Structure and Electronic Properties of an Expanded Terpyridine Complex of Nickel(II) [Ni(ddpd)2](BF4)2

2018

Magnetic Study of a Pentanuclear {Co 2 III Co 3 II } Cluster with a Bent {Co II 3 } Motif

2014

We have synthesised and structurally characterised a new pentanuclear mixed-valent cobalt cluster of formula [CoII3CoIII2(OH)2(piv)6(L)2(H2O)4] (piv = trimethylacetate, H2L = salicylideneanthranillic acid) from reaction of a dinuclear cobalt pivalate precursor with a Schiff base type ligand under mild reaction conditions. The core structure can be conveniently described as two fused Co3–μ3–OH triangles with a strict unique sharing vertex point. A complete picture of the magnetic behaviour of this compound is presented. Through combined use of susceptibility, magnetisation, and EPR data as well as broken-symmetry DFT calculations, we have supported the magnetic data that show weak and anisot…

{CoIII2DyIII2} single molecule magnet with two resolved thermal activated magnetization relaxation pathways at zero field

2014

The new complex [CoIII2DyIII 2(OMe)2(teaH)2(Piv)6] in the {CoIII2DyIII2} family, shows two well resolved thermal activated magnetization relaxation pathways under AC experiments in zero DC field. Fitted crystal field parameters suggest that the origin of these two pathways relies on two different excited mJ sub-levels. Fil: Funes, Víctor Alejandro. Consejo Nacional de Investigaciones Científicas y Técnicas. Oficina de Coordinación Administrativa Ciudad Universitaria. Instituto de Química, Física de los Materiales, Medioambiente y Energía. Universidad de Buenos Aires. Facultad de Ciencias Exactas y Naturales. Instituto de Química, Física de los Materiales, Medioambiente y Energía; Argentina …

Synthesis, Structural and Spectroscopic Characterization of Cr III , Fe III , Co III , Ni II and Cu II Complexes with an Asymmetric 1,3,4‐Thiadiazole…

2016

The reaction of the new asymmetric 1,3,4-thiadiazole-based ligand 2-[(5-ethylthio-1,3,4-thiadiazol-2-yl)hydrazonomethyl]phenol (H1ETHP) with various third-row transition metal salts resulted in the formation of six new mononuclear complexes [Cr(ETHP)2]ClO4 (1), [Fe(ETHP)2][FeCl4] (2), [Co(ETHP)(ETHP–H)] (3), [Ni(ETHP)(H1ETHP)]Cl (4), [Ni(ETHP)(H1ETHP)](ClO4) (5), [Ni(ETHP)(H1ETHP)]Br (6), and one tetranuclear complex [Cu2Cl3(ETHP)(H1ETHP)]2 (7). H1ETHP and all complexes have been analyzed by single crystal X-ray diffraction. Structural analysis of 1–6 reveals complexes of the [ML2]n+-type (n = 0,1), in which the mono anionic ligand ETHP coordinates in a tridentate NNO fashion via its imine,…

Inorganic Phosphate and Arsenate within New Tetranuclear Copper and Zinc Complexes: Syntheses, Crystal Structures, Magnetic, Electrochemical, and The…

2017

Three, PO43–/HPO42– and AsO43–-incorporated, new tetranuclear complexes of copper(II) and zinc(II) ions have been synthesized and fully characterized. In methanol–water, reactions of H3cpdp (H3cpdp = N,N′-Bis[2-carboxybenzomethyl]-N,N′-Bis[2-pyridylmethyl]-1,3-diaminopropan-2-ol) with copper(II) chloride in the presence of either NaOH/Na2HPO4·2H2O or KOH/Na2HAsO4·7H2O lead to the isolation of the tetranuclear complexes Na3[Cu4(cpdp)2(μ4-PO4)](OH)2·14H2O (1) and K2[Cu4(cpdp)2(μ4-AsO4)](OH)·162/3H2O (2), respectively. Similarly, the reaction of H3cpdp with zinc(II) chloride in the presence of NaOH/Na2HPO4·2H2O yields a tetranuclear complex, Na(H3O)2[Zn4(cpdp)2(μ4-HPO4)]Cl3·121/2H2O (3). All c…

Titelbild: Direct CH Metalation with Chromium(II) and Iron(II): Transition-Metal Host / Benzenediide Guest Magnetic Inverse-Crown Complexes (Angew. …

2009

Chrom und Eisen als die neuesten Erganzungen des Konzepts der alkalimetallvermittelten Metallierung stellen J. Klett, R. E. Mulvey et al. in ihrer Zuschrift auf S. 3367 ff. vor. Das elektropositivere Natrium ist wesentlich fur die Reaktion, doch das weniger elektropositive Chrom oder Eisen ist es, das Benzol tatsachlich deprotoniert. Diese neuartige Reaktivitat kann mit einem Schachspiel verglichen werden, bei dem die Konigin (Na) dem Konig Schach bietet und der Springer (Cr, Fe) Matt setzt.

Bis(μ-alkoxo) bridged dinuclear CuII2 and ZnII2 complexes of an isoindol functionality based new ligand: Synthesis, structure, spectral characterizat…

2014

Abstract Two new dinuclear copper(II) and zinc(II) complexes of an isoindol functionality based new dinucleating ligand, H3hdpa (H3hdpa = 2-({[2-hydoxyethyl]-[2-hydroxy-3-(1-oxo-1,3-dihydro-isoindol-2-yl)-propyl]-amino}-methyl)-benzoic acid) have been synthesized and characterized. In methanol, the reaction of stoichiometric amounts of Cu(OAc)2·H2O and the ligand H3hdpa in the presence of NaOH at ambient temperature afforded a new dinuclear copper(II) complex, [Cu2(Hhdpa)2]·2CH3OH·6H2O (1). Similarly, in methanol, the reaction of stoichiometric amounts of Zn(OAc)2·2H2O and H3hdpa in the presence of NaOH yielded a new dinuclear zinc(II) complex, Na4[Zn2(hdpa)2](OAc)2 (2). Characterization of…

New cyclic tetranuclear copper(II) complexes containing quadrilateral cores: Synthesis, structure, spectroscopy and their interactions with DNA in aq…

2017

Abstract Three new cyclic tetranuclear copper(II) complexes, Tetrakis{3-[(2-pyridylmethyl)-amino]-propionato}(tetrachloro)tetracopper(II)methanolhydrate (1·CH3OH·H2O), Tetrakis{3-[(2-pyridylmethyl)-amino]-propionato}(tetrathiocyanato)tetracopper(II) (2) and Tetrakis{3-[(2-pyridylmethyl)-amino]-propionato}(tetraazido)tetracopper(II) (3) have been synthesized by exploiting the chelating ability and bridging potential of a carboxyamine functionalized tridentate ligand, HL (HL = 3-[(2-Pyridylmethyl)-amino]-propionic acid). Complexes 1, 2 and 3 have been synthesized by carrying out reaction of the ligand HL with stoichiometric amounts of CuCl2·2H2O, CuCl2·2H2O/NH4SCN, and CuCl2·2H2O/NaN3, respec…

First Cobalt(II) Spin Crossover Compound with N4S2-Donorset

2020

Herein we report the synthesis and characterization of a novel bis-tridentate 1,3,4-thiadiazole ligand (L = 2,5-bis[(2-pyridylmethyl)thio]methyl-1,3,4-thiadiazole). Two new mononuclear complexes of the type [MII(L)2](ClO4)2 (with M = FeII (C1) and CoII (C2)) have been synthesized, containing the new ligand (L). In both complexes the metal centers are coordinated by an N4S2-donorset and each of the two ligands is donating to the metal ion with just one of the tridentate pockets. The iron(II) complex (C1) is in the low spin [LS] state below room temperature and shows an increase in the magnetic moment only above 300 K. In contrast, the cobalt(II) complex (C2) shows a gradual spin crossover (S…

Water‐Soluble Heteronuclear [NaCu II 6 ] Metallomacrocyclic Sandwich Complexes: Synthesis, Structure, Properties and In Vitro Biological Studies

2014

The water-soluble heteronuclear metallomacrocyclic sandwich clusters [NaCu6(hpnbpda)3(OH)3(OH2)3](NO3)·4H2O (1), [NaCu6(hpnbpda)3(OH)3(OH2)3](ClO4) (2), and [NaCu6(hpnbpda)3(OH)3(OH2)3](PF6) (3) [H3hpnbpda = N,N′-bis(2-pyridylmethyl)-2-hydroxy-1,3-propanediamine-N,N′-diacetic acid] have been synthesized in methanol at room temperature and fully characterized using several analytical techniques including single-crystal X-ray diffraction. The molecular architecture of complex 1 is built from the template assembly of three dinuclear [Cu2(hpnbpda)]+ fragments through their weak oxophillic interactions with a central sodium(I) cation. A close analysis of the single-crystal X-ray structure reveal…

