Iron(II) complexes of 2,6-di(1H-pyrazol-3-yl)-pyridine derivatives with hydrogen bonding and sterically bulky substituents

Thomas D. Roberts,^a   Marc A. Little,^a  Laurence J. Kershaw Cook^a and   Malcolm A. Halcrow*^a  

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Dalton Trans., 2014, Advance Article

DOI: 10.1039/C4DT00355A
Received 03 Feb 2014, Accepted 30 Mar 2014
First published online 31 Mar 2014

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Syntheses of 2,6-di(5-aminopyrazol-3-yl)pyridine (L¹), 2,6-di(5-tertbutylcarboxamidopyrazol-3-yl)pyridine (L²), 2,6-di(5-tertbutylpyrazol-3-yl)pyridine (L³), 2-(5-tertbutylpyrazol-3-yl)-6-(5-methylpyrazol-3-yl)pyridine (L⁴) and 2-(5-tertbutylpyrazol-3-yl)-6-(5-aminopyrazol-3-yl)pyridine (L⁵) are reported. Iron complex salts of the first four ligands were crystallographically characterised. The structures exhibit intermolecular hydrogen bonding between the cations and the anions and/or solvent, leading to a fluorite (flu) net, a 1D ladder structure, and a homochiral self-penetrating helical network related to the (10,3)-a (srs) topology. All the complexes are high-spin in the crystal, and bulk samples are also fully or predominantly high-spin at room temperature and below although two of the dried materials exhibit partial spin-state transitions on cooling.