scholarly journals Synthesis, Molecular and Supramolecular Structures of New Cd(II) Pincer-Type Complexes with s-TriazineCore Ligand

Crystals ◽  
2019 ◽  
Vol 9 (5) ◽  
pp. 226 ◽  
Author(s):  
Soliman ◽  
Almarhoon ◽  
El-Faham
Keyword(s):  
Metal Ions ◽  
13C Nmr Spectroscopy ◽  
X Ray Diffraction ◽  
Thermal Stabilities ◽  
Large Size ◽  
Distorted Octahedral ◽  
Hirshfeld Analysis ◽  
Chloride Ligand ◽  
Coordination Spheres

The manuscript described the synthesis and characterization of the new [Cd(BDMPT)2](ClO4)2; 1 and [Cd2(MBPT)2(H2O)2Cl](ClO4)3.4H2O ; 2s-triazine pincer-type complexes, where BDMPT and MBPT are 2,4-bis(3,5-dimethyl-1H-pyrazol-1-yl)-6-methoxy-1,3,5-triazine and 2-methoxy-4,6-bis(2-(pyridin-2-ylmsethylene)hydrazinyl)-1,3,5-triazinerespectively.The synthesized complexes were characterized using Fourier-transform infrared spectroscopy (FTIR), 1H and 13C NMR spectroscopy, and the single-crystal X-ray diffraction technique.The homoleptic mononuclear complex (1)contains a hexa-coordinated Cd(II) center with two tridentate N-pincer ligand (BDMPT) with a highly distorted octahedral coordination environment located as an intermediate case between the octahedron and trigonal prism. The heteroleptic dinuclear complex (2) contains two hepta-coordinated Cd(II) coordination spheres where each Cd(II) is coordinated with one pentadentate pincer N-chelate (MBPT), one water, and one bridged chloride ligand connecting the two metal ions. The different intermolecular interactions in the studied complexes were quantified using Hirshfeld analysis. Their thermal stabilities and FTIR spectra were compared with the corresponding free ligands. The strength and nature of Cd–N, Cd–O, and Cd–Cl coordination interactions were discussed in light of atoms in molecules calculations (AIM). The M(II)–BDMPT and M(II)–MBPT interaction energies revealed that such sterically hindered ligands have higher affinity toward large-size metal ions (M =Cd) compared to smaller ones (M= Ni or Mn).

Synthesis and Characterization of the Manganese Pyroarsenate Mn2As2O7 · 2H2O

2001 ◽  
Vol 56 (4-5) ◽  
pp. 359-363 ◽  
Author(s):  
N. Stock ◽  
G. D. Stucky ◽  
A. K. Cheetham
Keyword(s):  
Three Dimensional ◽  
Spectroscopic Studies ◽  
Mean Value ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Raman Spectroscopic ◽  
Distorted Octahedral ◽  
Ir And Raman ◽  
Hydrothermal Methods

Abstract The manganese pyroarsenate hydrate, Mn2As2O7 · 2 H2O, has been obtained as a single phase product using hydrothermal methods and the structure has been determined by single crystal X-ray diffraction. The title compound crystallizes in the monoclinic space group P21/n with a = 6.6576(4), b = 14.555(1), c = 7.8147(5) Å, β = 94.935(1)°, V = 754.46(8) Å3 and Z = 4. The manganese ions are each coordinated to five oxygen atoms and a water molecule in a distorted octahedral arrangement. Edge-sharing MnO6 octahedra form chains which are connected to a three-dimensional framework by As2O74- ions. The pyroarsenate anion, which attains a nearly eclipsed conformation, has a mean As-O distance for the terminal As-O bonds of 1.669(2) Å, while for the bridging oxygen atom a mean value of 1.757(2) Å is observed. Magnetic susceptibility measurements indicate the presence of high-spin Mn2+ ions. Thermogravimetric as well as IR and Raman spectroscopic studies of Mn2As2O7 · 2 H2O are presented.