Synthesis, structure and properties of new heterometallic octanuclear Li2Na2Cu4 and decanuclear Li2Zn8 complexes

2019

Abstract A carboxylate containing polydentate ligand in combination with exogeneous succinate (suc) has been used to stabilize heterometallic octanuclear [Li2Na2Cu4(cpdp)2(suc)2(CH3OH)2(H2O)4]Cl2·6H2O (1) and decanuclear Na(H3O)2[Li2Zn8(cpdp)4(suc)2(H2O)4]Cl2Br3·6MeOH·19H2O (2) complexes. The reaction of ligand H3cpdp (H3cpdp = N,N'-bis[2-carboxybenzomethyl]-N,N'-bis[2-pyridylmethyl]-1,3-diaminopropan-2-ol) with stoichiometric amounts of CuCl2/sodium succinate, and ZnCl2/sodium succinate, allowed isolation of complexes 1 and 2, respectively. Analyses of single crystal X-ray structures indicate that complex 1 is capped by two [Cu2(cpdp)]+ molecular building units and two succinate linkers, w…

Mononuclear Mn(III) and dinuclear Mn(III,III) Schiff base complexes: Influence of π–π stacking on magnetic properties

2012

Abstract Synthesis of a mononuclear Mn(III) (1) and a dinuclear Mn(III, III) (2) complex of a tetradentate N2O2 donor Schiff base ligand with ancillary carboxylate ligands are reported. Complex 1 crystallizes in the monoclinic space group C2/c, complex 2 in the triclinic space group P-1. In both complexes the central Mn(III) ions are hexacoordinated having a distorted octahedral MnN2O4 coordination environment. Intermolecular hydrogen bonding and strong π–π stacking in both 1 and 2 leads to dimerization of 1 and formation of a syn–anti one-dimensional chain for 2. Magnetic properties of 1 and 2 are reported. Both complexes show very weak intermolecular antiferromagnetic interaction. Most in…

One dimensional Mn(III) Schiff-base complex organization through very strong symmetrical H-bond interaction

2016

Abstract We are reporting the structural and magnetic characterization of a Mn(III) mononuclear complex based on a Schiff-base ligand with carboxylate pendant arm. Very strong symmetric H-interaction drives a one dimensional organization of this complex, densely packed through C–H⋯π further interactions. Low temperature magnetic behaviour appears governed by local ion zero field splitting obscuring any possible weak exchange interaction through the symmetric H-bond pathway.

Synthesis, structural characterization and magnetic behaviour of a family of [CoIII2LnIII2] butterfly compounds

2017

We have successfully prepared and structurally characterized a family of butterfly-like [Co2 IIILn2 III] complexes where all magnetic properties are due to the Ln(iii) ions. The complexes with Ln = Tb(1), Dy(2), Ho(3), Er(4) and Yb(5) are iso-structural. An exception is the complex with Ln = Gd(6) which strings in a one dimensional chain. The structural similarity together with the high tendency of the crystallites to align under an applied magnetic field allowed an overall DC magnetic data treatment to extract phenomenological crystal field parameters and hence to determine the ground state multiplet energy level splitting. The Dy(iii) member is the only one showing slow relaxation of magn…

Bis[(trimethylsilyl)methyl]manganese: Structural Variations of Its Solvent-Free and TMEDA-, Pyridine-, and Dioxane-Complexed Forms

2009

First synthesized in 1976 and recently taking on a new significance as a key precursor to heterobimetallic alkali-metal-manganese(II) complexes, bis[(trimethylsilyl)methyl] manganese has been structurally characterized by X-ray crystallography. It forms a polymeric chain structure of formula [{Mn(CH2SiMe3)(2)}(infinity)], 1, in which distorted tetrahedral, spiro Mn atoms are linked together via mu(2)-bonding alkyl ligands. The structure is notable for displaying two distinct categories of Mn-C bond lengths with a mean size differential of 0.225 angstrom and for being the first fully crystallographically characterized polymeric manganese(II) dialkyl compound. Magnetic measurements of 1 indic…

Exploring the Slow Relaxation of the Magnetization in CoIII -Decorated {DyIII 2 } Units

2016

We have prepared and structurally characterized a new member of the butterfly-like {CoIII 2DyIII 2} single-molecule magnets (SMMs) through further CoIIIdecoration, with the formula [CoIII 4DyIII 2(OH)2(teaH)2(tea)2(Piv)6] (teaH3=triethanolamine; Piv=trimethylacetate or pivalate). Direct current (DC) susceptibility and magnetization measurements were performed allowing the extraction of possible crystal-field parameters. A simple electrostatic modeling shows reasonable agreement with experimental data. Alternating current (AC) susceptibility measurements under a zero DC field and under small applied fields were performed at different frequencies (i.e., 10–1500 Hz) and at low temperatures (i.…

Titelbild: Luminescence and Light‐Driven Energy and Electron Transfer from an Exceptionally Long‐Lived Excited State of a Non‐Innocent Chromium(III) …

2019

Sodium-mediated manganation: direct mono- and dimanganation of benzene and synthesis of a transition-metal inverse-crown complex.

2007

Inside out approach: Twofold deprotonation of benzene by a sodium monoalkyl bisamido manganate(II) reagent derived from BuNa, 2,2,6,6-tetramethylpiperidine, and Mn(CH2SiMe3)2 has produced the first inverse-crown complex in which the transition-metal atoms are incorporated in the host (see X-ray structure, blue N, green Na, purple Mn). Variable-temperature magnetization measurements show that the complex is antiferromagnetic.

Linking PO43− and HAsO42− anions with a dinuclear [ZnII2] complex: Formation and stabilization of novel decanuclear metallomacrocyclic [ZnII10] and t…

2017

The linkage of PO43- and HAsO42--anions with a newly synthesized five-coordinate dinuclear zinc complex, Zn-2(cpdp)(H2O)(2)]Cl (1) H(3)cpdp =N,N'-bis2-carboxybenzomethyl]-N,N'-bis2-pyridylmethyl]-1,3diamino propan-2-ol], has been explored. In methanol-water, the reaction of 1 with Na2HPO4 center dot 2H(2)O and Na2HAsO4 center dot 7H(2)O/NaBr separately, at ambient temperature, yielded the novel phosphate-bridged decanuclear zinc cluster, (H3O)(4)Zn-10(cPdP)(4)(mu(5)-PO4)(2)(H2O)(6)](6 center dot Cl)center dot 53H(2)O (2) and hydrogen arsenate bridged tetranuclear zinc cluster, Na-2Zn-4(cpdp)(2)(mu(4)-HAsO4)]ClBr center dot 13H(2)O (3), respectively. Analysis of the single crystal X-ray stru…

A distorted honeycomb motif in divalent transition metal compounds based on 4-phosphonbenzoic acid and exchange coupled Co(II) and Cu(II): synthesis,…

2013

The first example of a two-dimensional inorganic hybrid material with cobalt as an open-shell transition metal ion and 4-phosphonbenzoic acid as a linker is presented together with its copper analogue. For both metal ions the inorganic part consists of edge-sharing metal–oxygen octahedra leading to a metal honeycomb motif. The magnetic properties of the cobalt compound are reported together with those of the corresponding copper compound based on the remarkably six-coordinated copper(II) ions.

