Ion pairing, H-bonding, and π–π interactions in copper(II) complex-organo-networks derived from a proton-transfer compound of the 1,10-phenanthroline-2,9-dicarboxylic acid

The one-pot reaction between the novel proton transfer compound (pydaH₂)²⁺(phendc)²⁻, LH₂, and Cu(II) afforded the compounds (pydaH)₂[Cu(phendc)₂]·10H₂O, 1, and (pydaH)₂[Cu(phendc)(phendcH)]₂·5H₂O, 2, where pyda=2,6-diaminopyridine, and phendcH₂=1,10-phenanthroline-2,9-dicarboxylic acid. The single crystal X-ray diffraction analysis of 1 and 2 revealed that these are two novel self-assembled 3D Cu(II) complex-organo-networks, in which (pydaH)⁺ ions and [Cu(phendc)₂]²⁻ or complex units are held together by ion pairing, H-bonding, and π–π interactions. Magnetic measurements over the temperature range 1.8–310 K revealed no significant magnetic coupling between Cu(II) centers in 1 or 2.     

A Novel Proton Transfer Self‐Associated Compound from Dipicolinic Acid and Guanidine and Its Cadmium(II) Complex: Synthesis,Characterization, Crystal Structure,and Solution Studies

A novel 1:2 proton transfer self‐associated compound LH₂ , (GH⁺)₂(pydc^2—), was synthesized from the reaction of dipicolinic acid, pydcH₂, (2, 6‐pyridinedicarboxylic acid), and guanidine hydrochloride, (GH⁺)(Cl^—). The characterization was performed using IR, ¹H and ¹³C NMR spectroscopy and single‐crystal X‐ray diffraction. LH₂ · H₂O crystallizes in the space group C2/c of the monoclinic system and contains eight molecules per unit cell. The unit cell dimensions are: a = 26.480(5)Å, b = 8.055(2)Å, c = 14.068(3)Å. The first coordination complex (GH)₂[Cd(pydc)₂] · 2H₂O, was prepared using LH₂ and cadmium(II) iodide, and characterized by ¹H and ¹³C NMR spectroscopy and X‐ray crystallography. The crystal system is triclinic with space group P1¯ with one molecule per unit cell. The unit cell dimensions are: a = 8.5125(7)Å, b = 11.0731(8)Å, c = 13.2404(10)Å. The cadmium(II) atom is six‐coordinated with a distorted octahedral geometry. The two pydc^2— units are almost perpendicular to each other. The protonation constants of the building blocks of the pydc‐guanidine adduct, the equilibrium constants for the reaction of pydc^2— with guanidine and the stoichiometry and stability of the Cd²⁺ complex with LH₂ in aqueous solution were accomplished by potentiometric pH titration. The solution studies strongly support a self‐association between pydc^2— and GH⁺ with a stoichiometry for the Cd^II complex similar to that observed for the isolated crystalline complex. In fact, the [Cd(pydc)₂]^2— complex was found as the most abundant species in solution (> 90 %) at a pH >5.     

High‐Efficiency Conversion of Trimethylsilyl Ethers to Their Corresponding Ethers using Carbon‐Based Solid Acid as a New Catalyst in Heterogeneous Mixtures

Carbon‐based solid acid was used as a new catalyst for conversion of trimethylsilyl ethers to their corresponding ethers in heterogeneous mixtures. The experiments were done moderately at room temperature, and high yields in suitable times were obtained under these conditions.     

Potentiometric and spectroscopic studies of three new mixed inorganic–organic hybrid materials based on Preyssler and Wells–Dawson heteropolyoxometalates containing proline, leucine, and asparagine

Three new organic–inorganic hybrid materials based on two important heteropolyoxometalates namely Preyssler (=K_12.5H_1.5[Na(H₂O)P₅W₃₀O₁₁₀]·35H₂O) and Wells–Dawson (=K₆[P₂W₁₈O₆₂]·10H₂O) anions, namely, (Hpro)₉(Hleu)₃K₂[Na(H₂O)P₅W₃₀O₁₁₀]·25H₂O (1), (Hpro)₄(Hasp)[HP₂W₁₈O₆₂]·20H₂O (2), and (Hpro)₁₁K₃[Na(H₂O)P₅W₃₀O₁₁₀]·18H₂O (3) where pro, leu, and asp are proline, leucine, and asparagine, respectively, were prepared and identified by elemental analysis, infrared and proton nuclear magnetic resonance spectroscopies, and thermogravimetric analysis. The hybrid materials are made up of positively charged amino acids, [Na(H₂O)P₅W₃₀O₁₁₀]^14? and [P₂W₁₈O₆₂]^6? anions, and H₂O molecules of crystallization. These constituents’ fragments held together into a three-dimensional supermolecular network through non-covalent interactions. The protonation constants of the amino acids used, and Preyssler and Wells–Dawson species in all possible protonated forms, the equilibrium constants for binary systems of proline–asparagine and proline–leucine, and the stoichiometry and stability constants of the corresponding binary and ternary hybrids with Preyssler and Wells–Dawson heteropolyoxometalates in aqueous solution were investigated by potentiometric pH titration method. The stoichiometries of the most hybrid species in solution were compared with the corresponding hybrids in the solid phase, in detail.     

