Discrete trinuclear copper(II) compounds as building blocks: the influence of the peripheral substituents on the magnetic coupling in oxamato-bridged complexes.

Two new trinuclear copper(ii) complexes without end-capping ligands, (Bu4N)2[Cu(dmso)2{Cu(dnopba)(dmso)}2] () and (Bu4N)2[Cu(dmso)2{Cu(dcopba)(dmso)}2] () [dnopba = 4,5-dinitro-ortho-phenylenebis(oxamate), dcopba = 4,5-dichloro-ortho-phenylenebis(oxamate), Bu4N(+) = tetra-n-butylammonium and dmso = dimethylsulfoxide], were synthesized and their structures were determined by single crystal X-ray diffraction. The crystal structures of and consist of two outer bis(oxamato)(dmso)cuprate(ii) units which act as bidentate ligands toward a trans-bis(dmso)copper(ii) inner entity leading to centrosymmetric tricopper(ii) complexes with copper-copper separations across the oxamate bridges of 5.1916(3) …

Rational design of a new class of heterobimetallic molecule-based magnets: Synthesis, crystal structures, and magnetic properties of oxamato-bridged (M′=LiI and MnII; M=NiII and CoII) open-frameworks with a three-dimensional honeycomb architecture

Abstract Two new series of oxamato-bridged heterobimetallic coordination networks of general formula Li5[Li3M2(mpba)3(H2O)6] · 31H2O [M = NiII (1a) and CoII (1b)] and Li2[Mn3M2(mpba)3(H2O)6] · 22H2O [M = NiII (2a) and CoII (2b)] have been prepared from the metal-mediated self-assembly of the hexakis(bidentate), triple-stranded dinickel(II) and dicobalt(II) complexes [M2(mpba)3]8− [mpba = meta-phenylenebis(oxamato)] with either monovalent lithium(I) or divalent manganese(II) ions respectively, in water. X-ray structural analyses of 1a and 1b show an anionic three-dimensional network formed by an infinite parallel array of oxamato-bridged Li 3 I M 2 II (M = Ni and Co) hexagonal layers, which …

Crystal Engineering Applied to Modulate the Structure and Magnetic Properties of Oxamate Complexes Containing the [Cu(bpca)]+ Cation

This work deals with the crystal engineering features of four related copper(II)-based compounds with formulas {[{Cu(bpca)}2(H2ppba)]·1.33DMF·0.66DMSO}n (2), [{Cu(bpca)(H2O)}2(H2ppba)] (3), [{Cu(bpca)}2(H2ppba)]·DMSO (4), and [{Cu(bpca)}2(H2ppba)]·6H2O (5) [H4ppba = N,N′-1,4-phenylenebis(oxamic acid) and Hbpca = bis(2-pyridylcarbonyl)amide] and how their distinct molecular and crystal structures translate into their different magnetic properties. 2 and 3 were obtained through the hydrolytic reaction of the double-stranded oxamato-based dipalladium(II) paracyclophane precursor of formula [{K4(H2O)2}{Pd2(ppba)2}] (1) with the mononuclear copper(II) complex [Cu(bpca)(H2O)2]+, either in a water…

A two-dimensional oxamate- and oxalate-bridged Cu(II)Mn(II) motif: crystal structure and magnetic properties of (Bu4N)2[Mn2{Cu(opba)}2ox].

A new compound of formula (Bu4N)2[Mn2{Cu(opba)}2ox] (1) [Bu4N(+) = tetra-n-butylammonium cation, H4opba = 1,2-phenylenebis(oxamic acid), and H2ox = oxalic acid] has been synthesized and magneto-structurally investigated. The reaction of manganese(II) acetate, [Cu(opba)](2-), and ox(2-) in dimethyl sulfoxide yielded single crystals of 1. The structure of 1 consists of heterobimetallic oxamato-bridged Cu(II)Mn(II) chains which are connected through bis-bidentate oxalate coordinated to the manganese(II) ions to afford anionic heterobimetallic layers of 6(3)-hcb net topology. The layers are interleaved by n-Bu4N(+) counterions. Each copper(II) ion in 1 is four-coordinate in a square planar envi…