Structure and properties of a novel staircase-like decanuclear [CuII10] cluster supported by carbonate and carboxylate bridges

2018

This article describes a novel staircase-like decanuclear copper(II) cluster [CuII10(cpdp)4(CO3)4(CH3OH)2]·3.33CH3OH·7.83H2O (1) (H3cpdp = N,N′-bis[2-carboxybenzomethyl]-N,N′-bis[2-pyridylmethyl]-1,3-diaminopropan-2-ol) composed of a pair of [CuII5] pentamers. In methanol, the reaction of H3cpdp with Cu(NO3)2·3H2O in the presence of K2CO3 leads to the isolation of complex 1. This complex has been characterized by various analytical techniques including single crystal X-ray crystallography. Structural analysis reveals that the two [CuII5] pentameric units are bridged together exclusively by two μ2:η2:η1 carbonate groups. Complex 1 shows a rare μ3:η2:η1:η1 bridging coordination mode of four b…

A Family of Dinuclear Iron(II) SCO Compounds Based on a 1,3,4‐Thiadiazole Bridging Ligand (Eur. J. Inorg. Chem. 22/2015)

2015

Triple bridged μ-phenoxo-bis(μ-carboxylate) and double bridged μ-phenoxo-μ1,1-azide/μ-methoxide dicopper(II) complexes: Syntheses, structures, magnet…

2013

Abstract The work in this paper presents syntheses, characterization, crystal structures, catecholase activity, electrospray ionization mass spectroscopy (ESI-MS positive), and magnetic properties of seven triple bridged μ-phenoxo-bis(μ-carboxylate) dicopper(II) complexes [CuII2L(μ-HCOO)2](ClO4)·CH3OH (1), [CuII2L(μ-CH3COO)2](ClO4) (2), [CuII2L(μ-CCl3COO)2(H2O)](ClO4) (3), [CuII2L(μ-CH3CH2COO)2](ClO4) (4), [CuII2L(μ-CH3CH2CH2COO)2](ClO4) (5), [CuII2L(μ-PhCOO)2](ClO4)·CH3CN (6) and [CuII2L(μ-o-ClPhCOO)2](ClO4) (7), one double bridged μ-phenoxo-μ1,1-azide system [CuII2L(μ1,1-N3)(N3)2] (8) and one double bridged μ-phenoxo-μ-methoxide system [CuII2L(μ-OCH3)(NCO)2] (9), derived from a new dinucl…

An intramolecular antiferromagnetically coupled pentanuclear homoleptic Mn(II) cluster: Synthesis, crystal structure, spectral and magnetic property

2013

Abstract A pyrazole based ditopic ligand 5(E)-5-methyl-N′-(pyridin-2-ylmethylene)-1H-pyrazole-3-carbohydrazide (PzOPyH), prepared by the reaction between 5-methylpyrazole-3-carbohydrazide and pyridine-2-carbaldehyde, reacts with Mn(ClO4)2·6H2O to form a self-assembled, antiferromagnetically coupled alkoxide bridged pentanuclear Mn(II) homoleptic cluster complex [Mn5(PzOPy)6](ClO4)4 (1). The complex has a central Mn5(μ-O6) core involving six ligand molecules. This pentanuclear core has a trigonal bipyramidal arrangement of Mn(II) atoms, where, the axial metal centers (Mn2 and Mn_2) have a N3O3 chromophore and the equatorial centers (Mn1, Mn_1 and Mn3) have N4O2 chromophore with distorted oct…

Phosphatase-like Activity of Tetranuclear Iron(III) and Zinc(II) Complexes

2018

Three new tetranuclear iron(III) and zinc(II) complexes, [Fe4(cpdp)2(phth)2(OH)2]·8H2O (1), [Fe4(cpdp)2(terephth)2(OH)2] (2), and [Zn4(Hcpdp)2(suc)]Br2·12H2O (3), have been synthesized as models for the active site of phosphoester hydrolases by utilizing a polydentate ligand, N, N'-bis[2-carboxybenzomethyl]- N, N'-bis[2-pyridylmethyl]-1,3-diaminopropan-2-ol (H3cpdp) in combination with exogeneous phthalate (phth), terephthalate (terephth), and succinate (suc). Single crystal X-ray analyses reveal that the metallic core of complex 1 consists of four distorted octahedral iron(III) ions with average intraligand Fe---Fe separation of 3.656(2) A, while the structure 3 represents a tetranuclear m…

Syntheses, structures, electrochemical measurements and magnetic properties of two iron(III) complexes derived from N,N′-o-phenylenebis(3-ethoxysalic…

2011

Abstract The work in this paper presents syntheses, characterizations, crystal structures, electrochemical measurements and magnetic properties of two iron(III) compounds [FeIIIL(H2O)(MeOH)](ClO4) (1) and [FeIIIL(H2O)2](NO3)·H2O (2) derived from the Schiff base compartmental ligand N,N′-o-phenylenebis(3-ethoxysalicylaldimine) (H2L). The two compounds are characterized by elemental analyses, IR, electrospray ionization mass (ESI-MS positive), UV–Vis spectra and conductance values. The structures of 1 and 2 show that these are mononuclear compounds having the metal ion in the N2O2 compartment. Two mononuclear moieties in both the compounds are self-assembled due to bifurcated hydrogen bonds i…

Phase Trapping in Multistep Spin Crossover Compound

2020

The dimeric motif is the smallest unit for two interacting spin centers allowing for systematic investigations of cooperative interactions. As spin transition compounds, dinuclear complexes are of particular interest, since they potentially reveal a two-step spin crossover (SCO), switching between the high spin-high spin [HS-HS], the high spin-low spin [HS-LS], and the low spin-low spin [LS-LS] states. Herein, we report the synthesis and characterization of six dinuclear iron(II) complexes [FeII2(μ2-L1)2](BF4)4 (C1), [FeII2(μ2-L1)2](ClO4)4 (C2), [FeII2(μ2-L1)2](F3CSO3)4 (C3), [FeII2(μ2-L2)2](BF4)4 (C4), [FeII2(μ2-L2)2](BF4)4 (C5), and [FeII2(μ2-L2)2](BF4)4 (C6), based on the 1,3,4-thiadiazo…

Tuning the Basicity of Synergic Bimetallic Reagents: Switching the Regioselectivity of the Direct Dimetalation of Toluene from 2,5‐ to 3,5‐Positions

2008

Meta-meta metalation: Remarkably, toluene can be directly dimanganated or dimagnesiated at the 3,5-positions using bimetallic bases with active Me3SiCH2 ligands (see scheme, blue). In contrast, n-butyl ligands lead to 2,5-metalation (red). tmp=2,2,6,6-tetramethylpiperidide.

Front Cover: Filling the Gap in the Metallacrown Family: The 9‐MC‐3 Chromium Metallacrown (Chem. Eur. J. 13/2021)

2021

Dinuclear and tetranuclear complexes of copper coordinated by an anthracene-based new μ-bis(tridentate) ligand: Synthesis, structure, spectroscopy an…

2016

Abstract Copper(II) complexes of an anthracene-based new μ-bis(tridentate) ligand, N,N′-bis[anthracene-2-ylmethyl]-N,N′-bis[carboxymethyl]-1,3-diaminopropan-2-ol (H3acdp) with mixed donating groups, have been studied in solid state as well as in solution. The reaction of stoichiometric amounts of CuSO4·5H2O and the ligand H3acdp in the presence of NaOH at ambient temperature in methanol-dichloromethane, afforded a new dinuclear copper complex, [Cu2(acdp)(MeO)(MeOH)2] (1). On the other hand, the reaction of stoichiometric amounts of Cu(OAc)2·H2O and the ligand H3acdp in the presence of NaOH at ambient temperature in methanol-dichloromethane yielded, a novel tetranuclear copper complex, [Cu4(…

A Vanadium(III) Complex with Blue and NIR-II Spin-Flip Luminescence in Solution.

2020

Luminescence from Earth-abundant metal ions in solution at room temperature is a very challenging objective due to the intrinsically weak ligand field splitting of first-row transition metal ions, which leads to efficient nonradiative deactivation via metal-centered states. Only a handful of 3d

Increasing the nuclearity and spin ground state in a new family of ferromagnetically-coupled {Ni10} disk-like complexes bearing exclusively end-on br…

2018

The synthesis of a new family of ferromagnetically-coupled {Ni10} clusters counterbalanced by various [Ln(NO3)5]2− ions is herein described. The resulting compounds are organic chelate-free and the metal ions are exclusively bridged by end-on azido ligands to stabilize a beautiful disk-like topology reminiscent of the structure of the brucite mineral.

Counter-complementarity control of the weak exchange interaction in a bent {Ni(ii)3 complex with a μ-phenoxide-μ-carboxylate double bridge

2019

We have prepared and structurally characterized a novel {Ni3} bent complex bearing a double μ-phenoxide-μ-carboxylate bridge. Both terminal Ni(ii) sites are symmetry related, offering a simplified exchange interaction scheme. DC magnetic data is consistent with a weak antiferromagnetic interaction between the central and terminal Ni(ii) ions. As expected for a Ni(ii) system, local zero-field splitting is observed, which can be experimentally established. Broken symmetry quantum chemical calculations, as well as ab initio CASSCF-SA-SOC computations that support the magnetic experimental data, were also performed. From the analysis of other reported closely related Ni(ii) systems, a counter-c…

Structural characterization and magnetic property studies of a mixed-valence {CoIIICoII4} complex with a μ4-oxo tetrahedral {CoII4} motif

2020

We have synthesized and structurally characterized a new mixed valence pentanuclear Co complex, bearing a rare μ4-O-tetrahedral CoII4 unit, by employing a pyridine-like Schiff base ligand. We have performed DC magnetic susceptibility and magnetization measurements over polycrystalline samples and chemical quantum computations in order to understand the exchange interaction pattern within Co(II) sites and ground state magnetic anisotropy. This new complex shows an overall antiferromagnetic exchange interaction whose strength strongly depends on the local symmetry of Co(II) sites. Also, local ion magnetic anisotropy reveals a strongly axial behaviour with the lowest Kramers doublet (KD) at ea…

Structure and reactivity of a mononuclear gold(II) complex.

