Synthesis of Novel Tetra(µ3-Methoxo) Bridged with [Cu(II)-O-Cd(II)] Double-Open-Cubane Cluster: XRD/HSA-Interactions, Spectral and Oxidizing Properties

A new double-open-cubane core Cd(II)-O-Cu(II) bimetallic ligand mixed cluster of type [Cl2Cu4Cd2(NNO)6(NN)2(NO3)2].CH3CN was made available in EtOH/CH3CN solution. The 1-hydroxymethyl-3,5-dimethylpyrazole (NNOH) and 3,5-dimethylpyrazole (NNH) act as N,O-polydentate anion ligands in coordinating the Cu(II) and Cd(II) centers. The structure of the cluster in the solid state was proved by XRD study and confirmed in the liquid state by UV-vis analysis. The XRD result supported the construction of two octahedral and one square pyramid geometries types around the four Cu(II) centers and only octahedral geometry around Cd(II) two centers. Interestingly, NNOH ligand acts as a tetra-µ3-oxo and tri-µ2-oxo ligand; meanwhile, the N-N in NNH acts as classical bidentate anion/neutral ligands. The interactions in the lattice were detected experimentally by the XRD-packing result and computed via Hirschfeld surface analysis (HSA). The UV-vis., FT-IR and Energy Dispersive X-ray (EDX), supported the desired double-open cubane cluster composition. The oxidation potential of the desired cluster was evaluated using a 3,5-DTB-catechol 3,5-DTB-quinone as a catecholase model reaction.

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Synthesis and characterization of a macrocyclic copper complex containing the 14-membered 1,3,5,8,10,12-hexaazacyclotetradecane unit

Zeitschrift für Naturforschung B ◽

10.1515/znb-2016-0199 ◽

2017 ◽

Vol 72 (2) ◽

pp. 115-118 ◽

Cited By ~ 8

Author(s):

Mohammad Hakimi ◽

Zahra Mardani ◽

Keyvan Moeini ◽

Fabian Mohr

Keyword(s):

Raman Spectroscopy ◽

Elemental Analysis ◽

Copper Complex ◽

Copper Atom ◽

Octahedral Geometry ◽

Synthesis And Characterization ◽

X Ray Diffraction ◽

X Ray ◽

Ft Ir

AbstractIn this work, a new macrocyclic copper complex, [Cu(ACE)(SCN)2]; ACE: 1,3,6,10,12,15-hexaazatricyclo[13.3.1.16,10]eicosane, was prepared and characterized by elemental analysis, FT-IR, Raman spectroscopy and single-crystal X-ray diffraction. X-ray analysis of [Cu(ACE)(SCN)2] reveals an elongated octahedral geometry around the copper atom in a centrosymmetric CuN6 environment.

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Structural and spectral study of coordination of 4,4′-dimethoxy-2,2′-bipyridine toward Zn(II) and Cd(II) containing thiocyanato or azido ligands

Zeitschrift für Naturforschung B ◽

10.1515/znb-2016-0083 ◽

2016 ◽

Vol 71 (9) ◽

pp. 959-965 ◽

Cited By ~ 5

Author(s):

Farzin Marandi ◽

Keyvan Moeini ◽

Hadi Amiri Rudbari

Keyword(s):

Crystal Structure ◽

Nmr Spectroscopy ◽

Octahedral Geometry ◽

Distorted Octahedral Geometry ◽

X Ray ◽

X Ray Crystallography ◽

Distorted Octahedral ◽

Ft Ir ◽

New Compounds ◽

C Nmr

AbstractThree new compounds of zinc(II) and cadmium(II) with the ligand 4,4′-dimethoxy-2,2′-bipyridine (4,4′-dmo-2,2′-bpy), including cis-[Zn(4,4′-dmo-2,2′-bpy)2(SCN)2] (1), cis-[Cd(4,4′-dmo-2,2′-bpy)2(SCN)2] (2), and [Cd3(4,4′-dmo-2,2′-bpy)3(N3)5(OAc)]n (3), have been obtained as white single crystals by the branched tube method and characterized by elemental analysis, FT-IR and 1H, 13C NMR spectroscopy, and X-ray crystallography. Single-crystal structure analyses of the isostructural complexes 1 and 2 showed distorted octahedral geometry for zinc(II) and cadmium(II) with ZnN6 and CdN6 environments. Complex 3 reveals a rare coordination polymer containing octahedrally coordinated cadmium(II) expanding to chains by two different bridging modes, including Cd‒O‒C‒O‒Cd and Cd‒N‒Cd.