Towards oxalate-bridged iron(ii), cobalt(ii), nickel(ii) and zinc(ii) complexes through oxotris(oxalato)niobate(v): an open air non-oxidizing synthetic route

Four compounds with the formula [M2(dmphen)4(μ-C2O4)](ClO4)2·2dmso [M = Fe (1), Co (2) and Zn (4); dmphen = 2,9-dimethyl-1,10-phenanthroline] and [Ni2(dmphen)4(μ-C2O4)]3[NbO(C2O4)3]2·16H2O (3) have been synthesized using the tris(oxalato)oxoniobate(V) complex anion as the oxalate source, and their structures have been determined by single crystal X-ray diffraction. X-ray quality crystals of highly insoluble oxalate-bridged species were obtained by taking advantage of the slow release of oxalate by the tris(oxalato)oxoniobate(V) complex anion. The structures of 1–4 all contain oxalate-bridged dimetal(II) units with didentate dmphen molecules acting as end-cap ligands; electroneutrality is ac…

Supramolecular coordination chemistry of aromatic polyoxalamide ligands: A metallosupramolecular approach toward functional magnetic materials

Abstract The impressive potential of the metallosupramolecular approach in designing new functional magnetic materials constitutes a great scientific challenge for the chemical research community that requires an interdisciplinary collaboration. New fundamental concepts and future applications in nanoscience and nanotechnology will emerge from the study of magnetism as a supramolecular function in metallosupramolecular chemistry. Our recent work on the rich supramolecular coordination chemistry of a novel family of aromatic polyoxalamide (APOXA) ligands with first-row transition metal ions has allowed us to move one step further in the rational design of metallosupramolecular assemblies of …

Relatively strong intramolecular antiferromagnetic coupling in a neutral Cr(III)2Nb(V)2 heterobimetallic molecular square.

A relatively large antiferromagnetic interaction between the two chromium(III) ions from the molecular square [{Cr(dmso)4}2{Nb(μ-O)2(C2O4)2}2] () (J = -12.0 cm(-1)) is mediated by the diamagnetic oxo-Nb(V)-oxo pathway, its nature and magnitude being substantiated by DFT type theoretical calculations.

A heterobimetallic [MnII5CuII5] nanowheel modulated by a flexible bis-oxamate type ligand

The synthesis, crystal structure and preliminary magnetic characterization of a new heterobimetallic [MnII5CuII5] wheel containing a flexible bis-oxamate type ligand are described. This decanuclear compound exhibits a relatively strong intra-wheel antiferromagnetic interaction leading to a ground spin state S = 10.

Monitoring the hydrogen bond net configuration and the dimensionality of aniline and phenyloxamate by adding 1 H -pyrazole and isoxazole as substituents for molecular self-recognition

This work describes the synthesis and characterization of a new class of oxamic acid derivatives containing pyrazole and isoxazole as substituents to investigate their ability to form hydrogen bonds aiming at applying them in crystal engineering and molecular self-recognition. In this respect, we report a new synthesis of 2-(4-nitrophenyl)-1,3-propanedial (1) in high yield using SOCl2 as a chlorinating agent. The new oxamic esters 4-(1H-pyrazol-4-yl)phenylene-N-(ethyloxamate) (2d) and 4-(1,2-oxazol-4-yl)phenylene-N-(ethyloxamate) (3d) were prepared from 1. The synthetic route consists of the cyclisation of 1 either with hydrazine to afford 4-(-aminophenyl)-1H-pyrazole (2a) or with hydroxyla…

Crystal Structure and Magnetic Properties of an Oxamato‐Bridged Heterobimetallic Tetranuclear [Ni II Cu II ] 2 Complex of the Rack Type

Palladium(II)–Copper(II) Assembling with Bis(2-pyridylcarbonyl)amidate and Bis(oxamate) Type Ligands