2017

Mononuclear gold(II) complexes are very rare labile species. Transient gold(II) species have been suggested in homogeneous catalysis and in medical applications, but their geometric and electronic structures have remained essentially unexplored: even fundamental data, such as the ionic radius of gold(II), are unknown. Now, an unprecedentedly stable neutral gold(II) complex of a porphyrin derivative has been isolated, and its structural and spectroscopic features determined. The gold atom adopts a 2+2 coordination mode in between those of gold(III) (four-coordinate square planar) and gold(I) (two-coordinate linear), owing to a second-order Jahn–Teller distortion enabled by the relativistical…

Aromatic dicarboxylate incorporated new di- and tetranuclear cobalt(II) complexes: Synthetic and structural aspects, and evaluation of properties and…

2020

Abstract The synthetic and structural aspects as well as evaluation of magnetic properties and catalytic activity toward aerial oxidation of 3,5-di-tert-butylcatechol to 3,5-di-tert-butylbenzoquinone of three new, two di- and one tetranuclear cobalt(II) complexes, [Co2(cpdp)(Hphth)]∙5H2O (1), [Co2(cpdp)(Hisophth)] (2) and [Co4(cpdp)2(terephth)]∙4.5CH3OH·5.5H2O (3), based on a symmetrical multidentate ligand, N,N'-Bis[2-carboxybenzomethyl]-N,N'-Bis[2-pyridylmethyl]-1,3-diaminopropan-2-ol (H3cpdp) in combination with exogeneous aromatic dicarboxylic acids, such as phthalic acid (H2phth), isophthalic acid (H2isophth) and terephthalic acid (H2terephth) are reported. All three coordination compl…

Spin Crossover and Long-Lived Excited States in a Reduced Molecular Ruby.

2020

Abstract The chromium(III) complex [CrIII(ddpd)2]3+ (molecular ruby; ddpd=N,N′‐dimethyl‐N,N′‐dipyridine‐2‐yl‐pyridine‐2,6‐diamine) is reduced to the genuine chromium(II) complex [CrII(ddpd)2]2+ with d4 electron configuration. This reduced molecular ruby represents one of the very few chromium(II) complexes showing spin crossover (SCO). The reversible SCO is gradual with T 1/2 around room temperature. The low‐spin and high‐spin chromium(II) isomers exhibit distinct spectroscopic and structural properties (UV/Vis/NIR, IR, EPR spectroscopies, single‐crystal XRD). Excitation of [CrII(ddpd)2]2+ with UV light at 20 and 290 K generates electronically excited states with microsecond lifetimes. This…

Strongly Red-Emissive Molecular Ruby [Cr(bpmp)2]3+ Surpasses [Ru(bpy)3]2+

2021

Gaining chemical control over the thermodynamics and kinetics of photoexcited states is paramount to an efficient and sustainable utilization of photoactive transition metal complexes in a plethora of technologies. In contrast to energies of charge transfer states described by spatially separated orbitals, the energies of spin-flip states cannot straightforwardly be predicted as Pauli repulsion and the nephelauxetic effect play key roles. Guided by multireference quantum chemical calculations, we report a novel highly luminescent spin-flip emitter with a quantum chemically predicted blue-shifted luminescence. The spin-flip emission band of the chromium complex [Cr(bpmp)2]3+ (bpmp = 2,6-bis(…

Slow relaxation of magnetization in a {Fe6Dy} complex deriving from a family of highly symmetric metallacryptands

2019

The synthesis and characterization of a new family of isostructural {Fe6Ln} complexes, (pipH)3{Fe6Ln(shiH)3(shi)6}·1.5 pip·xH2O (Ln = Gd (1), Dy (2), Tb (3) and Y (4), pip = piperidine, and shi3− = salicylhydroxamic acid) is reported. The resulting compounds possess an exceptionally unique structure of a metallacrown-like motif while the overall complexes feature more the structure of metallacryptates. Magnetic studies are reported and reveal that the {Fe6Dy} analogue belongs to the single-molecule magnet (SMM) family.

Exploring new water soluble bridged dicopper(II) assemblies: Synthesis, structure, spectroscopic characterization, properties, and their interactions…

2021

Abstract Three new water soluble dimetallic copper(II) complexes, [Cu(H2O)5][Cu2(cpdp)(µ-O2As(CH3)2)]2Br2·13.83H2O·0.67CH3OH (1), [Cu2(Hcpdp)(µ-SO4)]·5H2O (2) and [Cu2(cpdp)(µ-pz)]·16H2O (3) (H3cpdp = N,N′-Bis[2-carboxybenzomethyl]-N,N′-Bis[2-pyridylmethyl]-1,3-diaminopropan-2-ol; (CH3)2AsO2− = cacodylate; SO42− = sulfate; pz− = pyrazolate) have been successfully synthesized and characterized for the investigation of coordination/binding aspects with biologically significant monosaccharide, d -glucosamine. Preparation of 1, 2 and 3 has been achieved by carrying out reaction of H3cpdp with stoichiometric quantities of CuCl2·2H2O/NaO2As(CH3)2·3H2O, CuSO4·5H2O and CuCl2·2H2O/1H-pyrazole, respe…

Carboxylate Bridge Controlled Formation of Tetra‐ and Pentanuclear Nickel(II) Complexes: Synthesis, Crystal Structure, Spectroscopy and Magnetic Prop…

2019

Assessing the reactivity of sodium alkyl-magnesiates towards quinoxaline : single electron transfer (SET) vs. nucleophilic alkylation processes

2015

By exploring the reactivity of sodium butyl-magnesiate (1) supported by the bulky chelating silyl(bisamido) ligand {Ph2Si(NAr*)2}(2-) (Ar* = 2,6-iPr2-C6H3) towards Quinoxaline (Qx), the ability of this bimetallic system to effectively promote SET processes has been disclosed. Thus 1 executes the single-electron reduction of Qx affording complex (2) whose structure in the solid state contains two quinaxolyl radical anions Qx˙ stabilised within a dimeric magnesiate framework. Combining multinuclear NMR and EPR measurements with DFT calculations, new insights into the constitution of 2 in solution and its magnetic behaviour have been gained. Further evidence on the SET reactivity of 1 was foun…

A Discrete μ 4 ‐Oxido Tetranuclear Iron(III) Cluster

2012

Reaction of a Schiff base ligand derived from salicyloyl hydrazide and diacetyl monooxime (H2L) with a triangular μ3-oxido-centered [Fe3(μ3-O)]7+ core yields a new tetranuclear iron(III) complex. FeIII4(μ4-O) crystallizes in the triclinic space group P. Structural studies reveal that this tetranuclear iron(III) complex is a new structure type of an uncharged (alkoxido)(oxido)iron(III) cluster in which the four iron(III) ions are located at the corners of a distorted tetrahedron. A study of the magnetic properties supports the presence of antiferromagnetic interactions through the central μ4-oxido ion as well as the μ2-methoxy groups present, giving an an S = 0 ground state. Mossbauer spectr…

Oligonuclear Ferrocene Amides: Mixed‐Valent Peptides and Potential Redox‐Switchable Foldamers

2010

Trinuclear ferrocene tris-amides were synthesized from an Fmoc- or Boc-protected ferrocene amino acid, and hydrogen-bonded zigzag conformations were determined by NMR spectroscopy, molecular modelling, and X-ray diffraction. In these ordered secondary structures orientation of the individual amide dipole moments approximately in the same direction results in a macrodipole moment similar to that of α-helices composed of α-amino acids. Unlike ordinary α-amino acids, the building blocks in these ferrocene amides with defined secondary structure can be sequentially oxidized to mono-, di-, and trications. Singly and doubly charged mixed-valent cations were probed experimentally by Vis/NIR, param…

Luminescence and Light‐Driven Energy and Electron Transfer from an Exceptionally Long‐Lived Excited State of a Non‐Innocent Chromium(III) Complex

