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4. The Fe 2 (NO) 2 Diamond Core: A Unique Structural Motif In Non‐Heme Iron–NO Chemistry

   https://doi.org/10.1002/ange.201911968  

   Dong, Hai T. ; Speelman, Amy L. ; Kozemchak, Claire E. ; Sil, Debangsu ; Krebs, Carsten ; Lehnert, Nicolai ( October 2019 , Angewandte Chemie)

   Non‐heme high‐spin (hs) {FeNO}⁸complexes have been proposed as important intermediates towards N₂O formation in flavodiiron NO reductases (FNORs). Many hs‐{FeNO}⁸complexes disproportionate by forming dinitrosyl iron complexes (DNICs), but the mechanism of this reaction is not understood. While investigating this process, we isolated a new type of non‐heme iron nitrosyl complex that is stabilized by an unexpected spin‐state change. Upon reduction of the hs‐{FeNO}⁷complex, [Fe(TPA)(NO)(OTf)](OTf) (1), the N‐O stretching band vanishes, but no sign of DNIC or N₂O formation is observed. Instead, the dimer, [Fe₂(TPA)₂(NO)₂](OTf)₂(2) could be isolated and structurally characterized. We propose that2is formed from dimerization of the hs‐{FeNO}⁸intermediate, followed by a spin state change of the iron centers to low‐spin (ls), and speculate that2models intermediates in hs‐{FeNO}⁸complexes that precede the disproportionation reaction.

    

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5. The Fe 2 (NO) 2 Diamond Core: A Unique Structural Motif In Non‐Heme Iron–NO Chemistry

   https://doi.org/10.1002/anie.201911968  

   Dong, Hai T. ; Speelman, Amy L. ; Kozemchak, Claire E. ; Sil, Debangsu ; Krebs, Carsten ; Lehnert, Nicolai ( October 2019 , Angewandte Chemie International Edition)

   Non‐heme high‐spin (hs) {FeNO}⁸complexes have been proposed as important intermediates towards N₂O formation in flavodiiron NO reductases (FNORs). Many hs‐{FeNO}⁸complexes disproportionate by forming dinitrosyl iron complexes (DNICs), but the mechanism of this reaction is not understood. While investigating this process, we isolated a new type of non‐heme iron nitrosyl complex that is stabilized by an unexpected spin‐state change. Upon reduction of the hs‐{FeNO}⁷complex, [Fe(TPA)(NO)(OTf)](OTf) (1), the N‐O stretching band vanishes, but no sign of DNIC or N₂O formation is observed. Instead, the dimer, [Fe₂(TPA)₂(NO)₂](OTf)₂(2) could be isolated and structurally characterized. We propose that2is formed from dimerization of the hs‐{FeNO}⁸intermediate, followed by a spin state change of the iron centers to low‐spin (ls), and speculate that2models intermediates in hs‐{FeNO}⁸complexes that precede the disproportionation reaction.

    

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