scholarly journals Aromatic SNF-Approach to Fluorinated Phenyl tert-Butyl Nitroxides

Molecules ◽  
2019 ◽  
Vol 24 (24) ◽  
pp. 4493 ◽  
Author(s):  
Evgeny Tretyakov ◽  
Pavel Fedyushin ◽  
Elena Panteleeva ◽  
Larisa Gurskaya ◽  
Tatyana Rybalova ◽  
...  
Keyword(s):  
Magnetic Measurements ◽  
Exchange Interactions ◽  
Crystal Structure Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Tert Butyl ◽  
Ferromagnetic Exchange ◽  
Centrally Symmetric ◽  
Tert Butylamine ◽  
Molecular And Crystal Structures

The interaction of octafluorotoluene (1a), as well as pentafluorobenzonitrile (1b) with tert-butylamine, followed by the oxidation of thus formed tert-butylanilines (2a,b) with meta-chloroperoxybenzoic acid led to functionalized perfluorinated phenyl tert-butyl nitroxides [namely, 4-(N-tert-butyl(oxyl)amino)heptafluorotoluene (3a) and 4-(N-tert-butyl(oxyl)amino)tetrafluorobenzonitrile (3b)] with nearly quantitative total yields. The molecular and crystal structures of nitroxide 3a were proved by single crystal X-ray diffraction analysis. The radical nature of both nitroxides was confirmed by ESR data. The interaction of Cu(hfac)2 with the obtained nitroxides 3a,b gave corresponding trans-bis(1,1,1,5,5,5-hexafluoropentane-2,4-dionato-κ2O,O′)bis{4-(N-tert-butyl(oxyl)amino)perfluoroarene-κO}copper (II) complexes ([Cu(hfac)2(3a)2] and [Cu(hfac)2(3b)2]). X-ray crystal structure analysis showed square bipyramid coordination of a centrally symmetric Cu polyhedron with the axial positions occupied by oxygen atoms of the nitroxide groups. Magnetic measurements revealed intramolecular ferromagnetic exchange interactions between unpaired electrons of Cu(II) ions and paramagnetic ligands, with exchange interaction parameters JCu–R reaching 53 cm−1.

scholarly journals Synthesis of Nitroxide Diradical Using a New Approach

Molecules ◽  
2020 ◽  
Vol 25 (11) ◽  
pp. 2701 ◽  
Author(s):  
Pavel Fedyushin ◽  
Tatyana Rybalova ◽  
Nargiz Asanbaeva ◽  
Elena Bagryanskaya ◽  
Alexey Dmitriev ◽  
...  
Keyword(s):  
Quantum Chemical ◽  
Total Yield ◽  
Exchange Interactions ◽  
Free Form ◽  
Dihedral Angles ◽  
X Ray Diffraction ◽  
New Approach ◽  
X Ray ◽  
Tert Butyl ◽  
Organic Systems

A new synthetic pathway to diradical organic systems is proposed. The effectiveness of this approach was exemplified by the synthesis of a new nitroxide diradical. An interaction of perfluorobiphenyl with lithium tert-butylamide, followed by oxidation of the thusly formed N4,N4′-di-tert-butyl-2,2′,3,3′,5,5′,6,6′-octafluorobiphenyl-4,4′-diamine with meta-chloroperoxybenzoic acid, led to the polyfluorinated nitroxide diradical, N,N′-(perfluorobiphenyl-4,4′-diyl)bis(N-tert-butyl(oxyl)amine), with a good total yield. The polyfluorinated diradical is stable and can be isolated in free form and completely characterized. The structure of the nitroxide diradical was proved by single-crystal X-ray diffraction analysis. According to the X-ray diffraction data, the diradical is considerably twisted: dihedral angles between the planes of the nitroxide groups and aromatic cycles are 65.1° and 69.5°, and between aromatic cycles 52.6°. Quantum chemical calculations predict well-balanced size of both intramolecular and intermolecular exchange interactions with J from −2.65 to −1.14 cm−1.

