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

Electronic and Steric Influences of Pendant Amine Groups on the Protonation of Molybdenum Bis(dinitrogen) Complexes

Journal Article · Tue Apr 14 00:00:00 EDT 2015 · Inorganic Chemistry

DOI:https://doi.org/10.1021/acs.inorgchem.5b00209· OSTI ID:1385619

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

Pacific Northwest National Lab. (PNNL), Richland, WA (United States). Physical Sciences Division, Center for Molecular Electrocatalysis
Washington State Univ., Pullman, WA (United States). Dept. of Chemistry

In this paper, 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 $^i$Pr) 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 triflic acid (HOTf) to trans-Mo(N₂)₂(PMePh₂)₂(P^EtP^NRR') complexes in tetrahydrofuran 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 monoaryl-substituted pendant amines are protonated at Mo and the pendant amine site 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 is additionally protonated at a pendant amine site. In addition, trans-Mo(N₂)₂(PMePh₂)₂(depe) (depe = Et₂PCH₂CH₂PEt₂) was synthesized to serve as a counterpart lacking pendant amines. Treatment of this complex with HOTf generated a monocationic Mo(NNH₂) product. Protonolysis experiments conducted on several complexes in this study afforded trace amounts of NH₄⁺. Computational analysis 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 differences in their reactivity profiles.

View Accepted Manuscript (DOE)

Research Organization:: Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). National Energy Research Scientific Computing Center (NERSC); Pacific Northwest National Laboratory (PNNL), Richland, WA (United States). Center for Molecular Electrocatalysis (CME)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)

Contributing Organization:: Energy Frontier Research Centers (EFRC)

Grant/Contract Number:: AC05-76RL01830

OSTI ID:: 1385619

Alternate ID(s):: OSTI ID: 1208742
OSTI ID: 1210734

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

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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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
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Electronic and Steric Influences of Pendant Amine Groups on the Protonation of Molybdenum Bis(dinitrogen) Complexes

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