<i>N</i>-Oxide Coordination to Mn(III) Chloride

We report on the synthesis and characterization of Mn(III) chloride (Mn<sup>III</sup>Cl<sub>3</sub>) complexes coordinated with <i>N</i>-oxide ylide ligands, namely trimethyl-<i>N</i>-oxide (Me<sub>3</sub>NO) and pyridine-<i>N</i&g...

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Main Authors: Ananya Saju, Matthew R. Crawley, Samantha N. MacMillan, Pierre Le Magueres, Mark Del Campo, David C. Lacy
Format: Article
Language:English
Published: MDPI AG 2024-10-01
Series:Molecules
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Online Access:https://www.mdpi.com/1420-3049/29/19/4670
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author Ananya Saju
Matthew R. Crawley
Samantha N. MacMillan
Pierre Le Magueres
Mark Del Campo
David C. Lacy
author_facet Ananya Saju
Matthew R. Crawley
Samantha N. MacMillan
Pierre Le Magueres
Mark Del Campo
David C. Lacy
author_sort Ananya Saju
collection DOAJ
description We report on the synthesis and characterization of Mn(III) chloride (Mn<sup>III</sup>Cl<sub>3</sub>) complexes coordinated with <i>N</i>-oxide ylide ligands, namely trimethyl-<i>N</i>-oxide (Me<sub>3</sub>NO) and pyridine-<i>N</i>-oxide (PyNO). The compounds are reactive and, while isolable in the solid-state at room temperature, readily decompose into Mn(II). For example, “[Mn<sup>III</sup>Cl<sub>3</sub>(ONMe<sub>3</sub>)<sub>n</sub>]” decomposes into the 2D polymeric network compound complex salt [Mn<sup>II</sup>(µ-Cl)<sub>3</sub>Mn<sup>II</sup>(µ-ONMe<sub>3</sub>)]<sub>n</sub>[Mn<sup>II</sup>(µ-Cl)<sub>3</sub>]<sub>n</sub>·(Me<sub>3</sub>NO·HCl)<sub>3n</sub> (<b>4</b>). The reaction of Mn<sup>III</sup>Cl<sub>3</sub> with PyNO forms varied Mn(III) compounds with PyNO coordination and these react with hexamethylbenzene (HMB) to form the chlorinated organic product 1-cloromethyl-2,3,4,5,6-pentamethylbenzene (<b>8</b>). In contrast to <i>N</i>-oxide coordination to Mn(III), the reaction between [Mn<sup>III</sup>Cl<sub>3</sub>(OPPh<sub>3</sub>)<sub>2</sub>] and 2,2,6,6-tetramethyl-1-piperidinyloxy (TEMPO) resulted in electron transfer-forming <i>d</i><sup>5</sup> manganate of the [TEMPO] cation instead of TEMPO–Mn(III) adducts. The reactivity affected by <i>N</i>-oxide coordination is discussed through comparisons with other L–Mn<sup>III</sup>Cl<sub>3</sub> complexes within the context of reduction potential.
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spelling doaj-art-d45e5cdcfd2d4d70909aa0fb5e5b787a2025-08-20T02:16:54ZengMDPI AGMolecules1420-30492024-10-012919467010.3390/molecules29194670<i>N</i>-Oxide Coordination to Mn(III) ChlorideAnanya Saju0Matthew R. Crawley1Samantha N. MacMillan2Pierre Le Magueres3Mark Del Campo4David C. Lacy5Department of Chemistry, University at Buffalo, State University of New York, Buffalo, NY 14260, USADepartment of Chemistry, University at Buffalo, State University of New York, Buffalo, NY 14260, USADepartment of Chemistry and Chemical Biology, Cornell University, Ithaca, NY 14853, USARigaku Americas, The Woodlands, TX 77381, USARigaku Americas, The Woodlands, TX 77381, USADepartment of Chemistry, University at Buffalo, State University of New York, Buffalo, NY 14260, USAWe report on the synthesis and characterization of Mn(III) chloride (Mn<sup>III</sup>Cl<sub>3</sub>) complexes coordinated with <i>N</i>-oxide ylide ligands, namely trimethyl-<i>N</i>-oxide (Me<sub>3</sub>NO) and pyridine-<i>N</i>-oxide (PyNO). The compounds are reactive and, while isolable in the solid-state at room temperature, readily decompose into Mn(II). For example, “[Mn<sup>III</sup>Cl<sub>3</sub>(ONMe<sub>3</sub>)<sub>n</sub>]” decomposes into the 2D polymeric network compound complex salt [Mn<sup>II</sup>(µ-Cl)<sub>3</sub>Mn<sup>II</sup>(µ-ONMe<sub>3</sub>)]<sub>n</sub>[Mn<sup>II</sup>(µ-Cl)<sub>3</sub>]<sub>n</sub>·(Me<sub>3</sub>NO·HCl)<sub>3n</sub> (<b>4</b>). The reaction of Mn<sup>III</sup>Cl<sub>3</sub> with PyNO forms varied Mn(III) compounds with PyNO coordination and these react with hexamethylbenzene (HMB) to form the chlorinated organic product 1-cloromethyl-2,3,4,5,6-pentamethylbenzene (<b>8</b>). In contrast to <i>N</i>-oxide coordination to Mn(III), the reaction between [Mn<sup>III</sup>Cl<sub>3</sub>(OPPh<sub>3</sub>)<sub>2</sub>] and 2,2,6,6-tetramethyl-1-piperidinyloxy (TEMPO) resulted in electron transfer-forming <i>d</i><sup>5</sup> manganate of the [TEMPO] cation instead of TEMPO–Mn(III) adducts. The reactivity affected by <i>N</i>-oxide coordination is discussed through comparisons with other L–Mn<sup>III</sup>Cl<sub>3</sub> complexes within the context of reduction potential.https://www.mdpi.com/1420-3049/29/19/4670Mn(III)<i>N</i>-oxide ligandscoordination chemistryC–H chlorination
spellingShingle Ananya Saju
Matthew R. Crawley
Samantha N. MacMillan
Pierre Le Magueres
Mark Del Campo
David C. Lacy
<i>N</i>-Oxide Coordination to Mn(III) Chloride
Molecules
Mn(III)
<i>N</i>-oxide ligands
coordination chemistry
C–H chlorination
title <i>N</i>-Oxide Coordination to Mn(III) Chloride
title_full <i>N</i>-Oxide Coordination to Mn(III) Chloride
title_fullStr <i>N</i>-Oxide Coordination to Mn(III) Chloride
title_full_unstemmed <i>N</i>-Oxide Coordination to Mn(III) Chloride
title_short <i>N</i>-Oxide Coordination to Mn(III) Chloride
title_sort i n i oxide coordination to mn iii chloride
topic Mn(III)
<i>N</i>-oxide ligands
coordination chemistry
C–H chlorination
url https://www.mdpi.com/1420-3049/29/19/4670
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