Metal Cyanide Networks Formed at an Air-Water Interface: Structure and Magnetic Properties

2000 ◽  
Vol 658 ◽  
Author(s):  
Jeffrey T. Culp ◽  
A. Nicole Morgan ◽  
Mark W. Meisel ◽  
Daniel R. Talham
Keyword(s):  
Thin Films ◽  
Photoelectron Spectroscopy ◽  
Magnetic Measurements ◽  
Exchange Interactions ◽  
Water Interface ◽  
X Ray Diffraction ◽  
X Ray ◽  
Metal Cyanide ◽  
Air Water Interface ◽  
Show Evidence

ABSTRACTExtended two-dimensional coordinate covalent networks have been formed at an air-water interface by condensing a Langmuir monolayer of an amphiphillic pentacyanoferrate(III) complex and aqueous nickel(II) ions. The cyanide-bridged arrays were transferred to solid supports by the Langmuir-Blodgett (LB) technique. The resulting thin films were structurally characterized by UV-Vis and FT-IR spectroscopies, X-ray diffraction, X-ray photoelectron spectroscopy (XPS), and SQUID magnetometry. Magnetic measurements on the thin films transferred to Mylar show evidence for ferromagnetic exchange interactions between the S = 1/2 Fe(III) and S = 1 Ni(II) centers.

Temperature-dependent synchrotron X-ray diffraction, pair distribution function and susceptibility study on the layered compound CrTe3

2018 ◽  
Vol 233 (6) ◽  
pp. 361-370 ◽  
Author(s):  
Anna-Lena Hansen ◽  
Bastian Dietl ◽  
Martin Etter ◽  
Reinhard K. Kremer ◽  
David C. Johnson ◽  
...  
Keyword(s):  
Distribution Function ◽  
Pair Distribution Function ◽  
Exchange Interactions ◽  
Structural Distortion ◽  
Layered Compound ◽  
Minor Amount ◽  
Zero Field ◽  
X Ray Diffraction ◽  
X Ray ◽  
Anisotropic Expansion

Abstract Results of combined synchrotron X-ray diffraction and pair distribution function experiments performed on the layered compound CrTe3 provide evidence for a short range structural distortion of one of the two crystallographically independent CrTe6 octahedra. The distortion is caused by higher mobility of one crystallographically distinct Te ion, leading to an unusual large Debye Waller factor. In situ high temperature X-ray diffraction investigations show an initial crystallization of a minor amount of elemental Te followed by decomposition of CrTe3 into Cr5Te8 and Te. Additional experiments provide evidence that the Te impurity (<1%) cannot be avoided. Analyses of structural changes in the temperature range 100–754 K show a pronounced anisotropic expansion of the lattice parameters. The differing behavior of the crystal axes is explained on the basis of structural distortions of the Cr4Te16 structural building units. An abrupt distortion of the structure occurs at T≈250 K, which then remains nearly constant down to 100 K. The structural distortion affects the spin exchange interactions between Cr3+ cations. A significant splitting between field-cooled (fc) and zero-field-cooled (zfc) magnetic susceptibility is observed below about 200 K. Applying a small external magnetic field results in a substantial spontaneous magnetization, reminiscent of ferro- or ferrimagnet exchange interactions below ~240 K. A Debye temperature of ~150 K was extracted from heat capacity measurements.

scholarly journals Dissimilatory Iron-Reducing Microorganisms Are Present and Active in the Sediments of the Doce River and Tributaries Impacted by Iron Mine Tailings from the Collapsed Fundão Dam (Mariana, MG, Brazil)

Minerals ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 244
Author(s):  
Carolina N. Keim ◽  
Jilder D. P. Serna ◽  
Daniel Acosta-Avalos ◽  
Reiner Neumann ◽  
Alex S. Silva ◽  
...  
Keyword(s):  
Bottom Sediments ◽  
Magnetic Measurements ◽  
Culture Media ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ferric Oxyhydroxide ◽  
Transmission Electron ◽  
Iron Mine ◽  
Organic Matter Oxidation ◽  
Doce River

