Communications
crystal structure
iron thiocyanate
3-cyanopyridine
thermal properties
ir spectrum
title Synthesis, crystal structure and properties of tetrakis(pyridine-3-carbonitrile)dithiocyanatoiron(II) and of diaquabis(pyridine-3-carbonitrile)dithiocyanatoiron(II) pyridine-3-carbonitrile monosolvate
title_full Synthesis, crystal structure and properties of tetrakis(pyridine-3-carbonitrile)dithiocyanatoiron(II) and of diaquabis(pyridine-3-carbonitrile)dithiocyanatoiron(II) pyridine-3-carbonitrile monosolvate
title_fullStr Synthesis, crystal structure and properties of tetrakis(pyridine-3-carbonitrile)dithiocyanatoiron(II) and of diaquabis(pyridine-3-carbonitrile)dithiocyanatoiron(II) pyridine-3-carbonitrile monosolvate
title_full_unstemmed Synthesis, crystal structure and properties of tetrakis(pyridine-3-carbonitrile)dithiocyanatoiron(II) and of diaquabis(pyridine-3-carbonitrile)dithiocyanatoiron(II) pyridine-3-carbonitrile monosolvate
title_short Synthesis, crystal structure and properties of tetrakis(pyridine-3-carbonitrile)dithiocyanatoiron(II) and of diaquabis(pyridine-3-carbonitrile)dithiocyanatoiron(II) pyridine-3-carbonitrile monosolvate
title_sort synthesis crystal structure and properties of tetrakis pyridine 3 carbonitrile dithiocyanatoiron ii and of diaquabis pyridine 3 carbonitrile dithiocyanatoiron ii pyridine 3 carbonitrile monosolvate
topic crystal structure
iron thiocyanate
3-cyanopyridine
thermal properties
ir spectrum
url http://scripts.iucr.org/cgi-bin/paper?S205698902300909X
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