CaCl2 as a bifunctional reusable catalyst: diversity-oriented synthesis of 4H-pyran library under ultrasonic irradiation

CaCl₂ is applied as an efficient reusable and eco-friendly bifunctional catalyst for the one-pot three-component synthesis of 4H-pyrans under ultrasonic irradiation. A broad range of substrates including the aromatic and heteroaromatic aldehydes, indoline-2,3-dione (isatin) derivatives, acenaphthylene-1,2-dione (acenaphthenequinone) and 2, 2-dihydroxy-2H-indene-1,3-dione (ninhydrin) were condensed with carbonyl compounds possessing a reactive ??-methylene group and alkylmalonates. All reactions are completed in short times, and the products are obtained in good to excellent yields. The catalyst could be recycled and reused several times without any loss of efficiency.     

Normal bases via general Gauss periods

Gauss periods have been used successfully as a tool for constructing normal bases in finite fields. Starting from a primitive th root of unity, one obtains under certain conditions a normal basis for over , where is a prime and for some integer . We generalize this construction by allowing arbitrary integers with , and find in many cases smaller values of than is possible with the previously known approach.

     

Magnetic losses of the soft magnetic composites consisting of iron and Ni–Zn ferrite

Ferromagnetic powders which are surrounded by an electrically insulating film (soft magnetic composites (SMCs)) exhibit unique magnetic properties, such as relatively low magnetic losses and 3D isotropic magnetic behavior. In some electromagnetic applications, including microwave frequency range applications, it is necessary to increase electrical resistivity without any noticeable reduction in magnetic properties. To achieve this purpose, electrically resistant materials, for example, ferrites with acceptable magnetic properties, are suitable candidates. This paper focuses on the effects of the synthesized Ni–Zn ferrite addition on the magnetic properties of the SMCs containing Ni–Zn ferrite within iron particles. The structure was studied by means of X-ray diffraction (XRD). The microstructure and the powder morphology were examined by the use of scanning electron microscopy (SEM). The magnetic measurements on powders and samples were carried out using a vibrating sample magnetometer (VSM) and an LCR meter, respectively. The results indicate that the lowest magnetic loss and the highest magnetic permeability are related to the composites with 20 wt% ferrite and 2 wt% ferrite, respectively. Also, the composites with 10 wt% ferrite show a good combination of magnetic loss and magnetic permeability in the range 0–500 kHz.     

Preparation of nanocrystalline Fe–Ni powders by mechanical alloying used in soft magnetic composites

This paper focuses on the preparation of nanocrystalline Fe–Ni powders by mechanical alloying method, which can be used in soft magnetic composites. Fe–10 wt% Ni and Fe–20  wt % Ni alloys were prepared using a high-energy ball mill. The magnetic properties of samples were measured by a B–H curve analyzer and microstructures of the samples were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The bcc Fe(Ni) phase formation was identified by XRD and completed after 45 h of milling. It was found that higher milling time resulted in, larger lattice parameter, higher microstrains and smaller crystallite sizes. Also, results showed that with increasing the milling time, coercivity increased and saturation intrinsic flux density firstly increased noticeably and then decreased in higher milling times (>70 h).     

Combination of cloud point extraction and flame atomic absorption spectrometry for preconcentration and determination of trace iron in environmental and biological samples

In the presented work, the conditions for cloud point extraction of iron from aqueous solutions using 7-iodo-8-hydroxyquinolin-5-sulphonic acid (Ferron) was investigated and optimized. The procedure is based on the separation of its ferron complex into the micellar media by adding the surfactant Triton X-114. After phase separation, the surfactant-rich phase was dissolved with 1.0 M HNO3 in methanol. Iron was determined by flame atomic absorption spectrometry. Optimization of the pH, ligand and surfactant quantities, incubation time, temperature, viscosity, sample volume, and interfering ions were investigated. The effects of the matrix ions were also examined. The detection limits for three times the standard deviations of the blank for iron was 0.4 ng m L-1, enrichment factor of 19.6 and preconcentration factor of 30 could be achieved. The validity of cloud point extraction was checked by employing real samples including soil, blood, spinach, milk, meat, liver and orange juice samples using the standard addition method, which gave satisfactory results.In the presented work, the conditions for cloud point extraction of iron from aqueous solutions using 7-iodo-8-hydroxyquinolin-5-sulphonic acid (Ferron) was investigated and optimized. The procedure is based on the separation of its ferron complex into the micellar media by adding the surfactant Triton X-114. After phase separation, the surfactant-rich phase was dissolved with 1.0 M HNO₃ in methanol. Iron was determined by flame atomic absorption spectrometry. Optimization of the pH, ligand and surfactant quantities, incubation time, temperature, viscosity, sample volume, and interfering ions were investigated. The effects of the matrix ions were also examined. The detection limits for three times the standard deviations of the blank for iron was 0.4 ng m L⁻¹, enrichment factor of 19.6 and preconcentration factor of 30 could be achieved. The validity of cloud point extraction was checked by employing real samples including soil, blood, spinach, milk, meat, liver and orange juice samples using the standard addition method, which gave satisfactory results.