On 5 November 2015, a large tailing deposit failed in Brazil, releasing an estimated 32.6 to 62 million m3 of iron mining tailings into the environment. Tailings from the Fundão Dam flowed down through the Gualaxo do Norte and Carmo riverbeds and floodplains and reached the Doce River. Since then, bottom sediments have become enriched in Fe(III) oxyhydroxides. Dissimilatory iron-reducing microorganisms (DIRMs) are anaerobes able to couple organic matter oxidation to Fe(III) reduction, producing CO2 and Fe(II), which can precipitate as magnetite (FeO·Fe2O3) and other Fe(II) minerals. In this work, we investigated the presence of DIRMs in affected and non-affected bottom sediments of the Gualaxo do Norte and Doce Rivers. The increase in Fe(II) concentrations in culture media over time indicated the presence of Fe(III)-reducing microorganisms in all sediments tested, which could reduce Fe(III) from both tailings and amorphous ferric oxyhydroxide. Half of our enrichment cultures converted amorphous Fe(III) oxyhydroxide into magnetite, which was characterized by X-ray diffraction, transmission electron microscopy, and magnetic measurements. The conversion of solid Fe(III) phases to soluble Fe(II) and/or magnetite is characteristic of DIRM cultures. The presence of DIRMs in the sediments of the Doce River and tributaries points to the possibility of reductive dissolution of goethite (α-FeOOH) and/or hematite (α-Fe2O3) from sediments, along with the consumption of organics, release of trace elements, and impairment of water quality.

scholarly journals Structural Evolution in Wet Mechanically Alloyed Co-Fe-(Ta,W)-B Alloys

Metals ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 800
Author(s):  
Vladimír Girman ◽  
Maksym Lisnichuk ◽  
Daria Yudina ◽  
Miloš Matvija ◽  
Pavol Sovák ◽  
...  
Keyword(s):  
Structural Changes ◽  
Magnetic Measurements ◽  
Structural Evolution ◽  
High Energy ◽  
Control Agent ◽  
X Ray Diffraction ◽  
Mechanically Alloyed ◽  
X Ray ◽  
Transmission Electron ◽  
X Ray Absorption

In the present study, the effect of wet mechanical alloying (MA) on the glass-forming ability (GFA) of Co43Fe20X5.5B31.5 (X = Ta, W) alloys was studied. The structural evolution during MA was investigated using high-energy X-ray diffraction, X-ray absorption spectroscopy, high-resolution transmission electron microscopy and magnetic measurements. Pair distribution function and extended X-ray absorption fine structure spectroscopy were used to characterize local atomic structure at various stages of MA. Besides structural changes, the magnetic properties of both compositions were investigated employing a vibrating sample magnetometer and thermomagnetic measurements. It was shown that using hexane as a process control agent during wet MA resulted in the formation of fully amorphous Co-Fe-Ta-B powder material at a shorter milling time (100 h) as compared to dry MA. It has also been shown that substituting Ta with W effectively suppresses GFA. After 100 h of MA of Co-Fe-W-B mixture, a nanocomposite material consisting of amorphous and nanocrystalline bcc-W phase was synthesized.

Nitroxide radicals appended to phthalonitriles: synthesis, structural characterization and photophysical properties

2021 ◽  
Vol 77 (3) ◽  
pp. 137-143
Author(s):  
Ismail Fidan ◽  
Emel Onal ◽  
Catherine Hirel
Keyword(s):  
Magnetic Measurements ◽  
Photophysical Properties ◽  
Nucleophilic Aromatic Substitution ◽  
Structural Studies ◽  
Aromatic Substitution ◽  
Nitronyl Nitroxide ◽  
X Ray Diffraction ◽  
X Ray ◽  
Microwave Assisted ◽  
Ft Ir

The syntheses of 4-[4-(4,4,5,5-tetramethyl-2-imidazoline-3-oxide-1-oxyl-2-yl)phenoxy]phthalonitrile (3, C21H19N4O3) and 4-[4-(4,4,5,5-tetramethyl-2-imidazoline-1-oxyl-2-yl)phenoxy]phthalonitrile (4) were carried out by microwave-assisted nucleophilic aromatic substitution of 4-nitrophthalonitrile (2) by the pre-formed 2-(4-hydroxyphenyl)-4,4,5,5-tetramethyl-2-imidazoline-3-oxide-1-oxyl (1). Compounds 3 and 4 were characterized unambiguously by a rich array of analyses, such as melting point, FT–IR, MALDI–TOF MS, elemental analysis, UV–Vis, CV, EPR, magnetic measurements and single-crystal X-ray diffraction. Structural studies demonstrate that the C—H...X and C—X...π (X = O and N) interactions in the radical nitronyl nitroxide groups play an important role in the assembly of the crystal structures. Moreover, cyclic voltammetry analyses show that the phthalonitrile substituent retains the redox properties of the Ullman radicals.