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Synthesis and structural characterization of the complexes of 2-(menthoxycarbonyl)ethyltin chloride

Main Group Metal Chemistry ◽

10.1515/mgmc-2019-0003 ◽

2019 ◽

Vol 42 (1) ◽

pp. 37-45

Author(s):

Yichao Lin ◽

Minghui Guo ◽

Jin Liu ◽

Laijin Tian ◽

Xicheng Liu

Keyword(s):

Oxygen Atom ◽

Carbonyl Oxygen ◽

Octahedral Geometry ◽

Phen Ligand ◽

X Ray Diffraction ◽

Centrosymmetric Dimer ◽

X Ray ◽

Ester Moiety ◽

Ft Ir

AbstractThe complexes of 2-(menthoxycarbonyl)ethyltin chloride, MenOCOCH2CH2SnCl3⋅L (Men = Menthyl, L = benzyl phenyl sulfoxide (bpSO), 1; 2,2’-bipyridine (bpy), 2; 1,10-phenanthroline (phen), 3) and [MenOCOCH2CH2SnCl2(OCH3)]2 (4), have been synthesized and characterized by means of elemental analysis, FT-IR, NMR (1H, 13C and 119Sn) spectra. The crystal structures of 1, 3 and 4 have been determined by single crystal X-ray diffraction. The tin atoms in 1-4 are all hexa-coordinated. The tin atom in 1 adopts a distorted [CSnCl3O2] octahedral geometry with an oxygen atom of the ligand and an intramolecular coordination of the oxygen atom from the carbonyl group to the tin atom. Complex 3 possesses a distorted [CSnCl3N2] octahedral geometry with two nitrogen atoms of a chelating phen ligand. The carbonyl oxygen atom of the ester moiety is not coordinating. Compound 4 is a centrosymmetric dimer with a four-membered Sn2O2 ring, and the tin atom has a distorted [CSnCl2O3] octahedral geometry with an intramolecular C=O→Sn coordination and intermolecular methoxy bridging.

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Synthesis, Characterization, and Photocatalytic Activity of Microspheres Functionalized with Porphyrin

International Journal of Photoenergy ◽

10.1155/2012/348292 ◽

2012 ◽

Vol 2012 ◽

pp. 1-10 ◽

Cited By ~ 18

Author(s):

Jin-Hua Cai ◽

Jin-Wang Huang ◽

Han-Cheng Yu ◽

Liang-Nian Ji

Keyword(s):

Photocatalytic Activity ◽

Visible Light ◽

Photoelectron Spectroscopy ◽

Diffuse Reflectance ◽

Diffuse Reflectance Spectroscopy ◽

Reflectance Spectroscopy ◽

Model Reaction ◽

X Ray Diffraction ◽

X Ray ◽

Ft Ir

In order to utilize visible light more efficiently in the photocatalytic reaction, microspheres sensitized by 5-(4-allyloxy)phenyl-10,15,20-tri(4-methylphenyl)porphyrin (APTMPP) were prepared and characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), nitrogen physisorption, scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR) and UV-vis diffuse reflectance spectroscopy, and so forth, The characterization results indicated that APTMPP-MPS- was composed of the anatase crystal phase. The morphology of the composite materials was spheriform with size of 0.3–0.7 μm and the porphyrin was chemisorbed on the surface of through a Si–O–Ti bond. The photooxidation ofα-terpinene was employed as the model reaction to evaluate the photocatalytic activity of APTMPP-MPS- microspheres under visible light. The results indicated that the photodegradation ofα-terpinene was significantly enhanced in the presence of the APTMPP-MPS- compared with the nonmodified under visible light.

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Synthesis and Evaluation of Levulinic Ester as Biodiesel Additives

Revista de Chimie ◽

10.37358/rc.20.8.8275 ◽

2020 ◽

Vol 71 (8) ◽

pp. 21-26

Author(s):

Elena-Emilia Oprescu ◽

Cristina-Emanuela Enascuta ◽

Elena Radu ◽

Vasile Lavric

Keyword(s):

Maximum Yield ◽

Strength Distribution ◽

Point Of View ◽

Reaction Parameters ◽

X Ray ◽

Ethyl Levulinate ◽

Ft Ir ◽

Ir Analysis ◽

Biodiesel Blend ◽

Acid Strength Distribution

In this study, the SO42-/TiO2-La2O3-Fe2O3 catalyst was prepared and tested in the conversion of fructose to ethyl levulinate . The catalyst was characterized from the point of view of the textural analysis, FT-IR analysis, acid strength distribution, X-ray powder diffraction and pyridine adsorption IR spectra. The influence of the reaction parameters on the ethyl levulinate yield was study. The maximum yield of 37.95% in levulinate esters was obtained at 180 �C, 2 g catalyst and 4 h reaction time. The effect of ethyl levulinate addition to diesel-biodiesel blend in different rates, i.e, 0.5, 1, 2.5, 5 (w.t %) on density, kinematic viscosity and flash point was evaluated and compared with the European specification.