Preparation of Magnetically Modified Zeolites and the Application of Metal Ions Adsorption

2011 ◽  
Vol 299-300 ◽  
pp. 764-769
Author(s):  
Ming Liang Yuan ◽  
Liang Yu ◽  
Jia Hua Tao ◽  
Cong Song
Keyword(s):  
Metal Ions ◽  
Industrial Effluents ◽  
Nitrogen Adsorption ◽  
Vibrating Sample Magnetometer ◽  
X Ray Diffraction ◽  
Detailed Characterization ◽  
X Ray ◽  
Magnetic Process ◽  
Coprecipitation Process

Natural zeolites combined with the magnetic iron oxides are prepared by a chemical coprecipitation process. A detailed characterization of our magnetically modified zeolite (MMZ) is given, including powder X-ray diffraction (XRD), nitrogen adsorption and vibrating sample magnetometer (VSM). The results reveal that in comparison with Na-zeolite, the structure of MMZ has no obvious change but its surface area increases from 25.13 m2g-1to 100.90 m2g-1. The adsorption properties of MMZ to Pb2+and Cu2+were studied. The results show that the maximum loading capacities for Pb2+and Cu2+in the initial concentration range are 123.74 and 14.633 mg g-1, respectively. The MMZ can be used as an adsorbent for removal of heavy metal ions from industrial effluents or municipal waters, and the saturated adsorbent is separated from the medium by a simple magnetic process.

Supported optically active poly(amide-imide) on magnetic graphene oxide/Fe3O4 for Hg2+ adsorption from aqueous solution

2019 ◽  
pp. 089270571988909
Author(s):  
Sedigheh Khalili ◽  
Zahra Rafiee
Keyword(s):  
Graphene Oxide ◽  
Sem Analysis ◽  
Optically Active ◽  
X Ray Diffraction ◽  
One Pot ◽  
Thermal Stabilities ◽  
Magnetic Graphene Oxide ◽  
Methyl Phenyl

The ternary superparamagnetic nanocomposites consisting of graphene oxide (GO), Fe3O4 nanoparticles, and optically active poly(amide-imide) (PAI) were fabricated in three steps consisting of a facile one-pot in situ growth of Fe3O4 on GO, resulted in the preparation of the magnetic Fe3O4@GO, modification of Fe3O4@GO by 3-aminopropyltriethoxy silane to introduce amino groups on its surface, and subsequently its compositing by various levels of 5, 10, and 15 wt% with chiral PAI derived from 3,5-diamino- N-(4-(di(1H-indol-3-yl)methyl)phenyl)benzamide and N, N′-(4,4′-carbonyldiphthaloyl)-bis-l-phenylalanine diacid through ultrasonic irradiation. Characterization of the resulting nanocomposites was performed by Fourier transform infrared spectroscopy, X-ray diffraction, vibrating sample magnetometer, scanning electron microscope (SEM), and thermogravimetric analysis (TGA). The SEM analysis showed Fe3O4 nanoparticles with 30 nm size successfully decorated the GO nanosheets. The TGA analysis established the expected thermal stabilities for PAI/Fe3O4@GO nanocomposites. Furthermore, incorporation of Fe3O4@GO in polymer matrix improved the mechanical properties substantially. PAI/Fe3O4@GO 10 wt% was used to evaluate the sorption properties of Hg2+ at pH 7.

scholarly journals Selective Hydration of Nitriles to Corresponding Amides in Air with Rh(I)-N-Heterocyclic Complex Catalysts

Catalysts ◽  
2020 ◽  
Vol 10 (1) ◽  
pp. 125 ◽  
Author(s):  
Csilla Enikő Czégéni ◽  
Sourav De ◽  
Antal Udvardy ◽  
Nóra Judit Derzsi ◽  
Gergely Papp ◽  
...  
Keyword(s):  
Catalytic Activity ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
Catalytic Properties ◽  
13C Nmr Spectroscopy ◽  
Synthetic Method ◽  
X Ray Diffraction ◽  
Nitrile Hydration ◽  
X Ray

A new synthetic method for obtaining [RhCl(cod)(NHC)] complexes (1–4) (cod = η4-1,5-cyclooctadiene, NHC = N-heterocyclic carbene: IMes, SIMes, IPr, and SIPr, respectively) is reported together with the catalytic properties of 1–4 in nitrile hydration. In addition to the characterization of 1–4 in solution by 13C NMR spectroscopy, the structures of complexes 3, and 4 have been established also in the solid state with single-crystal X-ray diffraction analysis. The Rh(I)-NHC complexes displayed excellent catalytic activity in hydration of aromatic nitriles (up to TOF = 276 h−1) in water/2-propanol (1/1 v/v) mixtures in air.

