Photolytic activation of Ni(II)X2L explains how Ni-mediated cross coupling begins

Abstract Nickel photocatalysis has recently become vital to organic synthesis, but how the Ni(II)X2L pre-catalyst (X = Cl, Br; L = bidentate ligand) becomes activated to Ni(I)XL has remained puzzling and is typically addressed on a case-by-case basis. Here, we reveal a general mechanism where light...

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Main Authors: Max Kudisch, Reagan X. Hooper, Lakshmy K. Valloli, Justin D. Earley, Anna Zieleniewska, Jin Yu, Stephen DiLuzio, Rebecca W. Smaha, Hannah Sayre, Xiaoyi Zhang, Matthew J. Bird, Amy A. Cordones, Garry Rumbles, Obadiah G. Reid
Format: Article
Language:English
Published: Nature Portfolio 2025-07-01
Series:Nature Communications
Online Access:https://doi.org/10.1038/s41467-025-60729-x
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author Max Kudisch
Reagan X. Hooper
Lakshmy K. Valloli
Justin D. Earley
Anna Zieleniewska
Jin Yu
Stephen DiLuzio
Rebecca W. Smaha
Hannah Sayre
Xiaoyi Zhang
Matthew J. Bird
Amy A. Cordones
Garry Rumbles
Obadiah G. Reid
author_facet Max Kudisch
Reagan X. Hooper
Lakshmy K. Valloli
Justin D. Earley
Anna Zieleniewska
Jin Yu
Stephen DiLuzio
Rebecca W. Smaha
Hannah Sayre
Xiaoyi Zhang
Matthew J. Bird
Amy A. Cordones
Garry Rumbles
Obadiah G. Reid
author_sort Max Kudisch
collection DOAJ
description Abstract Nickel photocatalysis has recently become vital to organic synthesis, but how the Ni(II)X2L pre-catalyst (X = Cl, Br; L = bidentate ligand) becomes activated to Ni(I)XL has remained puzzling and is typically addressed on a case-by-case basis. Here, we reveal a general mechanism where light induces photolysis of the Ni(II)-X bond, either via direct excitation or triplet energy transfer. Photolysis produces Ni(I)XL and a halogen radical, X•. Subsequent hydrogen atom abstraction, often from the solvent, produces a C(sp3) radical, R•, that recombines with Ni(I) to form organonickel(II) complexes, Ni(II)XRL. Rather than acting as a loss pathway, Ni(II)XRL behaves as a light-activated reservoir of Ni(I) via photolysis of the Ni(II)-C bond. These results explain the role of the solvent in protecting the catalyst from off-cycle dimerization, demonstrate that two photons are often required to drive the reaction, and show how tuning the ligand can control the concentration of active Ni(I) species.
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spelling doaj-art-89c92e14144d4c46bd733b5a4f91a1c82025-08-20T03:45:34ZengNature PortfolioNature Communications2041-17232025-07-0116111110.1038/s41467-025-60729-xPhotolytic activation of Ni(II)X2L explains how Ni-mediated cross coupling beginsMax Kudisch0Reagan X. Hooper1Lakshmy K. Valloli2Justin D. Earley3Anna Zieleniewska4Jin Yu5Stephen DiLuzio6Rebecca W. Smaha7Hannah Sayre8Xiaoyi Zhang9Matthew J. Bird10Amy A. Cordones11Garry Rumbles12Obadiah G. Reid13Chemistry and Nanoscience, National Renewable Energy LaboratoryStanford PULSE Institute, SLAC National Accelerator LaboratoryBrookhaven National LaboratoryChemistry and Nanoscience, National Renewable Energy LaboratoryChemistry and Nanoscience, National Renewable Energy LaboratoryAdvanced Photon Source, Argonne National LaboratoryDepartment of Chemistry and Chemical Biology, Northeastern UniversityMaterials Science, National Renewable Energy LaboratoryDepartment of Chemistry and Chemical Biology, Northeastern UniversityAdvanced Photon Source, Argonne National LaboratoryBrookhaven National LaboratoryStanford PULSE Institute, SLAC National Accelerator LaboratoryChemistry and Nanoscience, National Renewable Energy LaboratoryChemistry and Nanoscience, National Renewable Energy LaboratoryAbstract Nickel photocatalysis has recently become vital to organic synthesis, but how the Ni(II)X2L pre-catalyst (X = Cl, Br; L = bidentate ligand) becomes activated to Ni(I)XL has remained puzzling and is typically addressed on a case-by-case basis. Here, we reveal a general mechanism where light induces photolysis of the Ni(II)-X bond, either via direct excitation or triplet energy transfer. Photolysis produces Ni(I)XL and a halogen radical, X•. Subsequent hydrogen atom abstraction, often from the solvent, produces a C(sp3) radical, R•, that recombines with Ni(I) to form organonickel(II) complexes, Ni(II)XRL. Rather than acting as a loss pathway, Ni(II)XRL behaves as a light-activated reservoir of Ni(I) via photolysis of the Ni(II)-C bond. These results explain the role of the solvent in protecting the catalyst from off-cycle dimerization, demonstrate that two photons are often required to drive the reaction, and show how tuning the ligand can control the concentration of active Ni(I) species.https://doi.org/10.1038/s41467-025-60729-x
spellingShingle Max Kudisch
Reagan X. Hooper
Lakshmy K. Valloli
Justin D. Earley
Anna Zieleniewska
Jin Yu
Stephen DiLuzio
Rebecca W. Smaha
Hannah Sayre
Xiaoyi Zhang
Matthew J. Bird
Amy A. Cordones
Garry Rumbles
Obadiah G. Reid
Photolytic activation of Ni(II)X2L explains how Ni-mediated cross coupling begins
Nature Communications
title Photolytic activation of Ni(II)X2L explains how Ni-mediated cross coupling begins
title_full Photolytic activation of Ni(II)X2L explains how Ni-mediated cross coupling begins
title_fullStr Photolytic activation of Ni(II)X2L explains how Ni-mediated cross coupling begins
title_full_unstemmed Photolytic activation of Ni(II)X2L explains how Ni-mediated cross coupling begins
title_short Photolytic activation of Ni(II)X2L explains how Ni-mediated cross coupling begins
title_sort photolytic activation of ni ii x2l explains how ni mediated cross coupling begins
url https://doi.org/10.1038/s41467-025-60729-x
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