2019

Abstract Photoactive metal complexes employing Earth‐abundant metal ions are a key to sustainable photophysical and photochemical applications. We exploit the effects of an inversion center and ligand non‐innocence to tune the luminescence and photochemistry of the excited state of the [CrN6] chromophore [Cr(tpe)2]3+ with close to octahedral symmetry (tpe=1,1,1‐tris(pyrid‐2‐yl)ethane). [Cr(tpe)2]3+ exhibits the longest luminescence lifetime (τ=4500 μs) reported up to date for a molecular polypyridyl chromium(III) complex together with a very high luminescence quantum yield of Φ=8.2 % at room temperature in fluid solution. Furthermore, the tpe ligands in [Cr(tpe)2]3+ are redox non‐innocent, …

New symmetrical dinucleating ligand based assembly of bridged dicopper(II) and dizinc(II) centers: Synthesis, structure, spectroscopy, magnetic prope…

2015

Two dinuclear copper(II) complexes Li(H2O)(3)(CH3OH)](4)Cu2Br4]Cu-2(cpdp)(mu-O2CCH3)](4)(OH)(2) (1), Cu (H2O)(4)]Cu-2(cpdp)(mu-O2CC6H5)](2)Cl-2 center dot 5H(2)O (2), and a dinuclear zinc(II) complex Zn-2(cpdp)(mu-O2CCH3)] (3) have been synthesized using pyridine and benzoate functionality based new symmetrical dinucleating ligand, N, N'-Bis2-carboxybenzomethyl]-N, N'-Bis2-pyridylmethyl]-1,3-diaminopropan-2-ol (H(3)cpdp). Complexes 1, 2 and 3 have been synthesized by carrying out reaction of the ligand H3cpdp with stoichiometric amounts of Cu-2(O2CCH3)(4)(H2O)(2)], CuCl2 center dot 2H(2)O/C6H5COONa, and Zn(CH3COO)(2)center dot 2H(2)O, respectively, in methanol in the presence of NaOH at amb…

A New Co-Ni-Heterometallic Butterfly Complex Obtained via a Novel Synthesis Approach

2011

Abstract. The heterometallic complex [Co2Ni2(OH)2(O2CtBu)6(HOEt)6]·2EtOH (1) with a so called butterfly structural motif was prepared by reaction of the homometallic precursor complexes [Co2(H2O)(O2CtBu)4(HO2CtBu)4] and [Ni2(H2O)(O2CtBu)4(HO2CtBu)4] in an one to one ratio under elevate temperature. Complex 1 was characterized by single-crystal X-ray diffraction, atomic absorption spectroscopy, elemental analyses, IR spectroscopy, and mass spectrometry. The magnetic data show an overall antiferromagnetic behavior, which can be explained with three different coupling constants, resulting in a paramagnetic ground state.

Aggregation of [Ln(12)(III)] clusters by the dianion of 3-formylsalicylic acid. Synthesis, crystal structures, magnetic and luminescence properties

2019

Three isostrucutral dodecanuclear clusters with the general formula [Ln(12)(fsa)(12)(mu f(3)-OH)(12)(DMF)(12)]center dot nDMF (fsa(2-) is the dianion of 3-formylsalicylic acid; Ln = Eu 1, Gd 2, Dy 3) have been obtained from the reaction of fromylsalicyclic acid (H(2)fsa), tetrabutylammonium hydroxide and Ln(NO3)(3)center dot 6H(2)O in methanol/DMF. Their structure consists of four vertex-sharing heterocubanes. Each heterocubane unit is assembled from four Ln(III) ions, three mu(3)-OH groups and one mu(3)-oxygen atom arising from the fsa(2-) carboxylato group. The photophysical properties of the europium derivative investigated at both 300 and 80 K sustain a relative intense emission obtaine…

Combination of single-molecule magnet behaviour and luminescence properties in a new series of lanthanide complexes with tris(pyrazolyl)borate and ol…

2020

A series of tris(pyrazolyl)borate mono-, di- and trinuclear complexes, [Tp2Ln]nX (Ln = Eu, Tb, Gd, Dy, Xn− = various mono-, bis- and tris(β-diketonates) has been prepared. The Tb3+ and Dy3+ complexes are luminescent single molecular magnets (SMM) and exhibit luminescence quantum efficiencies up to 73% for the Tb3+ and 4.4% for the Dy3+ compounds. Similar Eu3+ complexes display bright emission only at lower temperatures. The Dy3+ and Tb3+ complexes possess SMM behavior in a non-zero dc field at low temperatures, while the polynuclear Dy3+ complexes also show slow magnetic relaxation even in zero dc field up to 8 K. Ueff-values determined from dynamic magnetic measurements were up to 31 and 6…

Synthesis, structure, spectral characterization and DNA binding affinity of new water soluble trinuclear copper(II) complexes with partial cubane Cu3…

2015

Two new water soluble trinuclear copper(II) complexes, [Na 6 (H 3 O) 4 ][Cu 3 (cbal) 3 (μ 3 -OH)(H 2 O) 3 ] 4 (ClO 4 ) 6 ·3H 2 O ( 1 ) and [K(H 2 O) 2 ][Cu 3 (cbal) 3 (μ 3 -OH)(H 2 O)]·3.75H 2 O ( 2 ) have been synthesized in good yield via the reaction of an unsymmetrical amino dicarboxylic ligand, N-(2-carboxybenzomethyl)-β-alanine (H 2 cbal), Cu(ClO 4 ) 2 ·6H 2 O and NaOH/K 2 CO 3 in methanol at room temperature. Complexes 1 and 2 have been characterized by elemental analysis, room temperature magnetic susceptibility measurements, FTIR, UV–Vis, mass spectrometry and single crystal X-ray crystallography. Both complexes contain a partial cubane [Cu 3 O 4 ] core consisting of the trinuclear…

Core Cross-Linked Polymeric Micelles for Specific Iron Delivery: Inducing Sterile Inflammation in Macrophages.

2021

Iron is an essential co-factor for cellular processes. In the immune system, it can activate macrophages and represents a potential therapeutic for various diseases. To specifically deliver iron to macrophages, iron oxide nanoparticles are embedded in polymeric micelles of reactive polysarcosine-block-poly(S-ethylsulfonyl-l-cysteine). Upon surface functionalization via dihydrolipoic acid, iron oxide cores act as crosslinker themselves and undergo chemoselective disulfide bond formation with the surrounding poly(S-ethylsulfonyl-l-cysteine) block, yielding glutathione-responsive core cross-linked polymeric micelles (CCPMs). When applied to primary murine and human macrophages, these nanoparti…

Exploring the exchange interaction in a mixed valence {CoII4CoIII2} hexanuclear cluster with novel topology

2012

Abstract Reaction between [Co2(μ-OH2)(μ-Piv)2(Piv)2(HPiv)4] and a (salicylidene)ethanolamine ligand under ambient reaction conditions, affords hexanuclear complexes [CoIII2CoII4(Piv)8(HPiv)2(L)2(OH)2] (1–2). Both products have been characterized crystallographically and found to be mixed-valent, containing divalent and trivalent Co centers. Down to 30 K, the variable-temperature magnetic susceptibility data are dominated by the single-ion properties of high spin Co(II) centers with distorted-octahedral coordination geometries. Below this temperature, the effect of intramolecular ferromagnetic exchange interactions becomes apparent. Magnetic data has been analyzed in terms of ground isolated…

A Series of MIICuII3 Stars (M = Mn, Ni, Cu, Zn) Exhibiting Unusual Magnetic Properties

2014

The work in this report describes the syntheses, electrospray ionization mass spectromtery, structures, and experimental and density functional theoretical (DFT) magnetic properties of four tetrametallic stars of composition [M(II)(Cu(II)L)3](ClO4)2 (1, M = Mn; 2, M = Ni; 3, M = Cu; 4, M = Zn) derived from a single-compartment Schiff base ligand, N,N'-bis(salicylidene)-1,4-butanediamine (H2L), which is the [2 + 1] condensation product of salicylaldehyde and 1,4-diaminobutane. The central metal ion (Mn(II), Ni(II), Cu(II), or Zn(II)) is linked with two μ2-phenoxo bridges of each of the three [Cu(II)L] moieties, and thus the central metal ion is encapsulated in between three [Cu(II)L] units. …

Structures and Magnetic Properties of Bis(μ‐phenoxido), Bis(μ‐phenoxido)‐μ‐carboxylato and Bis(μ‐phenoxido)bis(μ‐carboxylato) Fe III Ni II Compounds …