Synthesis and structural characterization of two copper(II) complexes with 3-(4-(1H-benzo[d]imidazol-1-yl)-4-methoxyphenyl)-1-phenylprop- 2-en-1-one ligands

2015 ◽  
Vol 70 (3) ◽  
pp. 165-169 ◽  
Author(s):  
Gao-Feng Wang
Keyword(s):  
Infrared Spectroscopy ◽  
Single Crystal ◽  
Structural Characterization ◽  
X Ray Diffraction ◽  
Distorted Octahedral Environment ◽  
X Ray ◽  
Octahedral Environment ◽  
Distorted Octahedral ◽  
Elemental Analyses

AbstractThe synthesis of two new copper(II) complexes with benzimidazole type ligands, Cu(tta)2(L1)2 (1) and Cu(tta)2(L1) (2) (where L1 is 3-(4-(1H-benzo[d]imidazol-1-yl)-4-methoxy phenyl)-1-phenylprop-2-en-1-one; tta is 2-thenoyltrifluoroacetonate), are reported. Their structures have been characterized by infrared spectroscopy, elemental analyses and single-crystal X-ray diffraction. The copper(II) ion of 1 is in a distorted octahedral environment, while that of 2 is in a distorted square-pyramidal environment. In both cases, the donor atoms are provided by oxygen atoms of the tta ligands and nitrogen atoms of the L1 ligands.

scholarly journals Synthesis and Characterization of Magnetite-Alginate Nanoparticles for Enhancement of Nickel and Cobalt Ion Adsorption from Wastewater

2019 ◽  
Vol 2019 ◽  
pp. 1-8 ◽  
Author(s):  
Omnia A. A. El-Shamy ◽  
Ragaa E. El-Azabawy ◽  
Olfat. E. El-Azabawy
Keyword(s):  
Metal Ions ◽  
Adsorption Process ◽  
Ion Adsorption ◽  
X Ray Diffraction ◽  
Adsorption Method ◽  
Freundlich Model ◽  
X Ray ◽  
Transmission Electron ◽  
Absorption Measurements

Superparamagnetic magnetite-alginate nanoparticles (M-AlgNPs) were synthesized utilizing a coprecipitation method. Then, the prepared M-AlgNPs were characterized via Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction spectroscopy (XRD) to affirm the formation and the crystallinity of this composite. In addition, the surface morphology of the prepared nanoparticles was inspected by transmission electron microscopy (TEM) which revealed well-dispersed nanoparticles of Fe3O4 into alginate. The adsorption characteristics of the synthesized nanoparticles for removing Ni+2 and Co+2 from wastewater were evaluated via atomic absorption measurements (AAS). The elimination efficiency of the M-AlgNPs was detected at pH=7 in 100 ppm (initial concentration) of Ni+2 and Co+2, separately. The M-AlgNPs provided the maximum equilibrium uptake percentage for Ni+2 and Co+2 of 97.88 and 95.01%, respectively. The adsorption of Ni+2 and Co+2 onto the M-AlgNP surface was found to fit the Langmuir model with R2 values higher than that obtained from the Freundlich model for both metal ions. Moreover, RL “separating factor” for the adsorption process was assessed and found to be less than unity; this expresses the higher ability of the investigated metal ions to be adsorbed onto the M-AlgNP surface. The adsorption method was discovered to be pH-dependent and well-suited to the isothermal equations of Langmuir and Freundlich. For regeneration studies, M-AlgNPs have been investigated and results confirmed that it could be reused with effective sorption capacity over three cycles.

scholarly journals Synthesis and Characterization of Ammonium Acesulfamate

2014 ◽  
Vol 69 (6) ◽  
pp. 737-741 ◽  
Author(s):  
Gustavo A. Echeverría ◽  
Oscar E. Piro ◽  
Beatriz S. Parajón-Costa ◽  
Enrique J. Baran
Keyword(s):  
Molecular Structure ◽  
Ammonium Carbonate ◽  
Crystal And Molecular Structure ◽  
13C Nmr Spectroscopy ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
1H And 13C Nmr ◽  
X Ray

