Ultrasound-assisted synthesis of water-soluble monosubstituted diruthenium compounds

The elusive monosubstituted diruthenium complexes [Ru2Cl(DAniF)(O2CMe)3] (1), [Ru2Cl(DPhF)(O2CMe)3] (2), [Ru2Cl(D-p-CNPhF)(O2CMe)3] (3), [Ru2Cl(D-o-TolF)(O2CMe)3] (4), [Ru2Cl(D-m-TolF)(O2CMe)3] (5), [Ru2Cl(D-p-TolF)(O2CMe)3] (6) and [Ru2Cl(p-TolA)(O2CMe)3] (7) have been synthesized using for the fir...

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Autores principales: Aarón Terán, Miguel Cortijo, Ángel Gutiérrez, Ana E. Sánchez-Peláez, Santiago Herrero, Reyes Jiménez-Aparicio
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Publicado: Elsevier 2021
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spelling oai:doaj.org-article:0b1823fb103d4d76905622db056b17bd2021-12-02T04:59:53ZUltrasound-assisted synthesis of water-soluble monosubstituted diruthenium compounds1350-417710.1016/j.ultsonch.2021.105828https://doaj.org/article/0b1823fb103d4d76905622db056b17bd2021-12-01T00:00:00Zhttp://www.sciencedirect.com/science/article/pii/S1350417721003709https://doaj.org/toc/1350-4177The elusive monosubstituted diruthenium complexes [Ru2Cl(DAniF)(O2CMe)3] (1), [Ru2Cl(DPhF)(O2CMe)3] (2), [Ru2Cl(D-p-CNPhF)(O2CMe)3] (3), [Ru2Cl(D-o-TolF)(O2CMe)3] (4), [Ru2Cl(D-m-TolF)(O2CMe)3] (5), [Ru2Cl(D-p-TolF)(O2CMe)3] (6) and [Ru2Cl(p-TolA)(O2CMe)3] (7) have been synthesized using for the first time ultrasound-assisted synthesis to carry out a substitution reaction in metal–metal bonded dinuclear compounds (DAniF− = N,N′-bis(4-anisyl)formamidinate; DPhF− = N,N′-diphenylformamidinate; D-p-CNPhF− = N,N′-bis(4-cyanophenyl)formamidinate; D-o/m/p-TolF− = N,N′-bis(2/3/4-tolyl)formamidinate; p-TolA− = N-4-tolylamidate). This is a simpler and greener method than the tedious procedures described in the literature, and it has permitted to obtain water-soluble complexes with good yields in a short period of time. A synthetic study has been implemented to find the best experimental conditions to prepare compounds 1–7. Two different types of ligands, formamidinate and amidate, have been used to check the generality of the method for the preparation of monosubstituted complexes. Five new compounds (2–6) have been obtained using a formamidinate ligand, the synthesis of the previously described compound 1 has been improved, and an unprecedented monoamidate complex has been achieved (7). The crystal structures of compounds 3 and 7 have been solved by single crystal X-ray diffraction. These compounds show the typical paddlewheel structure with three acetate ligands and one formamidinate (3) or amidate (7) bridging ligand at the equatorial positions. The axial positions are occupied by the chloride ligand giving rise to one-dimensional polymer structures that were previously unknown for monosubstituted compounds.Aarón TeránMiguel CortijoÁngel GutiérrezAna E. Sánchez-PeláezSantiago HerreroReyes Jiménez-AparicioElsevierarticleSonochemistrySubstitution reactionDiruthenium compoundsWater-soluble compoundsChemistryQD1-999Acoustics. SoundQC221-246ENUltrasonics Sonochemistry, Vol 80, Iss , Pp 105828- (2021)
institution DOAJ
collection DOAJ
language EN
topic Sonochemistry
Substitution reaction
Diruthenium compounds
Water-soluble compounds
Chemistry
QD1-999
Acoustics. Sound
QC221-246
spellingShingle Sonochemistry
Substitution reaction
Diruthenium compounds
Water-soluble compounds
Chemistry
QD1-999
Acoustics. Sound
