Crystal structure and thermal behavior of isostructural binary complexes [Rh(en)3][Fe(CN)6] and [Rh(en)3][Cо(CN)6]

2018 ◽  
Vol 233 (1) ◽  
pp. 35-40 ◽  
Author(s):  
Pechenyuk Sophia ◽  
Zolotarev Andrey ◽  
Semushina Julia ◽  
Gosteva Alevtina
Keyword(s):  
Thermal Behavior ◽  
Thermal Analyses ◽  
Complex Compounds ◽  
Binary Complex ◽  
X Ray Diffraction ◽  
Monoclinic Crystal ◽  
Air Atmosphere ◽  
Binary Complexes ◽  
Higher Temperature ◽  
Heating Up

Abstract Binary complex compounds (BCC) [Rh(en)3][Fe(CN)6]·2H2O (I) and [Rh(en)3][Co(CN)6]·2H2O (II) have been prepared and characterized by the X-ray diffraction, crystal optic, elemental and thermal analyses. The crystal structures I and II (space group P21/n) are described within the monoclinic crystal system, are insular and isostructural. The thermal behavior of BCC I and II is identical, with an exception of a higher temperature (~by 50°C) of II decomposition. In air atmosphere, the ligand removal is followed by the formation of, respectively, Rh+1/2Fe2O3 and Rh+Co that on further heating up to 1000°C convert into RhFeO3 and RhCoO1.5. The residues of annealing at 1000°C in argon atmosphere are Rh+1/2Fe2O3 and Rh+CoO, respectively.

scholarly journals Synthesis, characterization and electroluminescence properties of a new mixed-ligand diorganotin(IV) complex

2019 ◽  
Vol 42 (1) ◽  
pp. 51-59 ◽  
Author(s):  
Asiyeh Mahmoudpour ◽  
Shohreh Nafisi ◽  
Ezzatollah Najafi ◽  
Behrouz Notash
Keyword(s):  
Thermal Behavior ◽  
Optical Devices ◽  
Uv Spectra ◽  
Mixed Ligand ◽  
X Ray Diffraction ◽  
Monoclinic System ◽  
Light Emitting ◽  
X Ray ◽  
Air Atmosphere ◽  
Ammonium N

Abstract A new mixed-ligand diorganotin(IV) complex, [μ-(4-dpe){Me2Sn(cup)2}2] (1), was synthesized by reacting dimethyltin(IV) dichloride with 1,2-di(4-pyridyl)ethylene (4-dpe) and ammonium N-Nitroso-N-phenylhydroxylamine (cup). The prepared complex was fully characterized by PXRD, 1H, 13C and 119Sn NMR, IR, and UV spectra and elemental analysis (CHN). The structural analysis of complex 1 by X-ray diffraction showed that this compound consists of centrosymmetric binuclear units that crystallize in the monoclinic system with the space group of P21/c. Thermal behavior of this complex was interrogated by thermogravimetric and differential thermal analysis (TGA and DTA) under air atmosphere. The study of thermal behavior and luminescence properties of prepared diorganotin(IV) complex exhibited that this complex can be used as a emitting layer in the preparation of optical devices. The prepared coordination compound was used in two different concentrations in the manufacture of two light-emitting diodes (OLEDs).

scholarly journals Thermal behaviour studies of solid state compounds of cinnamylidenepyruvate with trivalent lanthanides and yttrium (III) in an atmosphere of CO2

2002 ◽  
Vol 27 (0) ◽  
Author(s):  
José Dilson Silva de OLIVEIRA ◽  
Fernando Luís FERTONANI ◽  
Cristo Bladimiros MELIOS ◽  
Massao IONASHIRO
Keyword(s):  
Solid State ◽  
Thermal Behavior ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Trivalent Lanthanides ◽  
Air Atmosphere ◽  
Behavior Study ◽  
Derivative Thermogravimetry ◽  
Co2 Atmosphere

Solid state cinnamylidenepyruvate of trivalent lanthanides (except for promethium) and yttrium, were prepared. Thermogravimetry, derivative thermogravimetry (TG, DTG), differential scanning calorimetry (DSC), X-ray diffraction powder patterns and complexometry were used to characterize and to study the thermal behavior of these compounds in a dynamic CO2 atmosphere. The results obtained showed significative differences on the thermal stability and thermal decomposition of these compounds, with regard to the thermal behavior study in a dynamic air atmosphere.