Ammonium acesulfamate, (NH4)C4H4NO4S, was prepared by the reaction of acesulfamic acid and ammonium carbonate in aqueous solution, and characterized by elemental analysis and 1H and 13C NMR spectroscopy. Its crystal and molecular structure was determined by single-crystal X-ray diffraction methods. The substance crystallizes in the orthorhombic space group Pnma with Z = 4 molecules per unit cell. The NH4+ ion generates medium to strong hydrogen bonds with the carbonylic oxygen, the iminic nitrogen and the sulfonyl oxygen atoms of the acesulfamate anion. The FTIR spectrum of the compound was also recorded and is briefly discussed.

Synthesis and Characterization of a Three-dimensional Coordination Polymer Based on Copper(II) Nitrate and a Tridentate Tetrazole Ligand

2009 ◽  
Vol 64 (11-12) ◽  
pp. 1535-1541 ◽  
Author(s):  
Vera Hartdegen ◽  
Thomas M. Klapötke ◽  
Stefan M. Sproll
Keyword(s):  
Thermal Stability ◽  
Coordination Polymer ◽  
Physical Stability ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Thermal Stabilities ◽  
Dsc Measurements ◽  
Ethyl Amine ◽  
Thermal Stability Of

Tris(2-(1H-tetrazol-1-yl)ethyl)amine (1) was synthesized as gas-generating agent and characterized by vibrational (IR) and NMR spectroscopy. The energetic properties were determined by bomb calorimetric measurements along with calculations using the EXPLO5 software. Tris(2-(1H-tetrazol- 1-yl)ethyl)amine (1) was used for further reactions with copper(II) nitrate to form a three-dimensional coordination polymer 3. Both compounds were characterized by single crystal X-ray diffraction. The thermal stability was determined by DSC measurements and the physical stability by BAMstandards. Tris(2-(1H-tetrazol-1-yl)ethyl)amine (1) proved to be suitable as gas-generating agent with sufficient physical and thermal stabilities. The low thermal stability of the copper complex 3 disqualifies it as potential colorant agent for pyrotechnical applications

scholarly journals Synthesis, Structural Characterization of 4’,4’’-Dibenzoylcurcumin and Assessment of its Complexation with Fe3+ and Cu2+

2019 ◽  
Vol 35 (4) ◽  
Author(s):  
Pham Thu Thuy ◽  
Pham Chien Thang ◽  
Nguyen Viet Ha ◽  
Trieu Thi Nguyet
Keyword(s):  
Metal Ions ◽  
Structural Characterization ◽  
Solution Structure ◽  
13C Nmr Spectroscopy ◽  
Transition Metal Ions ◽  
Structural Features ◽  
Nmr Study ◽  
Supporting Base