2015

This report describes the syntheses, characterization, crystal structures and magnetic properties of five dinuclear FeIIINiII compounds derived from two Robson-type tetraiminodiphenol macrocyclic ligands H2L1 and H2L2, which are the [2+2] condensation products of 4-ethyl-2,6-diformylphenol and 1,3-diaminopropane (for H2L1) or 2,2-dimethyl-1,3-diaminopropane (for H2L2). The compositions of the compounds are [FeIII(N3)2L1NiII(H2O)2](ClO4) (1), [FeIII(benzoato)L1NiII(H2O)(μ1,3-benzoato)](ClO4) (2), [FeIII(benzoato)L2NiII(H2O)(μ1,3-benzoato)](ClO4) (3), [FeIIIL2NiII(μ1,3-acetato)2](ClO4)·H2O (4) and [FeIIIL2NiII(μ1,3-propionato)2](ClO4)·H2O (5). The bridging moieties between the two metal ions …

Limiting nuclearity in formation of polynuclear metal complexes through [2 + 3] cycloaddition: synthesis and magnetic properties of tri- and pentanuc…

2014

A tridentate ligand p-chloro-2-{(2-(dimethylamino)ethylimino)methyl}phenol (HL) was used to generate an octahedral nickel complex [Ni(L)Cl(H2O)2] 1 which was further converted into a square-planar nickel complex [Ni(L)(N3)] 2. The [2 + 3] cycloaddition reaction between metal coordinated azide 2 and different organonitriles under microwave irradiation afforded tri- and pentanuclear nickel(II) complexes 4a-4c. Reaction with benzonitrile and 3-cyano pyridine furnished the trinuclear species [Ni3L2(5-phenyltetrazolato)4(DMF)2] 4a and [Ni3L2{5-(3-pyridyl)-tetrazolato}4(DMF)2]·2H2O 4b, respectively. The nickel centers were found to be linearly disposed to each other and the complex is formed by a…

Syntheses, characterisation, magnetism and photoluminescence of a homodinuclear Ln(III)-Schiff base family.

2009

A novel family of homodinuclear complexes of the general formula [Ln(2)L(2)(X)(2)] (where Ln = Nd(3+), Pr(3+), Sm(3+) and Tb(3+) for 1, 2, 3 and 4, respectively and X, the coordinated NO(3)(-) or Cl(-) anion) has been synthesised from the corresponding lanthanide(III) salts with the pentadentate dianionic Schiff base ligand, H(2)L [N(1),N(3)-bis(salicylideneimino)diethylenetriamine], that exhibits a N(3)O(2) donor set. Single crystal X-ray diffraction studies evidenced the isostructurality of this family of centrosymmetric neutral dinuclear entities where the Ln(III) metal centres are coupled together by two phenolato oxygen atoms belonging to two units of ligand (H(2)L). Interestingly, the…

Magnetic Molecular Rectangles Constructed from Functionalized Nitronyl‐Nitroxide Ligands and Lanthanide(III) Ions

2020

Single Molecule Magnet Features in the Butterfly [Co III 2 Ln III 2 ] Pivalate Family with Alcohol‐Amine Ligands

2021

Field-Induced Slow Magnetic Relaxation In the First Dy(III)-centered 12-Metallacrown-4 Double-Decker

2019

The reaction of Dy(O2CMe)3·xH2O and Ga(NO3)3·xH2O led to the isolation of (nBu4N)[GaIII8DyIII(OH)4(shi)8] (1). The compound possesses a unique chemical structure enclosing the central magnetic DyIII ion between diamagnetic GaIII-based metallacrown 12-MC-4 ligands. The double-decker complex exhibits field-induced single-molecule magnet (SMM) behaviour with an effective energy barrier (Ueff) of 39 K (27.1 cm−1). Consistent with the observed slow relaxation of magnetization, theoretical calculations suggest a ground state mainly determined by |±11/2> in the easy axis direction.

Magnetic polyorganosiloxane core–shell nanoparticles: Synthesis, characterization and magnetic fractionation

2010

Abstact Here, we present the synthesis, characterization and magnetic separation of magnetic polyorganosiloxane nanoparticles. Magnetic iron oxide nanoparticles with average particle radii of 3.2 nm had been synthesized by a simple coprecipitation process of iron(II) and iron(III) salt in basic solution. Afterwards, the particles were successfully incorporated into a polyorganosiloxane network via a polycondensation reaction of trimethoxymethylsilane (T), diethoxydimethylsilane (D) and the functional monomer (chloromethylphenyl)trimethoxysilane (ClBz-T) in aqueous dispersion. A core–shell system was chosen to increase the flexibility of the system concerning size, composition and functional…

Syntheses, crystal structures and magnetic properties of a series of μ-phenoxo-μ1,1-carboxylato-μ1,3-carboxylato trinickel(II) compounds.

2014

The work in this report describes the syntheses, characterization, crystal structures and magnetic properties of eight linear trinickel(ii) compounds of the composition [Ni(II)3(L(sal-pyr))2(propionate)4] (), [Ni(II)3(L(sal-pyr))2(benzoate)4]·CH3CN (), [Ni(II)3(L(sal-pip))2(acetate)4]·2CH3CN (), [Ni(II)3(L(sal-pip))2(propionate)4] (), [Ni(II)3(L(sal-pip))2(benzoate)4]·CH2Cl2 (), [Ni(II)3(L(sal-mor))2(propionate)4] (), [Ni(II)3(L(sal-mor))2(benzoate)4]·3CH2Cl2 () and [Ni(II)3(L(sal-mor))2(o-Cl-benzoate)4]·2CH3CN·2H2O (), where HL(sal-pyr), HL(sal-pip) and HL(sal-mor) are the 1 : 1 condensation products of salicylaldehyde and 1-(2-aminoethyl)-pyrrolidine, 1-(2-aminoethyl)-piperidine and 4-(2-…

Switching nuclearity and Co(II) content through stoichiometry adjustment: {Co(II)6Co(III)3} and {Co(II)Co4(III)} mixed valent complexes and a study o…

2015

We are reporting two new mixed valent Co(ii)/Co(iii) polynuclear complexes, {Co II 6 Co III 3 } and {Co II Co III 4 }, bearing different amount of Co(ii) ions in their cores, through the employment of the multidentate triethanolamine (teaH 3 ) ligand in different stoichiometric ratios. We present a complete picture of the magnetic behaviour of both complexes through a combined usage of the susceptibility, magnetization and X-band EPR data as well as broken-symmetry DFT calculations. Compound 1 shows an atypical spin-only behaviour, probably due to the presence of four and five coordinated Co(ii) sites as well as highly distorted six coordinated Co(ii) ions, promoting a high degree of orbita…

Syntheses, structures, and magnetic properties of diphenoxo-bridged Cu(II)Ln(III) and Ni(II)(low-spin)Ln(III) compounds derived from a compartmental …

2010

Syntheses, characterization, and magnetic properties of a series of diphenoxo-bridged discrete dinuclear M(II)Ln(III) complexes (M = Cu or Ni, Ln = Ce-Yb) derived from the compartmental Schiff base ligand, H(2)L, obtained on condensation of 3-ethoxysalicylaldehyde with trans-1,2-diaminocyclohexane, are described. Single crystal X-ray structures of eight Cu(II)Ln(III) compounds (Ln = Ce (1), Pr (2), Nd (3), Sm (4), Tb (7), Ho (9), Er (10), and Yb (12)) and three Ni(II)Ln(III) (Ln = Ce (13), Sm (16), and Gd (18)) compounds have been determined. Considering the previously reported structure of the Cu(II)Gd(III) (6) compound (Eur. J. Inorg. Chem. 2005, 1500), a total of twelve structures are di…

Synthesis and Structure of a Potassium Potassiochromate: A Bis-Chromium(II) Molecule Held Together by Near-Square-Planar Potassium−Ligand Bridges

2010

No Cr-Cr bonding is found in a new type of mixed-metal ate complex having two coordinatively unsaturated but sterically saturated bisamido-monoalkyl Cr(II) groups linked via an unusual near-square-planar-coordinated K atom in the moiety of the ate, while the cationic moiety is a separated iris-tmeda solvated second potassium atom.

Filling the Gap in the Metallacrown Family: The 9‐MC‐3 Chromium Metallacrown

2021

Abstract In this work, we report on a long‐sought missing complex in the metallacrown family. We synthesized and characterized the novel chromium metallacrown (MC) complex {CrIII(μ 2‐piv)3[9‐MCCr(III)N(shi)‐3](morph)3}⋅MeOH (in which shi3−=salicyl hydroxamate, piv=pivalate, and morph=morpholine). The MC with a 9‐MC‐3 cavity of kinetically inert chromium(III) ions was synthesized by a solvothermal reaction. Magnetization measurements reveal a high spin ground state.