Five new complexes of formula K4[Pd2(mpba)2] · 4H2O (1), {[K4(H2O)(dmso)][Pd2(mpba)2]} (2), {[Cu(bpca)]4[Pd2(mpba)2]} · 6H2O (3), {[Cu(bpca)]2[Pd(opba)]} · 1.75dmso · 0.25H2O (4), {[Cu(bpca)]2[Pd(opba)]}n · ndmso (5) [H4mpba =1,3-phenylenebis(oxamic acid), H4opba = 1,2-phenylenebis(oxamic acid), Hbpca = bis(2-pyridylcarbonyl)amide, and dmso = dimethyl sulfoxide] have been prepared and investigated by infrared spectroscopy, thermal analysis, single crystal X-ray diffraction, and magnetic susceptibility techniques. The structure of 2 consists of a [Pd2(mpba)2]4– anionic entity in which the palladium(II) cations are coordinated by two mpba ligands resulting in a dipalladium(II) unit that acts …

A hybrid catalyst for decontamination of organic pollutants based on a bifunctional dicopper(II) complex anchored over niobium oxyhydroxide

Abstract This article describes the preparation and characterization of a hybrid oxidation catalyst for decontamination of organic pollutants which involves a bifunctional dicopper(II) complex and the niobium(V) oxyhydroxide as the active species, the later one being also a solid support. The pH range for the existence of the active species was determined by potentiometric and UV–vis spectroscopy at 25 °C and 0.15 M NaCl in a H 2 O/EtOH (70:30 v/v) solvent mixture containing copper(II) and the ligand N , N -2,2′-ethylenediphenylenebis(oxamic acid) (H 4 L). As far as the hybrid material is concerned, FTIR, FT-Raman, TEM and SEM images, surface area and TG/DTA analyses showed the occurrence o…

Building-up host-guest helicate motifs and chains: a magneto-structural study of new field-induced cobalt-based single-ion magnets.

In this work, we present the synthetic pathway, a refined structural description, complete solid-state characterization and the magnetic properties of four new cobalt(II) compounds of formulas [Co(H2O)6][Co2(H2mpba)3]·2H2O·0.5dmso (1), [Co(H2O)6][Co2(H2mpba)3]·3H2O·0.5dpss (2), [Co2(H2mpba)2(H2O)4]n·4nH2O (3), and [Co2(H2mpba)2(CH3OH)2(H2O)2]n·0.5nH2O·2ndpss (4) [dpss = 2,2′-dipyridyldisulfide and H4mpba = 1,3-phenylenebis(oxamic) acid], where 2 and 4 were obtained from [Co(dpss)Cl2] (Pre-I) as the source of cobalt(II). All four compounds are air-stable and were prepared under ambient conditions. 1 and 2 were obtained from a slow diffusion method [cobalt(II) : H2mpba2− molar ratio used 1 : …

Oxotris(oxalato)niobate(V) as counterion in cobalt(II) spin-crossover systems

Abstract This work is devoted to the investigation of the thermally induced spin-crossover behavior from a high-spin state (HS, S = 3/2) at higher temperatures to a low-spin phase (LS, S = 1/2) at lower temperatures of the six-coordinate cobalt(II) complex in the compound [Co(terpy)2]3[NbO(C2O4)3]2·3CH​3OH·4H2O (2). The crystal structure of 2 together with that of its counterion as tetraphenylarsonium(V) salt (AsPh4)3[NbO(C2O4)3]·9H2O (1) are also included. The spin-crossover process was followed by the thermal variation of the χMT product between 2.0 and 400 K under the warming mode, with the LS configuration being achieved at T ⩽ 200 K and the LS → HS interconversion being incomplete at 4…

A CuIICoII Metallacyclophane-Based Metamagnet with a Corrugated Brick-Wall Sheet Architecture

Oxotris(oxalate)niobate(V): An oxalate delivery agent in the design of building blocks

