Hydrogen Atom Abstraction from an OsII(NH3)2 Complex Generates an OsIV(NH2)2 Complex: Experimental and Computational Analysis of the N–H Bond Dissociation Free Energies and Reactivity

Dunn, Peter L.; Barona-Mosquera, Melissa; Johnson, Samantha I.; Raugei, Simone; Bullock, R. Morris

doi:10.1021/acs.inorgchem.2c00708

Hydrogen Atom Abstraction from an Os^II(NH₃)₂ Complex Generates an Os^IV(NH₂)₂ Complex: Experimental and Computational Analysis of the N–H Bond Dissociation Free Energies and Reactivity

Journal Article · Mon Sep 19 00:00:00 EDT 2022 · Inorganic Chemistry

DOI:https://doi.org/10.1021/acs.inorgchem.2c00708· OSTI ID:1893322

^[1]; Barona-Mosquera, Melissa ^[1]; ^[1]; ^[1]; ^[1]

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

We report double hydrogen atom abstraction from (TMP)Os^II(NH₃)₂ (TMP = tetramesitylporphyrin) with phenoxyl or nitroxyl radicals leads to (TMP)Os^IV(NH₂)₂. This unusual bis(amide) complex is diamagnetic and displays an N-H resonance at 12.0 ppm in its ¹H NMR spectrum. ¹H-¹⁵N correlation experiments identified a ¹⁵N NMR spectroscopic resonance at –267 ppm. Experimental reactivity studies and density functional theory calculations support relatively weak N-H bonds of 73.3 kcal/mol for (TMP)Os^II(NH³)² and 74.2 kcal/mol for (TMP)Os^III(NH₃)(NH₂). Cyclic voltammetry experiments provide an estimate of the pK_a of [(TMP)Os^III(NH₃)₂]⁺. In the presence of Barton’s base, a current enhancement is observed at the Os(III/II) couple, consistent with an ECE event. Spectroscopic experiments confirmed (TMP)Os^IV(NH₂)₂ as the product of bulk electrolysis. Double hydrogen atom abstraction is influenced by π donation from the amides of (TMP)Os^IV(NH₂)₂ into the d orbitals of the Os center, favoring the formation of (TMP)Os^IV(NH₂)₂ over N-N coupling. This π donation leads to a Jahn-Teller distortion that splits the energy levels of the d_xz and d_yz orbitals of Os, results in a low spin electron configuration, and leads to minimal aminyl character on the N atoms, rendering (TMP)Os^IV(NH₂)₂ unreactive towards amide-amide coupling.

View Accepted Manuscript (DOE)

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

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

Grant/Contract Number:: AC05-76RL01830

OSTI ID:: 1893322

Report Number(s):: PNNL-SA-170965

Journal Information:: Inorganic Chemistry, Journal Name: Inorganic Chemistry Journal Issue: 39 Vol. 61; ISSN 0020-1669

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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Hydrogen Atom Abstraction from an Os^II(NH₃)₂ Complex Generates an Os^IV(NH₂)₂ Complex: Experimental and Computational Analysis of the N–H Bond Dissociation Free Energies and Reactivity