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Thermal Behaviour of Candesartan Active substance and in pharmaceutical compounds

Revista de Chimie ◽

10.37358/rc.17.8.5787 ◽

2017 ◽

Vol 68 (8) ◽

pp. 1895-1902

Author(s):

Ioana Cristina Tita ◽

Eleonora Marian ◽

Bogdan Tita ◽

Claudia Crina Toma ◽

Laura Vicas

Keyword(s):

Thermal Behaviour ◽

Active Substance ◽

Pharmaceutical Research ◽

Pharmaceutical Product ◽

Nitrogen Atmosphere ◽

Pure Substance ◽

Scanning Calorimetry ◽

X Ray ◽

Ft Ir

Thermal analysis is one of the most frequently used instrumental techniques in the pharmaceutical research, for the thermal characterization of different materials from solids to semi-solids, which are of pharmaceutical relevance. In this paper, simultaneous thermogravimetry/derivative thermogravimetry (TG/DTG) and differential scanning calorimetry (DSC) were used for characterization of the thermal behaviour of candesartan cilexetil � active substance (C-AS) under dynamic nitrogen atmosphere and nonisothermal conditions, in comparison with pharmaceutical product containing the corresponding active substance. It was observed that the commercial samples showed a different thermal profile than the standard sample, caused by the presence of excipients in the pharmaceutical product and to possible interaction of these with the active substance. The Fourier transformed infrared spectroscopy (FT-IR) and X-ray powder diffraction (XRPD) were used as complementary techniques adequately implement and assist in interpretation of the thermal results. The main conclusion of this comparative study was that the TG/DTG and DSC curves, together with the FT-IR spectra, respectively X-ray difractograms constitute believe data for the discrimination between the pure substance and pharmaceutical forms.

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Photocatalytic Reduction of CO2 to Methanol Using a Copper-Zirconia Imidazolate Framework

Catalysts ◽

10.3390/catal11030346 ◽

2021 ◽

Vol 11 (3) ◽

pp. 346

Author(s):

Sonam Goyal ◽

Maizatul Shima Shaharun ◽

Ganaga Suriya Jayabal ◽

Chong Fai Kait ◽

Bawadi Abdullah ◽

...

Keyword(s):

Photoelectron Spectroscopy ◽

Catalyst Support ◽

Oxidation Potential ◽

Molar Ratio ◽

X Ray Diffraction ◽

X Ray ◽

Molar Ratios ◽

Optimum Parameters ◽

Reduction Of Co2 ◽

Enhanced Yield

A set of novel photocatalysts, i.e., copper-zirconia imidazolate (CuZrIm) frameworks, were synthesized using different zirconia molar ratios (i.e., 0.5, 1, and 1.5 mmol). The photoreduction process of CO2 to methanol in a continuous-flow stirred photoreactor at pressure and temperature of 1 atm and 25 °C, respectively, was studied. The physicochemical properties of the synthesized catalysts were studied using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and photoluminescence (PL) spectroscopy. The highest methanol activity of 818.59 µmol/L.g was recorded when the CuZrIm1 catalyst with Cu/Zr/Im/NH4OH molar ratio of 2:1:4:2 (mmol/mmol/mmol/M) was employed. The enhanced yield is attributed to the presence of Cu2+ oxidation state and the uniformly dispersed active metals. The response surface methodology (RSM) was used to optimize the reaction parameters. The predicted results agreed well with the experimental ones with the correlation coefficient (R2) of 0.99. The optimization results showed that the highest methanol activity of 1054 µmol/L.g was recorded when the optimum parameters were employed, i.e., stirring rate (540 rpm), intensity of light (275 W/m2) and photocatalyst loading (1.3 g/L). The redox potential value for the CuZrIm1 shows that the reduction potential is −1.70 V and the oxidation potential is +1.28 V for the photoreduction of CO2 to methanol. The current work has established the potential utilization of the imidazolate framework as catalyst support for the photoreduction of CO2 to methanol.

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Enhancement of Chloroprene/Natural/Butadiene Rubber Nanocomposite Properties Using Organoclays and Their Combination with Carbon Black as Fillers

Polymers ◽

10.3390/polym13071085 ◽

2021 ◽

Vol 13 (7) ◽

pp. 1085

Author(s):

Patricia Castaño-Rivera ◽

Isabel Calle-Holguín ◽

Johanna Castaño ◽

Gustavo Cabrera-Barjas ◽

Karen Galvez-Garrido ◽

...