QC221-246
Aarón Terán
Miguel Cortijo
Ángel Gutiérrez
Ana E. Sánchez-Peláez
Santiago Herrero
Reyes Jiménez-Aparicio
Ultrasound-assisted synthesis of water-soluble monosubstituted diruthenium compounds
description The elusive monosubstituted diruthenium complexes [Ru2Cl(DAniF)(O2CMe)3] (1), [Ru2Cl(DPhF)(O2CMe)3] (2), [Ru2Cl(D-p-CNPhF)(O2CMe)3] (3), [Ru2Cl(D-o-TolF)(O2CMe)3] (4), [Ru2Cl(D-m-TolF)(O2CMe)3] (5), [Ru2Cl(D-p-TolF)(O2CMe)3] (6) and [Ru2Cl(p-TolA)(O2CMe)3] (7) have been synthesized using for the first time ultrasound-assisted synthesis to carry out a substitution reaction in metal–metal bonded dinuclear compounds (DAniF− = N,N′-bis(4-anisyl)formamidinate; DPhF− = N,N′-diphenylformamidinate; D-p-CNPhF− = N,N′-bis(4-cyanophenyl)formamidinate; D-o/m/p-TolF− = N,N′-bis(2/3/4-tolyl)formamidinate; p-TolA− = N-4-tolylamidate). This is a simpler and greener method than the tedious procedures described in the literature, and it has permitted to obtain water-soluble complexes with good yields in a short period of time. A synthetic study has been implemented to find the best experimental conditions to prepare compounds 1–7. Two different types of ligands, formamidinate and amidate, have been used to check the generality of the method for the preparation of monosubstituted complexes. Five new compounds (2–6) have been obtained using a formamidinate ligand, the synthesis of the previously described compound 1 has been improved, and an unprecedented monoamidate complex has been achieved (7). The crystal structures of compounds 3 and 7 have been solved by single crystal X-ray diffraction. These compounds show the typical paddlewheel structure with three acetate ligands and one formamidinate (3) or amidate (7) bridging ligand at the equatorial positions. The axial positions are occupied by the chloride ligand giving rise to one-dimensional polymer structures that were previously unknown for monosubstituted compounds.
format article
author Aarón Terán
Miguel Cortijo
Ángel Gutiérrez
Ana E. Sánchez-Peláez
Santiago Herrero
Reyes Jiménez-Aparicio
author_facet Aarón Terán
Miguel Cortijo
Ángel Gutiérrez
Ana E. Sánchez-Peláez
Santiago Herrero
Reyes Jiménez-Aparicio
author_sort Aarón Terán
title Ultrasound-assisted synthesis of water-soluble monosubstituted diruthenium compounds
title_short Ultrasound-assisted synthesis of water-soluble monosubstituted diruthenium compounds
title_full Ultrasound-assisted synthesis of water-soluble monosubstituted diruthenium compounds
title_fullStr Ultrasound-assisted synthesis of water-soluble monosubstituted diruthenium compounds
title_full_unstemmed Ultrasound-assisted synthesis of water-soluble monosubstituted diruthenium compounds
title_sort ultrasound-assisted synthesis of water-soluble monosubstituted diruthenium compounds
publisher Elsevier
publishDate 2021
url https://doaj.org/article/0b1823fb103d4d76905622db056b17bd
work_keys_str_mv AT aaronteran ultrasoundassistedsynthesisofwatersolublemonosubstituteddirutheniumcompounds
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AT anaesanchezpelaez ultrasoundassistedsynthesisofwatersolublemonosubstituteddirutheniumcompounds
AT santiagoherrero ultrasoundassistedsynthesisofwatersolublemonosubstituteddirutheniumcompounds
AT reyesjimenezaparicio ultrasoundassistedsynthesisofwatersolublemonosubstituteddirutheniumcompounds
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