Synthesis, Crystal Structure and Thermal Properties of Copper(II) Orotato Complex with 2,2’-Bipyridine

2005 ◽  
Vol 60 (11) ◽  
pp. 1138-1142 ◽  
Author(s):  
Okan Zafer Yeşilel ◽  
Halis Ölmez ◽  
Hasan İçbudak ◽  
Orhan Büyükgüngör
Keyword(s):  
Diffraction Analysis ◽  
Thermal Analyses ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Carboxylate Oxygen ◽  
Air Atmosphere ◽  
Dimensional Network ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

A mixed-ligand orotato (HOr) complex of Cu(II) with 2,2’-bipyridine (bipy) was synthesized and characterized by elemental analysis, magnetic susceptibility, UV-vis and FT-IR spectroscopy, TG / DTA techniques and X-ray diffraction analysis. X-Ray diffraction analysis has shown that the squarepyramidal five-coordinate copper atom is chelated by the deprotonated N3 pyrimidine atom and the carboxylate oxygen atom of the bidentate orotato dianion, and to the two nitrogen atoms of the 2,2’- bipyridine molecule. A water molecule is attached above the N3O plane. Thermal analyses showed that the title compound decomposes in two steps over the range 20 - 1000 °C on heating in a static air atmosphere. Intermolecular hydrogen-bonds and π-ring interactions lead to the formation of a three-dimensional network.

scholarly journals Synthesis, structural characterization and luminescence properties of 1-carboxymethyl-3-ethylimidazolium chloride

2018 ◽  
Vol 74 (6) ◽  
pp. 653-658 ◽  
Author(s):  
Denis Prodius ◽  
Magdalena Wilk-Kozubek ◽  
Anja-Verena Mudring
Keyword(s):  
Hydrogen Bonds ◽  
Thermal Analyses ◽  
Three Dimensional ◽  
Attenuated Total Reflectance ◽  
X Ray Diffraction ◽  
Imidazolium Chloride ◽  
Air Atmosphere ◽  
Ft Ir ◽  
Fourier Transform Ir ◽  
Ethylimidazolium Chloride

A microcrystalline carboxyl-functionalized imidazolium chloride, namely 1-carboxymethyl-3-ethylimidazolium chloride, C7H11N2O2 +·Cl−, has been synthesized and characterized by elemental analysis, attenuated total reflectance Fourier transform IR spectroscopy (ATR-FT-IR), single-crystal X-ray diffraction, thermal analysis (TGA/DSC), and photoluminescence spectroscopy. In the crystal structure, cations and anions are linked by C—H...Cl and C—H...O hydrogen bonds to create a helix along the [010] direction. Adjacent helical chains are further interconnected through O—H...Cl and C—H...O hydrogen bonds to form a (10\overline{1}) layer. Finally, neighboring layers are joined together via C—H...Cl contacts to generate a three-dimensional supramolecular architecture. Thermal analyses reveal that the compound melts at 449.7 K and is stable up to 560.0 K under a dynamic air atmosphere. Photoluminescence measurements show that the compound exhibits a blue fluorescence and a green phosphorescence associated with spin-allowed (1π←1π*) and spin-forbidden (1π←3π*) transitions, respectively. The average luminescence lifetime was determined to be 1.40 ns for the short-lived (1π←1π*) transition and 105 ms for the long-lived (1π←3π*) transition.

scholarly journals THERMAL BEHAVIOR OF DOUBLE COMPLEXES [Co(NH3)6][Fe(CN)6] AND [CO(en)3][Fe(CN)6]·2H2O

2018 ◽  
Vol 61 (4-5) ◽  
pp. 49 ◽  
Author(s):  
Sofiya I. Pechenyuk ◽  
Denis P. Domonov ◽  
Alevtina N. Gosteva ◽  
Yuliya P. Semushina ◽  
Alexey A. Shimkin
Keyword(s):  
Thermal Behavior ◽  
Gaseous Medium ◽  
Complex Compounds ◽  
Partial Reduction ◽  
Double Complex ◽  
Temperature Range ◽  
Air Atmosphere ◽  
Temperature Ranges ◽  
Double Complex Compounds ◽  
Neutral Ligands