Syntheses, Structures, Magnetic Properties, and Density Functional Theory Magneto-Structural Correlations of Bis(μ-phenoxo) and Bis(μ-phenoxo)-μ-acet…

2013

The bis(mu-phenoxo) (FeNiIII)-Ni-II compound [Fe-III(N-3)(2)LNiII(H2O)(CH3CN)](ClO4) (1) and the bis(mu-phenoxo)-mu-acetate/bis(mu-phenoxo)-bis(mu-acetate) (FeNiII)-Ni-III compound {[Fe-III(OAc)LNiII(H2O)(mu-OAc)](0.6)center dot[(FeLNiII)-L-III(mu-OAc)(2)](0.4)}(ClO4)center dot 1.1H(2)O (2) have been synthesized from the Robson type tetraiminodiphenol macrocyclic ligand H2L, which is the [2 + 2] condensation product of 4-methyl-2,6-diformylphenol and 2,2'-dimethy1-1,3-diaminopropane. Single-crystal X-ray structures of both compounds have been determined. The cationic part of the dinuclear compound 2 is a cocrystal of the two species [Fe-III(OAc)LNiII(H2O)(mu-OAc)](+) (2A) and [(FeLNiII)-L-I…

Synthesis, structure and properties of a novel self-assembled tetranuclear copper(II) complex derived from carboxylate-based multidentate ligand

2020

Abstract A novel tetranuclear copper(II) complex, [Cu(H2O)5][Cu4(cpdp)2(adip)]ClBr∙2CH3OH·8H2O (1) of carboxylate-based symmetrical multidentate ligand, H3cpdp [H3cpdp = N,N'-Bis[2-carboxybenzomethyl]-N,N'-Bis[2-pyridylmethyl]-1,3-diaminopropan-2-ol; adip = adipate], has been synthesized and fully characterized. Complex 1 has been synthesized by carrying out reaction of ligand H3cpdp with stoichiometric amounts of CuCl2·2H2O/Na2(CH2CH2COO)2 in methanol-water in the presence of NaOH at room temperature. The solid state structure of 1 consists of a [Cu4(µ4-adip)] core unit which is held together by two multidentate bridging ligands, cpdp3−. In fact, complex 1 can be viewed as a “dimer-of-dime…

Hydrolytically active tetranuclear [NiII2]2 complexes: synthesis, structure, spectroscopy and phosphoester hydrolysis

2015

Three tetranuclear nickel(II) complexes, [Ni4(H2chdp)2(H2O)4]Br2·4CH3OH·3H2O (1), [Ni4(H2chdp)2(H2O)4](PF6)2 (2) and [Ni4(H2chdp)2(H2O)4](ClO4)2·3.2CH3OH·0.8H2O (3) have been synthesized by exploiting the flexibility, chelating ability and bridging potential of a new symmetrical μ-bis(tetradentate) ligand, H5chdp (H5chdp = N,N′-bis[2-carboxybenzomethyl]-N,N′-bis[2-hydroxyethyl]-1,3-diaminopropan-2-ol). Complexes 1, 2 and 3 have been synthesized by carrying out reaction of the ligand H5chdp with stoichiometric amounts of NiCl2·6H2O/NaBr, NiCl2·6H2O/NH4PF6, and Ni(ClO4)2·6H2O, respectively, in methanol–water in the presence of NaOH at ambient temperature. Characterizations of the complexes ha…

Sodium Congener of the Classical Lithium Methylchromate Dimer: Synthetic, X-ray Crystallographic, and Magnetic Studies of Me8Cr2[Na(OEt2)]4

2011

One of the milestone structures in the development of transition-metal complexes with metal metal bonds of multiple bond order was the lithium methylchromate dimer Me8Cr2[Li(donor)](4) (donor = THF or Et2O). Using a simple salt metathesis reaction mixing this compound with sodium tert-butoxide, the sodium congener Me8Cr2-[Na(OEt2)]4 has been synthesized as a green crystalline compound and isolated in 51% yield. Its solid-state structure was determined by single-crystal X-ray diffraction. Exhibiting exact crystallographic C-4h symmetry, this heavier alkali-metal chromate structure is also dimeric, formally comprising a (Me8Cr4)(4-) tetranionic core with four peripheral Na+ cations carrying s…

Coordination of expanded terpyridine ligands to cobalt

2013

Abstract The tridentate expanded terpyridine-like ligand N,N′-dimethyl-N,N′-dipyridin-2-yl-pyridin-2,6-diamine (ddpd) and [Co(H2O)6](BF4)2 give the high-spin complex mer-[Co(ddpd)2](BF4)2 with a tetragonally compressed CoN6 coordination geometry according to X-ray diffraction and SQUID measurements. UV–Vis–NIR spectra indicate a large ligand field splitting close to the high-spin/low-spin crossover point. Oxidation of the CoII complex to CoIII is achieved with silver triflate. The self exchange between high-spin CoII and low-spin CoIII is slow on the NMR time scale.

A Family of Dinuclear Iron(II) SCO Compounds Based on a 1,3,4‐Thiadiazole Bridging Ligand

2015

A new family of dinuclear iron(II) spin-crossover (SCO) compounds with the formula [Fe2(μ-L)2]X4, with three different counteranions [X = BF4– (1), ClO4– (2) and F3CSO3– (3)], was prepared and characterized by single-crystal X-ray diffraction, variable-temperature magnetic susceptibility and Mossbauer measurements. These are the first dinuclear iron(II) SCO complexes with a 1,3,4-thiadiazole bridging ligand L {with L = 2,5-bis[(2-pyridylmethyl)amino]methyl-1,3,4-thiadiazole}. The magnetic measurements reveal a gradual and incomplete SCO of the three compounds around room temperature, starting from a diamagnetic [LS–LS] state. The diamagnetic ground state is in agreement with the single-crys…

Cover Picture: Direct CH Metalation with Chromium(II) and Iron(II): Transition-Metal Host / Benzenediide Guest Magnetic Inverse-Crown Complexes (Ang…

2009

Chromation and ferration are the latest additions to the concept of alkali-metal-mediated metalation, as described by J. Klett, R. E. Mulvey, and co-workers in their Communication on page 3317 ff. While the more electropositive sodium is essential for the reaction, it is the less electropositive chromium or iron that actually performs deprotonation of benzene. This novel reactivity can be likened to a game of chess in which the queen (Na) holds the king in check, while the knight (Cr, Fe) scores checkm(etal)ate.

Direct C-H metalation with chromium(ii) and iron(ii): transition- metal host/benzenediide guest magnetic inverse-crown complexes

2009

Check M(etal)ate: The chessboard and the figures represent a special reaction in which different low-polarity metals can metalate arenes directly when they are brought into the right position. In a combination of queen (sodium) and knight (chromium or iron), it is possible for the knight (usually the weaker piece) to make a direct deadly hit on the king (benzene) in this game of elemental chess. Fil: Alborés, Pablo. Johannes Gutenberg Universitat Mainz; Alemania. Consejo Nacional de Investigaciones Científicas y Técnicas; Argentina Fil: Carrella, Luca M.. Johannes Gutenberg Universitat Mainz; Alemania Fil: Clegg, William. University of Newcastle; Reino Unido Fil: García Álvarez, Pablo. Univ…

3d/4f Sandwich Complex Based on Metallacrowns.

2021

A novel lanthanide double-decker complex with nickel metallacrowns (MCs) as coordinating ligands has been synthesized. In the 3d/4f metallacrown complex TbIII[12-MCNiIIN(shi)-4]2, the central lanthanide ion is sandwiched between two [12-MC-4] units, forming an almost ideal square-antiprismatic coordination sphere. The resulting zenithal angles at the central lanthanide ion are smaller than those for previously reported sandwich compounds. Magnetic measurements reveal an energy barrier of 346 K under zero field and up to 585 K under 3200 Oe, the highest reported for metallacrowns with D4d symmetry.

