Molecular Catalysts with Intramolecular Re–O Bond for Electrochemical Reduction of Carbon Dioxide

Rotundo, Laura; Polyansky, Dmitry E.; Gobetto, Roberto; Grills, David C.; Fujita, Etsuko; Nervi, Carlo; Manbeck, Gerald F.

doi:10.1021/acs.inorgchem.0c01181

Title: Molecular Catalysts with Intramolecular Re–O Bond for Electrochemical Reduction of Carbon Dioxide

Journal Article · Mon Aug 17 00:00:00 EDT 2020 · Inorganic Chemistry

DOI:https://doi.org/10.1021/acs.inorgchem.0c01181· OSTI ID:1766356

Rotundo, Laura ^[1]; Polyansky, Dmitry E. ^[2];

^[1];

^[2];

^[1];

^[2]

Chemistry Department, University of Torino, Via P. Giuria 7, 10125 Torino, Italy, CIRCC (Bari), University of Bari, Via Celso Ulpiani 27, 70126 Bari, Italy
Chemistry Division, Brookhaven National Laboratory, Upton, New York 11973-5000, United States

A new Re bipyridine-type complex, namely, fac-Re(pmbpy)(CO)₃Cl (pmbpy = 4-phenyl-6-(2-hydroxy-phenyl)-2,2'-bipyridine), 1, carrying a single OH moiety as local proton source, has been synthesized, and its electrochemical behavior under Ar and under CO₂ has been characterized. Two isomers of 1, namely, 1-cis characterized by the proximity of Cl to OH and 1-trans, are identified. The interconversion between 1-cis and 1-trans is clarified by DFT calculations, which reveal two transition states. The energetically lower pathway displays a non-negligible barrier of 75.5 kJ mol^–1. The 1e^– electrochemical reduction of 1 affords the neutral intermediate 1-OPh, formally derived by reductive deprotonation and loss of Cl^– from 1. 1-OPh, which exhibits an entropically favored intramolecular Re–O bond, has been isolated and characterized. The detailed electrochemical mechanism is demonstrated by combined chemical reactivity, spectroelectrochemistry, spectroscopic (IR and NMR), and computational (DFT) approaches. Comparison with previous Re and Mn derivatives carrying local proton sources highlights that the catalytic activity of Re complexes is more sensitive to the presence of local OH groups. Similar to Re-2OH (2OH = 4-phenyl-6-(phenyl-2,6-diol)-2,2'-bipyridine), 1 and Mn-1OH display a selective reduction of CO₂ to CO. In the case of the Re bipyridine-type complex, the formation of a relatively stable Re–O bond and a preference for phenolate-based reactivity with CO₂ slightly inhibit the electrocatalytic reduction of CO₂ to CO, resulting in a low TON value of 9, even in the presence of phenol as a proton source.

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Research Organization:: Brookhaven National Laboratory (BNL), Upton, NY (United States)

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

Grant/Contract Number:: SC0012704

OSTI ID:: 1766356

Alternate ID(s):: OSTI ID: 1661651

Report Number(s):: BNL-219841-2020-JAAM

Journal Information:: Inorganic Chemistry, Journal Name: Inorganic Chemistry Vol. 59 Journal Issue: 17; ISSN 0020-1669

Publisher:: American Chemical SocietyCopyright Statement

Country of Publication:: United States

Language:: English

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Redox reactions
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Electrolysis
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Title: Molecular Catalysts with Intramolecular Re–O Bond for Electrochemical Reduction of Carbon Dioxide

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