Thermal behavior of double complex compounds (DCC) of first transition metal row has been studied on the example of [СоA6][Fe(CN)6] (A = NH3, C2H8N2/2) in oxidative(air), inert(argon, nitrogen, helium) and reductive(hydrogen) atmospheres. The analysis of solid and gaseous thermolysis products has been performed for separate temperature ranges. The TG curves of the thermolysis first stage coincide with each other for all the investigated atmospheres up to approximately 300 °C. DCC [Со(NH3)6][Fe(CN)6] (I) and [Со(en)3][Fe(CN)6] (II) undergo to first stage of thermal decomposition with the removal of the part of neutral ligands and 1-2, but not more as 3 CN groups in temperature range of 160-300 and 200-350°С in oxidative and 160-400 and 210-550 °С, in inert medium, respectively. DCC I forms the intermediate [(NH3)2CoFeC4N3], [(NH3)2.6CoFe(CN)5] and [(NH3)3CoFe(CN)4.3] at 330, 350 и 430 °С in atmosphere of air, argon and hydrogen. For DCC II the intermediates are not registered. At temperatures above 300 °C the TG curves diverge and relate already to the interaction of thermolysis products with the gaseous medium. The thermolysis in argon and hydrogen is accompanied by partial reduction of ligands and central atoms of DCCs, thermolysis in the air atmosphere - complete oxidation of ligands and central ions. The thermal behavior of DCC is compared with the thermal behavior of 3d metals cationic complexes on base of literature data. The thermolysis of all the DCC and cation complexes discussed here proceeds with the removal of neutral ligands in the temperature range of 50-400 °C. For citation:Pechenyuk S.I., Domonov D.P., Gosteva A.N., Semushina Yu.P., Shimkin A.A. Thermal behavior of double complexes [Co(NH3)6][Fe(CN)6] and [Co(en)3][Fe(CN)6]·2H2O. Izv. Vyssh. Uchebn. Zaved. Khim. Khim. Tekhnol. 2018. V. 61. N 4-5. P. 49-56

scholarly journals Product Prediction: Intermediates Formed During Rare Earth Reactions

2017 ◽  
Vol 58 (1) ◽  
Author(s):  
Rodrigo Castañeda ◽  
Elizabeth Chavira ◽  
Oscar Peralta
Keyword(s):  
Rare Earth ◽  
Solid State ◽  
High Resolution ◽  
Thermal Behavior ◽  
Thermal Analyses ◽  
Experimental Results ◽  
Solid State Reactions ◽  
X Ray Diffraction ◽  
X Ray

<p>Thermal analyses, X-ray diffraction (XRD), and HR-XRD (High Resolution XRD) were used to identify thermal behavior products in a family of solid-state reactions involving rare earth (REE) reagents. REE where sorted in light and heavy groups. The general reactions under study were: REE<sub>2</sub>O<sub>3</sub> + Fe<sub>2</sub>O<sub>3</sub> + As<sub>2</sub>O<sub>3</sub> → 2REEFeO<sub>3</sub> +<br />As<sub>2</sub>O<sub>3</sub>↑ and 2REE(OH)<sub>3</sub> + Fe<sub>2</sub>O<sub>3</sub> + As<sub>2</sub>O<sub>3</sub> → 2REEFeO<sub>3</sub> + As<sub>2</sub>O<sub>3</sub>↑ + 3H<sub>2</sub>O↑, REE= La, Ce, Nd, Sm, Gd, Dy, Ho, Er, and Yb. Based on the experimental results, it is possible to predict the different compounds of REE products in a series of reactions analyzing only three of the reactions, two for light REE and one for heavy REE.</p>

ON THE MECHANISMS OF POROUS SILICON COMBUSTION IN OXYGEN AND AIR ATMOSPHERE WHEN SODIUM PERCHLORATE IS INCORPORATED IN PORES

2020 ◽  
Author(s):  
V. N. MIRONOV ◽  
◽  
O. G. PENYAZKOV ◽  
P. N. KRIVOSHEYEV ◽  
I. A. IVANOV ◽  
...  
Keyword(s):  
Porous Silicon ◽  
Porous Layer ◽  
Sodium Perchlorate ◽  
Spark Ignition ◽  
Joule Heat ◽  
Air Atmosphere ◽  
Breakdown Region ◽  
Ignition And Combustion ◽  
Heating Up

The processes of pSi ignition and combustion in oxygen are described. When spark ignition in the porous layer releases the Joule heat, it leads to a significant heating-up of the breakdown region.

New Coordination Compounds of Fe(III) with Organic Ligands

2009 ◽  
Vol 59 (12) ◽  
Author(s):  
Mihaela Flondor ◽  
Ioan Rosca ◽  
Doina Sibiescu ◽  
Mihaela-Aurelia Vizitiu ◽  
Daniel-Mircea Sutiman ◽  
...  
Keyword(s):  
Chemical Analysis ◽  
Complex Compounds ◽  
Organic Ligands ◽  
X Ray Diffraction ◽  
X Ray ◽  
Elemental Chemical Analysis ◽  
Structural Formulae ◽  
Paramagnetic Properties