Control of Exchange Interactions in Trinuclear Complexes Based on Orthogonal Magnetic Orbitals

2009

The reaction of copper(II) acetate with the tetradentate Schiff base like ligand H4L {(E,E)-[{diethyl 2,2′-[4,5-dihydroxy-1,2-phenylenebis(iminomethylidyne)]bis(3-oxobutanoate)}] leads to the formation of the square planar N2O2 coordinated complex [H2CuL]. Reaction of two equivalents of this complex with copper(II) acetylacetonato or vanadyl(IV) acetylacetonato yields the trinuclear complexes [V(O)Cu2L2][N(nBu)4]2·2MeOH (1) and [Cu3L2][N(nBu)4]2·2DMF (2). Both complexes were characterised by using magnetic measurements and X-ray crystallography. Special attention was given to the spin-exchange coupling through the bridging phenylene ring. The principle of strict orthogonality of the magneti…

Azide bridged dicopper(II), dicobalt(II) complexes and a rare double μ-chloride bridged ferromagnetic dicobalt(II) complex of a pyrazolyl-pyrimidine …

2012

Abstract Two new dinuclear copper(II) complexes [Cu2(PymPz)2(N3)2Cl2] (1), [Cu2(PymPz)2(N3)4] (2) and two new dinuclear cobalt(II) complexes [Co2(PymPz)2Cl4] (3), [Co2(PymPz)2(N3)4] (4) [PymPz = 2-(3,5-dimethyl-1H-pyrazol-1-yl)-4,6-dimethylpyrimidine] have been synthesized and characterized crystallographically and spectroscopically. In each of the complexes 1, 2 and 4 the two adjacent metal centers are bridged by a pair of μ-1,1 azide groups whereas in 3 the metal centers are bridged by a pair of chloride ions. In the complexes, all the metal centers are pentacoordinated. In 1 and 2 the copper(II) centers have distorted square pyramidal geometry (τ = 0.18 for 1 and 0.091 for 2) but in 3 an…

Structural and Magnetic Insights into the Trinuclear Ferrocenophane and Unexpected Hydrido Inverse Crown Products of Alkali‐Metal‐Mediated Manganatio…

2008

With the aim of introducing the diisopropylamide [NiPr(2)](-) ligand to alkali-metal-mediated manganation (AMMMn) chemistry, the temperature-dependent reactions of a 1:1:3 mixture of butylsodium, bis(trimethylsilylmethyl)manganese(II), and diisopropylamine with ferrocene in hexane/toluene have been investigated. Performed at reflux temperature, the reaction affords the surprising, ferrocene-free, hydrido product [Na(2)Mn(2) (mu-H)(2){N(iPr)(2)}(4)]2 toluene (1), the first Mn hydrido inverse crown complex. Repeating the reaction rationally, excluding ferrocene, produces 1 in an isolated crystalline yield of 62 %. At lower temperatures, the same bimetallic amide mixture leads to the manganati…

Copper(II) complexes with 1,5-bis(2-hydroxybenzaldehyde)carbohydrazone

2014

Abstract The acid–base properties of 1,5-bis(2-hydroxybenzaldehyde)carbohydrazone (H4L) and its thioanalogue 1,5-bis(2-hydroxybenzaldehyde)thiocarbohydrazone (H4LS) have been studied experimentally by pH-potentiometry and UV–Vis spectrophotometry and theoretically by using DFT methods. Copper(II) complexes [Cu2(HL)(DMSO)2(H2O)]NO3·H2O (1), [{Cu2(HL)(DMF)(H2O)}n][{Cu2(HL)(DMF)NO3}n](NO3)n (2), [Cu2(HL)(DMF)2(H2O)]HSO4·H2O (3), [Cu2(HL)(DMF)2(H2O)][Cu2(HL)(SO4)(H2O)(DMF)2]·2H2O (4) and [Cu4(HL)2(HSO4)(DMF)2]HSO4 (5), where H4L = 1,5-bis(2-hydroxybenzaldehyde)carbohydrazone, have been synthesised. Complexes 1–3 have been characterised by elemental analysis, IR spectroscopy, ESI mass spectromet…

CCDC 1825561: Experimental Crystal Structure Determination

2019

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CCDC 1431264: Experimental Crystal Structure Determination

2015

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CCDC 1949845: Experimental Crystal Structure Determination

2020

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CCDC 1980403: Experimental Crystal Structure Determination

2020

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CCDC 977382: Experimental Crystal Structure Determination

2016

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CCDC 978467: Experimental Crystal Structure Determination

2014

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CCDC 1979793: Experimental Crystal Structure Determination

2020

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CCDC 1979785: Experimental Crystal Structure Determination

2020

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CCDC 1949842: Experimental Crystal Structure Determination

2020

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CCDC 1876390: Experimental Crystal Structure Determination

2019

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CCDC 1979783: Experimental Crystal Structure Determination

2020

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CCDC 1979777: Experimental Crystal Structure Determination

2020

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CCDC 1979787: Experimental Crystal Structure Determination

2020

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CCDC 977085: Experimental Crystal Structure Determination

2016

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CCDC 978468: Experimental Crystal Structure Determination

2014

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CCDC 1959867: Experimental Crystal Structure Determination

2020

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CCDC 1949843: Experimental Crystal Structure Determination

2020

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CCDC 1979786: Experimental Crystal Structure Determination

2020

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CCDC 1864765: Experimental Crystal Structure Determination

2018

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CCDC 1989536: Experimental Crystal Structure Determination

2021

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CCDC 1959865: Experimental Crystal Structure Determination

2020

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CCDC 978469: Experimental Crystal Structure Determination

2014

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CCDC 1958562: Experimental Crystal Structure Determination

2020

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CCDC 1979788: Experimental Crystal Structure Determination

2020

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CCDC 961048: Experimental Crystal Structure Determination

2014

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CCDC 1979789: Experimental Crystal Structure Determination

2020

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CCDC 1062667: Experimental Crystal Structure Determination

2015

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CCDC 1873577: Experimental Crystal Structure Determination

2019

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CCDC 1949841: Experimental Crystal Structure Determination

2020

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CCDC 1825562: Experimental Crystal Structure Determination

2019

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CCDC 808523: Experimental Crystal Structure Determination

2013

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CCDC 1980402: Experimental Crystal Structure Determination

2020

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CCDC 961049: Experimental Crystal Structure Determination

2014

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CCDC 1829268: Experimental Crystal Structure Determination

2018

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CCDC 2093069: Experimental Crystal Structure Determination

2021

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CCDC 1979781: Experimental Crystal Structure Determination

2020

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CCDC 1980401: Experimental Crystal Structure Determination

2020

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CCDC 978470: Experimental Crystal Structure Determination

2014

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CCDC 1979776: Experimental Crystal Structure Determination

2020

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CCDC 1431266: Experimental Crystal Structure Determination

2015

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CCDC 2083757: Experimental Crystal Structure Determination

2021

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CCDC 977386: Experimental Crystal Structure Determination

2016

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CCDC 977380: Experimental Crystal Structure Determination

2016

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CCDC 1873578: Experimental Crystal Structure Determination

2019

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CCDC 942761: Experimental Crystal Structure Determination

2013

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CCDC 1979790: Experimental Crystal Structure Determination

2020

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CCDC 1431263: Experimental Crystal Structure Determination

2015

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CCDC 961050: Experimental Crystal Structure Determination

2014

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CCDC 1869182: Experimental Crystal Structure Determination

2018

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CCDC 977406: Experimental Crystal Structure Determination

2016

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CCDC 1958093: Experimental Crystal Structure Determination

2020

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CCDC 977392: Experimental Crystal Structure Determination

2016

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CCDC 1062665: Experimental Crystal Structure Determination

2015

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CCDC 1989537: Experimental Crystal Structure Determination

2021

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CCDC 1979782: Experimental Crystal Structure Determination

2020

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CCDC 1979775: Experimental Crystal Structure Determination

2020

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CCDC 1876389: Experimental Crystal Structure Determination

2019

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CCDC 1903450: Experimental Crystal Structure Determination

2019

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CCDC 1959866: Experimental Crystal Structure Determination

2020

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CCDC 1873576: Experimental Crystal Structure Determination

2019

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CCDC 1959864: Experimental Crystal Structure Determination

2020

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CCDC 1864766: Experimental Crystal Structure Determination

2018

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CCDC 1431265: Experimental Crystal Structure Determination

2015

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CCDC 1864767: Experimental Crystal Structure Determination

2018

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CCDC 1979780: Experimental Crystal Structure Determination

2020

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CCDC 978466: Experimental Crystal Structure Determination

2014

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CCDC 984713: Experimental Crystal Structure Determination

2014

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CCDC 1979791: Experimental Crystal Structure Determination

2020

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CCDC 977454: Experimental Crystal Structure Determination

2016

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CCDC 1873575: Experimental Crystal Structure Determination

2019

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CCDC 1979794: Experimental Crystal Structure Determination

2020

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CCDC 1949844: Experimental Crystal Structure Determination

2020

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CCDC 1979778: Experimental Crystal Structure Determination

2020

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CCDC 1979784: Experimental Crystal Structure Determination

2020

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CCDC 1062666: Experimental Crystal Structure Determination

2015

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CCDC 977381: Experimental Crystal Structure Determination

2016

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CCDC 1825560: Experimental Crystal Structure Determination

2019

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CCDC 1979779: Experimental Crystal Structure Determination

2020

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CCDC 1979792: Experimental Crystal Structure Determination

2020

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CCDC 2047296: Experimental Crystal Structure Determination

2021

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