The curcumin derivative 4’,4’’-dibenzoylcurcumin (HL) was synthesized by the reaction between curcumin and benzoyl chloride in the presence of pyridine as a supporting base. The composition and structure of HL were characterized by spectroscopic methods such as IR, 1H and 13C NMR spectroscopy. Reactions of HL and transition metal ions, such as Fe3+ and Cu2+, in mixtures of CH3OH and CH2Cl2 gave rise to the corresponding complexes, compositions and structural features of which were studied by thermal analysis and IR spectroscopy. The results strongly suggested the obtained complexes with the compositions of [FeL3] and [CuL2]. In such compounds, metal ions coordinates with the deprotonated ligands L– through the donor sets (O,O) of the keto-enol moieties. Keywords: Curcumin, 4’,4’’-dibenzoylcurcumin, β-diketone, Fe(III) complexes, Cu(II) complexes. References [1] A. Goel, A.B. Kannumakkara, B.B. Aggarwal, Curcumin as “Curecumin”: From Kitchen to Clinic, Biochem. Pharmacol. 75 (2008) 787-809. https://doi.org/10.1016/j.bcp.2007.08.016.[2] T. Esatbeyoglu, P. Huebbe, I.M.A. Ernst, D. Chin, A.E. Wagner, G. Rimbach, Curcumin - From Molecule to Biological Function, Angew. Chem. Int. Ed. 51 (2012) 5308-5332. https://doi.org/ 10.1002/anie.201107724.[3] K. Priyadarsini, The Chemistry of Curcumin: From Extraction to Therapeutic Agent, Molecules 19 (2014) 20091-20112. https://doi.org/10.3390/ molecules191220091.[4] S. Wanninger, V. Lorenz, A. Subhan, F.T. Edelmann, Metal complexes of curcumin – synthetic strategies, structures and medicinal applications, Chem. Soc. Rev. 44 (2015) 4986-5002. https://doi.org/10.1039/C5CS00088B.[5] J. Wang, D. Wei, B. Jiang, T. Liu, J. Ni, S. Zhou, Two copper(II) complexes of curcumin derivatives: synthesis, crystal structure and in vitro antitumor activity, Transition Met. Chem. 39 (2014) 553-558. https://doi.org/10.1007/s11243-014-9831-z.[6] R. Pettinari, F. Marchetti, C. Pettinari, F. Condello, A. Petrini, R. Scopelliti, T. Riedel, P.J. Dyson, Organometallic rhodium(III) and iridium(III) cyclopentadienyl complexes with curcumin and bisdemethoxycurcumin co-ligands, Dalton Transactions 44 (2015) 20523-20531. https://doi.org/10.1039/C5DT03037D.[7] P.T. Thùy, P.C. Thắng, N.H. Huy, N.V. Hà, T.T. Nguyệt, Synthesis, structural characterization of 4,4’-diacetylcurcumin and its complexes with Fe(III), Co(II) (in Vietnamese), Vietnam Journal of Chemistry 55 (2017) 33-37. [8] P.C. Thắng, P.T. Thùy, T.T.K. Ngân, L.C. Định, Đ.T. Đạt, T.T. Nguyệt, Synthesis, structural characterization of 4’,4’’-dimethoxy-4-methylcurcumin and evaluation of its complexation with Co2+ and Cu2+ (in Vietnamese), Vietnam Journal of Chemistry 56 (2018) 113-117. [9] P.T. Thùy, P.C. Thắng, V.T.B. Ngoc, T.T. Nguyệt, Synthesis and structural characterization of a heteroleptic Pd(II) complex with 4,4’-diacetylcurcumin (in Vietnamese), Vietnam Journal of Chemistry 56 (2018) 119-123. [10] K. Singletary, C. MacDonald, M. Iovinelli, C. Fisher, M. Wallig, Effect of the beta-diketones diferuloylmethane (curcumin) and dibenzoylmethane on rat mammary DNA adducts and tumors induced by 7,12-dimethylbenz[a] anthracene, Carcinogenesis 19 (1998) 1039-1043. https://doi.org/10.1093/carcin/ 19.6.1039.[11] F. Payton, P. Sandusky, W.L. Alworth, NMR Study of the Solution Structure of Curcumin, J. Nat. Prod. 70 (2007) 143-146. https://doi.org/10. 1021/np060263s.  

scholarly journals Spectral, thermal and magnetic characterization of 2, 3-dimethoxybenzoates of Co(II), Ni(II) and Cu(II)

2005 ◽  
Vol 70 (6) ◽  
pp. 833-842 ◽  
Author(s):  
Wieslawa Ferenc ◽  
Agnieszka Walkow-Dziewulska ◽  
Pawel Sadowsk ◽  
Janusz Chrusciel
Keyword(s):  
Magnetic Moments ◽  
Electronic Spectroscopy ◽  
X Ray Diffraction ◽  
Magnetic Studies ◽  
Thermal Stabilities ◽  
Bridging Ligands ◽  
X Ray ◽  
Carboxylate Groups ◽  
Polycrystalline Solids

Complexes of 2,3-dimethoxybenzoates of Co(II), Ni(II) and Cu(II) have been synthesized as hydrated or anhydrous polycrystalline solids and characterized by elemental analysis, IR, FIR and electronic spectroscopy, magnetic studies and X-ray diffraction measurements. The carboxylate groups bind as monodentate or symmetrical, bidentate chelating and bridging ligands. The thermal stabilities were determined in air. When heated they dehydrate to form anhydrous salts which are decomposed to the oxides of the respective metals. The magnetic susceptibilities of the complexes were measured over the range 77?300 K and the magnetic moments were calculated. The results show that the complexes of Ni(II) and Co(II) are high-spin complexes and that of Cu(II) forms a dimer.

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