This work concerns the oxalate delivery process that occurs when using (NH4)3[NbO(C2O4)3]·6H2O as a suitable oxalate source in the synthesis of two compounds, [Cu(dmphen)(C2O4)(H2O)] (1) and [{Cu(dmphen)(CH3OH)}2(μ-C2O4)](ClO4)2 (2) (dmphen = 2,9-dimethyl-1,10-phenanthroline). {[Fe{HB(pz)3}(CN)2(μ-CN)]2[{Cu(dmphen)}2(μ-C2O4)]}∙xCH3OH (3) (2.0 ≤ x ≤ 2.4) was obtained by reacting 2 and PPh4[Fe{HB(pz)3}(CN)3]∙H2O [ = tetraphenylphosphonium and = tris(pyrazolyl)borate]. Crystal structures of 1–3 have been determined by single-crystal X-ray diffraction experiments: 1 is a mononuclear trigonal bipyramidal copper(II) species, 2 is a centrosymmetric oxalato-bridged dicopper(II) complex, and 3 consi…

Solvent effects on the dimensionality of oxamato-bridged manganese(II) compounds

Two new oxamate-containing manganese(II) complexes, [{Mn(H2edpba)(H2O)2}2]n (1) and [Mn(H2edpba)(dmso)2]∙dmso∙CH3COCH3∙H2O (2) (H4edpba = N,N′-ethylenediphenylenebis(oxamic acid) and dmso = dimethylsulfoxide), have been synthesized and the structures of 1 and 2 were characterized by single crystal X-ray diffraction. The structure of 1 consists of neutral honeycomb networks in which each manganese(II) is six-coordinate by one H2edpba2− ligand and two carboxylate–oxygens from two other H2edpba2− ligands building the equatorial plane. Each manganese is connected to its nearest neighbor through two carboxylate(monoprotonated oxamate) bridges in an anti-syn conformation. A dmso solution of singl…

Solvent-driven dimensionality control in molecular systems containing CuII, 2,2′-bipyridine and an oxamato-based ligand

A discrete dicopper(II) system, [Cu(bipy)(H2mpba)]2·2H2O (1), and its isomeric chain, [Cu(bipy)(H2mpba)]·dmso (2) [bipy = 2,2′-bipyridine and H4mpba = N,N′-1,3-phenylenebis(oxamic acid)], were obtained by modifying the ratio of the H2O–dmso solvent mixture, and their interconversion was also monitored by changing the solvents during the synthesis. The solvents play an essential role in the formation and crystallization of these complexes, presenting different dimensionalities and connectivities. The double deprotonated H2mpba2− adopts the bidentate/monodentate (1) and bis-bidentate (2) bridging modes toward the (2,2′-bipyridyl)copper(II) units affording a dinuclear compound (1) and a linear…

Unexpected formation of a dodecanuclear {CoII6CuII6} nanowheel under ambient conditions: magneto-structural correlations.

We report the unique heterobimetallic dodecanuclear oxamate-based {CoII6CuII6} nanowheel obtained using an environmentally friendly synthetic protocol. The effective Hamiltonian methodology employed herein allows the rationalisation of magnetic isotropic or anisotropic metal clusters, being a significant advance for future studies of exciting properties only observed at low and ultralow temperatures.

Cover Feature: Design of Magnetic Coordination Polymers Built from Polyoxalamide Ligands: A Thirty Year Story (Eur. J. Inorg. Chem. 3‐4/2018)

Influence of Copper(II) and Nickel(II) Ions in the Topology of Systems Based on a Flexible Bis-Oxamate and Bipyridine Building Blocks

Single crystals of the mononuclear bis-oxamate nickel(II) complex [Ni(bipy)(H2edpba)]·dmso (1) are obtained by reacting [Ni(bipy)Cl2]·H2O and the flexible K2(H2edpba) ligand [bipy = 2,2′-bipyridine; H4edpba = N,N′-2,2′-ethylenediphenylenebis(oxamic acid)]. The reaction of 1 with copper(II) ions resulted in two products in which the replacement of the nickel(II) ion by copper(II) took place: the chain compound [Cu(bipy)(H2edpba)]n·3nH2O·ndmso [dmso = dimethyl sulfoxide] (2) and the analogous chain compound without dmso crystallization molecules [Cu(bipy)(H2edpba)]n·1.5nH2O (3a) in its polycrystalline form. The reaction of [Cu(bipy)Cl2] and K2(H2edpba) yielded single crystals of [Cu(bipy)(H2e…