Structure, Magnetic Properties and Hyperfine Parameters of Nd-Substituted Ni-Fe-Ga Heusler Alloys

MRS Advances ◽  
2017 ◽  
Vol 2 (25) ◽  
pp. 1341-1346
Author(s):  
Monica Sorescu ◽  
Felicia Tolea ◽  
Mihaela Valeanu ◽  
Mihaela Sofronie
Keyword(s):  
Melt Spinning ◽  
Magnetic Measurements ◽  
Heusler Alloys ◽  
Hyperfine Magnetic Field ◽  
Rapid Quenching ◽  
Linear Least Squares ◽  
X Ray Diffraction ◽  
Hyperfine Parameters ◽  
X Ray ◽  
Field Distributions

ABSTRACTSamples of Ni57-xNdxFe18Ga25 with x=2 and 4 were prepared in ribbon form by rapid quenching via melt spinning route. The samples were analyzed by X-ray diffraction (XRD), magnetic measurements and Mössbauer spectroscopy, both in the as-quenched form and after thermal annealing at 900 oC for 2 min and 400 °C for 2 hours. For x=2 the Nd atoms are completely dissolved in the Ni-Fe-Ga matrix, while for x=4 the additional occurrence of the secondary 2:17 phase could be resolved. These findings were supported by the analysis of hyperfine magnetic field distributions obtained from the non-linear least-squares fitting of the Mössbauer spectra.

Influence of Alloying Additions on Enhancement of Soft Magnetic Properties Effect and Crystallization in FeXSiB (X=Cu, V, Co, Zr, Nb) Amorphous Alloys

2007 ◽  
Vol 130 ◽  
pp. 171-174 ◽  
Author(s):  
Z. Stokłosa ◽  
G. Badura ◽  
P. Kwapuliński ◽  
Józef Rasek ◽  
G. Haneczok ◽  
...  
Keyword(s):  
Magnetic Properties ◽  
Amorphous Alloys ◽  
Crystallization Process ◽  
Annealing Temperature ◽  
Magnetic Measurements ◽  
X Ray Diffraction ◽  
Soft Magnetic ◽  
X Ray ◽  
Second Stage ◽  
Transmission Electron

The crystallization and optimization of magnetic properties effects in FeXSiB (X=Cu, V, Co, Zr, Nb) amorphous alloys were studied by applying X-ray diffraction methods, high resolution transmission electron microscopy (HRTEM), resistometric and magnetic measurements. The temperatures of the first and the second stage of crystallization, the 1h optimization annealing temperature and the Curie temperature were determined for different amorphous alloys. Activation energies of crystallization process were obtained by applying the Kissinger method. The influence of alloy additions on optimization effect and crystallization processes was carefully examined.

X-Ray and Magnetic Measurements of TmFeTi2O7

2014 ◽  
Vol 215 ◽  
pp. 470-473 ◽  
Author(s):  
Tamara V. Drokina ◽  
German A. Petrakovskii ◽  
Dmitrii A. Velikanov ◽  
Maksim S. Molokeev
Keyword(s):  
Spin Glass ◽  
Solid Phase ◽  
Magnetic Measurements ◽  
Diffraction Method ◽  
Freezing Temperature ◽  
Solid Phase Reaction ◽  
Phase Reaction ◽  
X Ray Diffraction ◽  
X Ray ◽  
History Of

In this paper we are reported about a peculiarity of the crystal structure and the magnetic state of TmFeTi2O7. The compound TmFeTi2O7 has been synthesizedusing the solid-phase reaction method. Using X-ray diffraction method the disorder in the distribution of the iron ions over five nonequivalent crystal sites was observed, also the populations of the iron atoms positions were determined. We show that below Tf = 6 K the magnetization of TmFeTi2O7 depends on the magnetic history of the sample. There are indications for spin glass state. This results allow us to assume the state of spin glass is realized below freezing temperature Tf = 6 K in TmFeTi2O7.

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