Crystal structure of dichlorido(4,11-dimethyl-1,4,8,11-tetraazabicyclo[6.6.2]hexadecane)iron(III) hexafluoridophosphate

Funwie, Neil L.; Cain, Amy N.; Fanning, Brian Z.; Hageman, Serena A.; Mullens, Malorie; Roberts, Travis K.; Turner, Daniel J.; Valdez, Cammi N.; Vaughan, Robert W.; Ermias, Henok G.; Silversides, Jon D.; Archibald, Stephen J.; Hubin, Timothy J.; Prior, Timothy J.

Abstract

The title compound, [FeCl₂(C₁₄H₃₀N₄)]PF₆, contains Fe³⁺ coordinated by the four nitro­gen atoms of an ethyl­ene cross-bridged cyclam macrocycle and two cis chloride ligands in a distorted octa­hedral environment. In contrast to other similar compounds this is a monomer. Inter­molecular C-H...Cl inter­actions exist in the structure between the complex ions. Comparison with the mononuclear Fe²⁺ complex of the same ligand shows that the smaller Fe³⁺ ion is more fully engulfed by the cavity of the bicyclic ligand. Comparison with the μ-oxido dinuclear complex of an unsubstituted ligand of the same size demonstrates that the methyl groups of 4,11-dimethyl-1,4,8,11-tetra­aza­bicyclo­[6.6.2]hexa­decane prevent dimerization upon oxidation.

Citation

Funwie, N. L., Cain, A. N., Fanning, B. Z., Hageman, S. A., Mullens, M., Roberts, T. K., Turner, D. J., Valdez, C. N., Vaughan, R. W., Ermias, H. G., Silversides, J. D., Archibald, S. J., Hubin, T. J., & Prior, T. J. (2015). Crystal structure of dichlorido(4,11-dimethyl-1,4,8,11-tetraazabicyclo[6.6.2]hexadecane)iron(III) hexafluoridophosphate. Acta Crystallographica Section E: Crystallographic Communications, 71(9), 1073-1076. https://doi.org/10.1107/S2056989015015340

• Journal Article Type: Article
• Acceptance Date: Aug 17, 2015
• Online Publication Date: Aug 26, 2015
• Publication Date: Sep 1, 2015
• Deposit Date: Oct 1, 2015
• Publicly Available Date: Nov 23, 2017
• Journal: Acta crystallographica. Section E
• Print ISSN: 2056-9890
• Publisher: International Union of Crystallography
• Peer Reviewed: Peer Reviewed
• Volume: 71
• Issue: 9
• Pages: 1073-1076
• DOI: https://doi.org/10.1107/S2056989015015340
• Keywords: Crystal structure, Macrocycle, Cross bridge, Iron, Cylam
• Public URL: https://hull-repository.worktribe.com/output/379417
• Publisher URL: http://scripts.iucr.org/cgi-bin/paper?S2056989015015340
• Additional Information: Copy of article published in: Acta crystallographica. Section E, 2005, v.71
• Contract Date: Nov 23, 2017