Keyword(s):

Mechanical Properties ◽

Carbon Black ◽

High Performance ◽

Rubber Matrix ◽

Butadiene Rubber ◽

X Ray Diffraction ◽

X Ray ◽

Rubber Blends ◽

Ft Ir ◽

Chloroprene Rubber

Organoclay nanoparticles (Cloisite® C10A, Cloisite® C15) and their combination with carbon black (N330) were studied as fillers in chloroprene/natural/butadiene rubber blends to prepare nanocomposites. The effect of filler type and load on the physical mechanical properties of nanocomposites was determined and correlated with its structure, compatibility and cure properties using Fourier Transformed Infrared (FT-IR), X-ray Diffraction (XRD), Thermogravimetric Analysis (TGA) and rheometric analysis. Physical mechanical properties were improved by organoclays at 5–7 phr. Nanocomposites with organoclays exhibited a remarkable increase up to 46% in abrasion resistance. The improvement in properties was attributed to good organoclay dispersion in the rubber matrix and to the compatibility between them and the chloroprene rubber. Carbon black at a 40 phr load was not the optimal concentration to interact with organoclays. The present study confirmed that organoclays can be a reinforcing filler for high performance applications in rubber nanocomposites.

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Release of toxic methylene blue from water by mesoporous silicalite-1: characterization, kinetics and isotherm studies

Applied Water Science ◽

10.1007/s13201-021-01435-z ◽

2021 ◽

Vol 11 (7) ◽

Author(s):

Sabarish Radoor ◽

Jasila Karayil ◽

Aswathy Jayakumar ◽

Jyotishkumar Parameswaranpillai ◽

Suchart Siengchin

Keyword(s):

Electron Microscopy ◽

Contact Time ◽

Dye Removal ◽

Batch Adsorption ◽

Aqueous Environment ◽

Order Kinetic ◽

Adsorption Method ◽

X Ray ◽

Ft Ir ◽

Adsorption Desorption

AbstractIn the present work, we have developed a mesoporous silicalite-1 using CMC as a template for the removal of MB from aqueous solution. The synthesized silicalite-1 were characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), Energy-dispersive X-ray spectroscopy (EDAX) and N2 adsorption–desorption isotherm (BET). XRD and FT-IR analysis confirmed the formation of crystallinity and development of MFI structure in the mesoporous silicalite-1. The adsorption of MB dye on mesoporous silicalite-1 was conducted by batch adsorption method. The effect of various parameters such as adsorbent dosage, initial dye concentration, contact time and temperature on the dye uptake ability of silicalite-1 was investigated. The operating parameters for the maximum adsorption are silicalite-1 dosage (0.1 wt%), contact time (240 min), initial dye concentration (10 ppm) and temperature (30 ℃). The MB dye removal onto mesoporous silicalite-1 followed pseudo-second-order kinetic and Freundlich isotherm. The silicalite-1 exhibits 86% removal efficiency even after six adsorption–desorption cycle. Therefore, the developed mesoporous silicalite-1 is an effective eco-friendly adsorbent for MB dye removal from aqueous environment.

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Electrospun Nanosystems Based on PHBV and ZnO for Ecological Food Packaging

Polymers ◽

10.3390/polym13132123 ◽

2021 ◽

Vol 13 (13) ◽

pp. 2123

Author(s):

Maria Râpă ◽

Maria Stefan ◽

Paula Popa ◽

Dana Toloman ◽

Cristian Leostean ◽

...

Keyword(s):

Food Packaging ◽

Spin Trapping ◽

X Ray Diffraction ◽

Paramagnetic Resonance ◽

Hno3 Solution ◽

X Ray ◽

Trapping Method ◽

Ft Ir ◽

Doped Zno ◽

Electron Paramagnetic

The electrospun nanosystems containing poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) and 1 wt% Fe doped ZnO nanoparticles (NPs) (with the content of dopant in the range of 0–1 wt% Fe) deposited onto polylactic acid (PLA) film were prepared for food packaging application. They were investigated by scanning electron microscopy (SEM), energy dispersive X-ray (EDX), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), antimicrobial analysis, and X-ray photoelectron spectrometry (XPS) techniques. Migration studies conducted in acetic acid 3% (wt/wt) and ethanol 10% (v/v) food simulants as well as by the use of treated ashes with 3% HNO3 solution reveal that the migration of Zn and Fe falls into the specific limits imposed by the legislation in force. Results indicated that the PLA/PHBV/ZnO:Fex electrospun nanosystems exhibit excellent antibacterial activity against the Pseudomonas aeruginosa (ATCC-27853) due to the generation of a larger amount of perhydroxyl (˙OOH) radicals as assessed using electron paramagnetic resonance (EPR) spectroscopy coupled with a spin trapping method.

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