Electronic and steric influences of pendant amine groups on the protonation of molybdenum bis (dinitrogen) complexes

Labios, Liezel A.; Heiden, Zachariah M.; Mock, Michael T.

doi:10.1021/acs.inorgchem.5b00209

Title: Electronic and steric influences of pendant amine groups on the protonation of molybdenum bis (dinitrogen) complexes

Journal Article · Mon May 04 00:00:00 EDT 2015 · Inorganic Chemistry

DOI:https://doi.org/10.1021/acs.inorgchem.5b00209· OSTI ID:1208742

Labios, Liezel A. ^[1]; Heiden, Zachariah M. ^[2]; Mock, Michael T. ^[1]

Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
Washington State Univ., Pullman, WA (United States)

The synthesis of a series of P^EtP^NRR' (P^EtP^NRR' = Et₂PCH₂CH₂P(CH₂NRR')₂, R = H, R' = Ph or 2,4-difluorophenyl; R = R' = Ph or ⁱPr) diphosphine ligands containing mono- and disubstituted pendant amine groups, and the preparation of their corresponding molybdenum bis(dinitrogen) complexes trans-Mo(N₂)₂(PMePh₂)₂(P^EtP^NRR') is described. In situ IR and multinuclear NMR spectroscopic studies monitoring the stepwise addition of (HOTf) to trans-Mo(N₂)₂(PMePh₂)₂(P^EtP^NRR') complexes in THF at -40 °C show that the electronic and steric properties of the R and R' groups of the pendant amines influence whether the complexes are protonated at Mo, a pendant amine, a coordinated N2 ligand, or a combination of these sites. For example, complexes containing mono-aryl substituted pendant amines are protonated at Mo and pendant amine to generate mono- and dicationic Mo–H species. Protonation of the complex containing less basic diphenyl-substituted pendant amines exclusively generates a monocationic hydrazido (Mo(NNH₂)) product, indicating preferential protonation of an N₂ ligand. Addition of HOTf to the complex featuring more basic diisopropyl amines primarily produces a monocationic product protonated at a pendant amine site, as well as a trace amount of dicationic Mo(NNH₂) product that contain protonated pendant amines. In addition, trans-Mo(N₂)₂(PMePh₂)₂(depe) (depe = Et₂PCH₂CH₂PEt₂) without a pendant amine was synthesized and treated with HOTf, generating a monocationic Mo(NNH₂) product. Protonolysis experiments conducted on select complexes in the series afforded trace amounts of NH₄⁺. Computational analysis of the series of trans-Mo(N₂)₂(PMePh₂)₂(P^EtP^NRR') complexes provides further insight into the proton affinity values of the metal center, N₂ ligand, and pendant amine sites to rationalize the differing reactivity profiles. This research was supported as part of the Center for Molecular Electrocatalysis, an Energy Frontier Research Center funded by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences. Computational resources provided by the National Energy Research Scientific Computing Center (NERSC) at Lawrence Berkeley National Laboratory. Pacific Northwest National Laboratory is operated by Battelle for the U.S. Department of Energy.

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Research Organization:: Pacific Northwest National Laboratory (PNNL), Richland, WA (United States)

Sponsoring Organization:: USDOE

DOE Contract Number:: AC05-76RL01830

OSTI ID:: 1208742

Report Number(s):: PNNL-SA-107233; KC0307010

Journal Information:: Inorganic Chemistry, Vol. 54, Issue 9; ISSN 0020-1669

Publisher:: American Chemical Society (ACS)

Country of Publication:: United States

Language:: English

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CCDC 1063284: Experimental Crystal Structure Determination Labios, Liezel A.; Heiden, Zachariah M.; Mock, Michael T. https://doi.org/10.5517/cc14pfhr The current record is supplemented by this dataset	dataset	January 2015
CCDC 1063287: Experimental Crystal Structure Determination Labios, Liezel A.; Heiden, Zachariah M.; Mock, Michael T. https://doi.org/10.5517/cc14pflv The current record is supplemented by this dataset	dataset	January 2015
CCDC 1063288: Experimental Crystal Structure Determination Labios, Liezel A.; Heiden, Zachariah M.; Mock, Michael T. https://doi.org/10.5517/cc14pfmw The current record is supplemented by this dataset	dataset	January 2015
CCDC 1063285: Experimental Crystal Structure Determination Labios, Liezel A.; Heiden, Zachariah M.; Mock, Michael T. https://doi.org/10.5517/cc14pfjs The current record is supplemented by this dataset	dataset	January 2015
CCDC 1063286: Experimental Crystal Structure Determination Labios, Liezel A.; Heiden, Zachariah M.; Mock, Michael T. https://doi.org/10.5517/cc14pfkt The current record is supplemented by this dataset	dataset	January 2015