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Breaking New Ground towards Innovative Synthesis of Palladacycles: The Electrochemical Synthesis of a Tetranuclear Thiosemicarbazone-[,,] Palladium(II) Complex.
Molecules
September 2024
Department of Inorganic Chemistry, University of Santiago de Compostela, E-15782 Santiago de Compostela, Spain.
The electrochemical oxidation of anodic metals (M = nickel and palladium) in an acetonitrile solution of the thiosemicarbazone ligands ()-2-(1-(4-methoxyphenyl)ethylidene)-N-methylhydrazine-1-carbothioamide (a), ()-2-(1-(p-tolyl)ethylidene)hydrazine-1-carbothioamide (b), and ()-N-phenyl-2-(1-(p-tolyl)ethylidene)hydrazine-1-carbothioamide (c) yielded the homoleptic complexes [ML], , , , and and [ML], as air-stable solids. The crystal structures for , , , and show the ligands in a transoid disposition with the [S,S] and [N,N] donor atom pairs occupying positions on the nearly square planar coordination plane of the metal. The structure for of S4 symmetry comprises a tetranuclear palladacycle where the metalated ligands are arranged around a central PdS environment: a crown ring with alternating palladium and sulfur atoms.
View Article and Find Full Text PDFRetrosynthetic Analysis Applied to Clip-off Chemistry: Synthesis of Four Rh(II)-Based Complexes as Proof-of-Concept.
Angew Chem Int Ed Engl
November 2023
Catalan Institute of Nanoscience and Nanotechnology (ICN2), CSIC and The Barcelona Institute of Science and Technology, Campus UAB, Bellaterra, 08193, Barcelona, Spain.
Clip-off Chemistry is a synthetic strategy that our group previously developed to obtain new molecules and materials through selective cleavage of bonds. Herein, we report recent work to expand Clip-off Chemistry by introducing into it a retrosynthetic analysis step that, based on virtual extension of the products through cleavable bonds, enables one to define the required precursor materials. As proof-of-concept, we have validated our new approach by synthesising and characterising four aldehyde-functionalised Rh(II)-based complexes: a homoleptic cluster; a cis-disubstituted paddlewheel cluster; a macrocycle; and a crown.
View Article and Find Full Text PDFSyntheses and crystal structures of new naphthalene- and anthracene-vanadate salts and an unprecedented dimetallabis(anthracene) sandwich complex: [Na(tetrahydrofuran)][V(anthracene)].
Acta Crystallogr C Struct Chem
March 2022
Department of Chemistry, 207 Pleasant Street SE, University of Minnesota, Minneapolis, MN 55455, USA.
Reduction of bis(naphthalene)vanadium(0) by potassium naphthalene (KNp) in tetrahydrofuran (THF) provides a highly reactive, thermolabile, and so far unisolable brown substance, which affords the first reported derivatives of bis(naphthalene)vanadates. From these solutions, thermally stable (298 K) and structurally characterized compounds have been obtained, including dark-red rods of catena-poly[bis(μ-η:η:η-naphthalene)tetrakis(tetrahydrofuran)dipotassiumvanadium], [KV(CHO)(CH)] or [K(THF)][V(CH)] (3), and red plates of (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.
View Article and Find Full Text PDFCrystal structures of two novel iron isocyanides from the reaction of 2,6-di-methyl-phenyl isocyanide, CNXyl, with bis-(anthracene)ferrate(-1).
Acta Crystallogr E Crystallogr Commun
January 2022
Department of Chemistry, 207 Pleasant Street SE, University of Minnesota, Minneapolis, MN 55455, USA.
The reaction of the [K(18-crown-6)(thf)] (thf is tetra-hydro-furan) salt of bis-(anthracene)ferrate(-1), or [Fe(CH)], with 2,6-di-methyl-phenyl isocyan-ide (CNX-yl) in thf resulted in the formation of two new iron isocyanide complexes, namely, [(1,2,3,4-η)-anthracene]tris-(2,6-di-methyl-phenyl isocyanide)iron, [Fe(CH)(CHN)] or [Fe(1,2,3,4-η-CH)(CNX-yl)], and {5,6-bis-(2,6-di-methyl-anilino)-3-(2,6-di-methyl-phen-yl)-1,2,7-tris-[(2,6-di-methyl-phen-yl)imino]-3-azoniahept-3-ene-1,4,7-triido}tris-(2,6-di-methyl-phenyl isocyanide)iron tetra-hydro-furan disolvate, [Fe(CHN)(CHN)]·2CHO or [Fe(CHN)(CNX-yl)]·2CHO, which were characterized by single-crystal X-ray diffraction. The former is likely an inter-mediate along the path to the known homoleptic [Fe(CNX-yl)], while the latter contains a tridentate ligand that is formed from the 'coupling' of six CNXyl ligands. A third crystal structure from this reaction, (7-methyl-indol-1-ido-κ)(1,4,7,10,13,16-hexa-oxa-cyclo-octa-decane-κ )potassium, [K(CHN)(CHO)] or [K(CHN)(18-crown-6)], contains a 7-methyl-indol-1-ide anion, in which one CNXyl ligand has shed a proton during its reductive cyclization.
View Article and Find Full Text PDFIron(II), Cobalt(II), and Nickel(II) Complexes of Bis(sulfonamido)benzenes: Redox Properties, Large Zero-Field Splittings, and Single-Ion Magnets.
Inorg Chem
March 2021
Institut für Physikalische Chemie, Universität Stuttgart, Pfaffenwaldring 55, 70569 Stuttgart, Germany.
Metal complexes of 1,2-diamidobenzenes have been long studied because of their intriguing redox properties and electronic structures. We present here a series of such complexes with 1,2-bis(sulfonamido)benzene ligands to probe the utility of these ligands for generating a large zero-field splitting (ZFS, ) in metal complexes that possibly act as single-ion magnets. To this end, we have synthesized a series of homoleptic ate complexes of the form (X)[M{bis(sulfonamido)benzene}] ( equals 4 minus the oxidation state of the metal), where M (Fe/Co/Ni), X [K/(K-18-c-6)/(HNEt), with 18-c-6 = 18-crown ether 6], and the substituents (methyl and tolyl) on the ligand [bmsab = 1,2-bis(methanesulfonamido)benzene; btsab = 1,2-bis(toluenesulfonamido)benzene] were varied to analyze their effect on the ZFS, possible single-ion-magnet properties, and redox behavior of these metal complexes.
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