Characterization of an Fe≡N–NH 2 intermediate relevant to catalytic N2 reduction to NH3
Abstract
The ability of certain transition metals to mediate the reduction of N2 to NH3 has attracted broad interest in the biological and inorganic chemistry communities. Early transition metals such as Mo and W readily bind N2 and mediate its protonation at one or more N atoms to furnish M(NxHy) species that can be characterized and, in turn, extrude NH3. By contrast, the direct protonation of Fe–N2 species to Fe(NxHy) products that can be characterized has been elusive. In this paper, we show that addition of acid at low temperature to [(TPB)Fe(N2)][Na(12-crown-4)] results in a new S = 1/2 Fe species. EPR, ENDOR, Mössbauer, and EXAFS analysis, coupled with a DFT study, unequivocally assign this new species as [(TPB)Fe≡N–NH2]+, a doubly protonated hydrazido(2–) complex featuring an Fe-to-N triple bond. This unstable species offers strong evidence that the first steps in Fe-mediated nitrogen reduction by [(TPB)Fe(N2)][Na(12-crown-4)] can proceed along a distal or “Chatt-type” pathway. Finally, a brief discussion of whether subsequent catalytic steps may involve early or late stage cleavage of the N–N bond, as would be found in limiting distal or alternating mechanisms, respectively, is also provided.
- Authors:
-
- California Inst. of Technology (CalTech), Pasadena, CA (United States)
- Northwestern Univ., Evanston, IL (United States)
- Northwestern Univ., Evanston, IL (United States); Illinois College, Jacksonville, IL (United States)
- California Inst. of Technology (CalTech), Pasadena, CA (United States); Univ. of Nebraska, Lincoln, NE (United States)
- Publication Date:
- Research Org.:
- California Institute of Technology (CalTech), Pasadena, CA (United States); Northwestern Univ., Evanston, IL (United States)
- Sponsoring Org.:
- USDOE Office of Science (SC), Biological and Environmental Research (BER); National Inst. of Health (NIH) (United States); National Science Foundation (NSF)
- OSTI Identifier:
- 1347701
- Grant/Contract Number:
- MCB-1118613; DGE-0824162; GM 070757; GM 111097; P41GM103393; P31RR001209
- Resource Type:
- Accepted Manuscript
- Journal Name:
- Journal of the American Chemical Society
- Additional Journal Information:
- Journal Volume: 137; Journal Issue: 24; Journal ID: ISSN 0002-7863
- Publisher:
- American Chemical Society (ACS)
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
Citation Formats
Anderson, John S., Cutsail, III, George E., Rittle, Jonathan, Connor, Bridget A., Gunderson, William A., Zhang, Limei, Hoffman, Brian M., and Peters, Jonas C. Characterization of an Fe≡N–NH 2 intermediate relevant to catalytic N2 reduction to NH3. United States: N. p., 2015.
Web. doi:10.1021/jacs.5b03432.
Anderson, John S., Cutsail, III, George E., Rittle, Jonathan, Connor, Bridget A., Gunderson, William A., Zhang, Limei, Hoffman, Brian M., & Peters, Jonas C. Characterization of an Fe≡N–NH 2 intermediate relevant to catalytic N2 reduction to NH3. United States. https://doi.org/10.1021/jacs.5b03432
Anderson, John S., Cutsail, III, George E., Rittle, Jonathan, Connor, Bridget A., Gunderson, William A., Zhang, Limei, Hoffman, Brian M., and Peters, Jonas C. Fri .
"Characterization of an Fe≡N–NH 2 intermediate relevant to catalytic N2 reduction to NH3". United States. https://doi.org/10.1021/jacs.5b03432. https://www.osti.gov/servlets/purl/1347701.
@article{osti_1347701,
title = {Characterization of an Fe≡N–NH 2 intermediate relevant to catalytic N2 reduction to NH3},
author = {Anderson, John S. and Cutsail, III, George E. and Rittle, Jonathan and Connor, Bridget A. and Gunderson, William A. and Zhang, Limei and Hoffman, Brian M. and Peters, Jonas C.},
abstractNote = {The ability of certain transition metals to mediate the reduction of N2 to NH3 has attracted broad interest in the biological and inorganic chemistry communities. Early transition metals such as Mo and W readily bind N2 and mediate its protonation at one or more N atoms to furnish M(NxHy) species that can be characterized and, in turn, extrude NH3. By contrast, the direct protonation of Fe–N2 species to Fe(NxHy) products that can be characterized has been elusive. In this paper, we show that addition of acid at low temperature to [(TPB)Fe(N2)][Na(12-crown-4)] results in a new S = 1/2 Fe species. EPR, ENDOR, Mössbauer, and EXAFS analysis, coupled with a DFT study, unequivocally assign this new species as [(TPB)Fe≡N–NH2]+, a doubly protonated hydrazido(2–) complex featuring an Fe-to-N triple bond. This unstable species offers strong evidence that the first steps in Fe-mediated nitrogen reduction by [(TPB)Fe(N2)][Na(12-crown-4)] can proceed along a distal or “Chatt-type” pathway. Finally, a brief discussion of whether subsequent catalytic steps may involve early or late stage cleavage of the N–N bond, as would be found in limiting distal or alternating mechanisms, respectively, is also provided.},
doi = {10.1021/jacs.5b03432},
journal = {Journal of the American Chemical Society},
number = 24,
volume = 137,
place = {United States},
year = {Fri May 22 00:00:00 EDT 2015},
month = {Fri May 22 00:00:00 EDT 2015}
}
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