Journal
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION
Volume 54, Issue 5, Pages 1499-1503Publisher
WILEY-V C H VERLAG GMBH
DOI: 10.1002/anie.201409676
Keywords
cyclophanes; dinitrogen activation; iron clusters; macrobicycles; redox cooperativity
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Funding
- University of Florida
- ACS Petroleum Research Fund [ACS-PRF 52704-DNI3]
- NSF departmental instrumentation award [CHE-1048604]
- NSF [CHE-0821346]
- UF
- Labex ARCANE [ANR-11-LABX-0003-01]
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Reaction of a trinuclear iron(II) complex, Fe3Br3L (1), with KC8 under N-2 leads to dinitrogen activation products (2) from which Fe-3(NH)(3)L (2-1; L is a cyclophane bridged by three beta-diketiminate arms) was characterized by X-ray crystallography. H-1 NMR spectra of the protonolysis product of 2 synthesized under N-14(2) and N-15(2) confirm atmospheric N-2 reduction, and ammonia is detected by the indophenol assay (yield similar to 30%). IR and Mossbauer spectroscopy, and elemental analysis on 2 and 2-1 as well as the tri(amido)triiron(II) 3 and tri(methoxo)triiron 4 congeners support our assignment of the reduction product as containing protonated N-atom bridges.
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