In this paper the synthesis and the study of some complex compounds of Fe(III) with ligands derived from: 2-(4-chloro-phenylsulfanyl)-1-(2-hydroxy-3,5-diiodo-phenyl)-ethanone (HL1), 1-(3,5-dibromo-2-hydroxy-phenyl)-2-phenylsulfanyl-ethanone(HL2), and 2-(4-chloro-phenylsulfanyl)-1-(3,5-dibromo-2-hydroxy-phenyl)-ethanone (HL3) is presented. The characterization of these complexes is based on method as: the elemental chemical analysis, IR and ESR spectroscopy, M�ssbauer, the thermogravimetric analysis and X-ray diffraction. Study of the IR and chemical analysis has evidenced that the precipitates form are a complexes and the combination ratio of M:L is 1:2. The central atoms of Fe(III) presented paramagnetic properties and a octaedric hybridization. Starting from this precipitation reactions, a method for the gravimetric determination of Fe(III) with this organic ligands has been possible. Based on the experimental data on literature indications, the structural formulae of the complex compounds are assigned.

scholarly journals One-step synthesis of nitrogen-grafted copper-gallic acid for enhanced methylene blue removal

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Shella Permatasari Santoso ◽  
Vania Bundjaja ◽  
Artik Elisa Angkawijaya ◽  
Chintya Gunarto ◽  
Alchris Woo Go ◽  
...  
Keyword(s):  
Methylene Blue ◽  
Adsorption Capacity ◽  
Gallic Acid ◽  
Synthesis Method ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Temperature Dependent ◽  
One Step ◽  
Detailed Assessment ◽  
Higher Temperature

AbstractNitrogen-grafting through the addition of glycine (Gly) was performed on a metal- phenolic network (MPN) of copper (Cu2+) and gallic acid (GA) to increase its adsorption capacity. Herein, we reported a one-step synthesis method of MPN, which was developed according to the metal–ligand complexation principle. The nitrogen grafted CuGA (Ng-CuGA) MPN was obtained by reacting Cu2+, GA, and Gly in an aqueous solution at a molar ratio of 1:1:1 and a pH of 8. Several physicochemical measurements, such as Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), N2 sorption, X-ray diffraction (XRD), and thermal gravimetry analysis (TGA), were done on Ng-CuGA to elucidate its characteristics. The analysis revealed that the Ng-CuGA has non-uniform spherical shaped morphology with a pore volume of 0.56 cc/g, a pore size of 23.25 nm, and thermal stability up to 205 °C. The applicational potential of the Ng-CuGA was determined based on its adsorption capacity against methylene blue (MB). The Ng-CuGA was able to adsorb 190.81 mg MB per g adsorbent at a pH of 6 and temperature of 30 °C, which is 1.53 times higher than the non-grafted CuGA. Detailed assessment of Ng-CuGA adsorption properties revealed their pH- and temperature-dependent nature. The adsorption capacity and affinity were found to decrease at a higher temperature, demonstrating the exothermic adsorption behavior.

scholarly journals Impact of high temperatures on aluminoceladonite studied by Mössbauer, Raman, X-ray diffraction and X-ray photoelectron spectroscopy

2021 ◽  
Author(s):  
Mariola Kądziołka-Gaweł ◽  
Maria Czaja ◽  
Mateusz Dulski ◽  
Tomasz Krzykawski ◽  
Magdalena Szubka
Keyword(s):  
Photoelectron Spectroscopy ◽  
Integral Intensity ◽  
Photoelectron Spectra ◽  
X Ray Diffraction ◽  
Structural Reorganization ◽  
Oh Groups ◽  
X Ray ◽  
Al Content ◽  
Integral Intensity Ratio ◽  
Higher Temperature

AbstractMössbauer, Raman, X-ray diffraction and X-ray photoelectron spectroscopies were used to examine the effects of temperature on the structure of two aluminoceladonite samples. The process of oxidation of Fe2+ to Fe3+ ions started at about 350 °C for the sample richer in Al and at 300 °C for the sample somewhat lower Al-content. Mössbauer results show that this process may be associated with dehydroxylation or even initiate it. The first stage of dehydroxylation takes place at a temperature > 350 °C when the adjacent OH groups are replaced with a single residual oxygen atom. Up to ~500 °C, Fe ions do not migrate from cis-octahedra to trans-octahedra sites, but the coordination number of polyhedra changes from six to five. This temperature can be treated as the second stage of dehydroxylation. The temperature dependence on the integral intensity ratio between bands centered at ~590 and 705 cm−1 (I590/I705) clearly reflects the temperature at which six-coordinated polyhedra are transformed into five-coordinated polyhedra. X-ray photoelectron spectra obtained in the region of the Si2p, Al2p, Fe2p, K2p and O1s core levels, highlighted a route to identify the position of Si, Al, K and Fe cations in a structure of layered silicates with temperature. All the measurements show that the sample with a higher aluminum content and a lower iron content in octahedral sites starts to undergo a structural reorganization at a relatively higher temperature than the less aluminum-rich sample does. This suggests that iron may perform an important role in the initiation of the dehydroxylation of aluminoceladonites.

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