Design of Magnetic Coordination Polymers Built from Polyoxalamide Ligands: A Thirty Year Story

International audience; The aim of this review is to pay tribute to the legacy of O. Kahn. Kahn's credo was to synthesize magnetic compounds with predictable structure and magnetic properties. This is illustrated herein with results obtained by Kahn's group during his Orsay period thirty years ago, but also on the basis of our recent results on the synthesis of coordination polymers with oxamate ligands. The first part of this review is devoted to a short description of the necessary knowledge in physics and theoretical chemistry that Kahn and his group have used to select oxamate ligands, the complex‐as‐ligand strategy and the synthesis of heterobimetallic systems. Then, we describe the st…

A pH-triggered bistable copper(II) metallacycle as a reversible emulsion switch for biphasic processes.

A unique bistable copper-metallacyclic complex is used as an elegant molecular switch for the reversible formation of emulsions by simple pH variation. This switch may have several exciting applications in biphasic processes such as catalysis and separation science technologies.

A Metallacryptand-Based Manganese(II)–Cobalt(II) Ferrimagnet with a Three-Dimensional Honeycomb Open-Framework Architecture

Magneto‐Structural Study of an Oxamato‐Bridged Pd II Co II Chain: X‐ray Crystallographic Evidence of a Single‐Crystal‐to‐Single‐Crystal Phase Transition

Two new mononuclear oxamato-containing palladium(II) complexes of formula K2[Pd(opba)]·2H2O (1) and (PPh4)2[Pd(opba)]·2H2O (2) and the heterodimetallic palladium(II)–cobalt(II) chain {[Co(H2O)2Pd(opba)]·dmso}n (3) [opba = 1,2-phenylenebis(oxamate), PPh4+ = tetraphenylphosphonium cation and dmso = dimethyl sulfoxide] have been prepared, and the structures of two of them (compounds 2 and 3) were determined by X-ray diffraction analysis of single crystals. The structure of 2 consists of discrete anions of [Pd(opba)2]2– and PPh4+ cations. Each PdII ion in 2 is surrounded by two oxamate nitrogen atoms and two carboxylate oxygen atoms in a square-planar surrounding. Compound 3 is a neutral chain …

CCDC 1016163: Experimental Crystal Structure Determination

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CCDC 1469224: Experimental Crystal Structure Determination

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CCDC 1818142: Experimental Crystal Structure Determination

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CCDC 1830425: Experimental Crystal Structure Determination

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CCDC 1034456: Experimental Crystal Structure Determination

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CCDC 1469225: Experimental Crystal Structure Determination

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CCDC 1958348: Experimental Crystal Structure Determination

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CCDC 1843195: Experimental Crystal Structure Determination

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CCDC 1830430: Experimental Crystal Structure Determination

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CCDC 951253: Experimental Crystal Structure Determination

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CCDC 1843197: Experimental Crystal Structure Determination

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CCDC 1883575: Experimental Crystal Structure Determination

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CCDC 923163: Experimental Crystal Structure Determination

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CCDC 2002706: Experimental Crystal Structure Determination

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CCDC 1031230: Experimental Crystal Structure Determination

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CCDC 1958349: Experimental Crystal Structure Determination

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CCDC 951150: Experimental Crystal Structure Determination

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CCDC 1402554: Experimental Crystal Structure Determination

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CCDC 942308: Experimental Crystal Structure Determination

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CCDC 1402553: Experimental Crystal Structure Determination

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CCDC 1883574: Experimental Crystal Structure Determination

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CCDC 1469223: Experimental Crystal Structure Determination

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CCDC 1883576: Experimental Crystal Structure Determination

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CCDC 1469222: Experimental Crystal Structure Determination

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CCDC 1818144: Experimental Crystal Structure Determination

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CCDC 927505: Experimental Crystal Structure Determination

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CCDC 1818143: Experimental Crystal Structure Determination

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CCDC 1034455: Experimental Crystal Structure Determination

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