A Versatile Approach to Access Trimetallic Complexes Based on Trisphosphinite Ligands

A straightforward method for the preparation of trisphosphinite ligands in one step, using only commercially available reagents (1,1,1-tris(4-hydroxyphenyl)ethane and chlorophosphines) is described. We have made use of this approach to prepare a small family of four trisphosphinite ligands of formula [CH3C{(C6H4OR2)3], where R stands for Ph (1a), Xyl (1b, Xyl = 2,6-Me2-C6H3), iPr (1c), and Cy (1d). These polyfunctional phosphinites allowed us to investigate their coordination chemistry towards a range of late transition metal precursors. As such, we report here the isolation and full characterization of a number of Au(I), Ag(I), Cu(I), Ir(III), Rh(III) and Ru(II) homotrimetallic complexes, including the structural characterization by X-ray diffraction studies of six of these compounds. We have observed that the flexibility of these trisphosphinites enables a variety of conformations for the different trimetallic species.

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One Step Synthesis and Characterization of Zirconia-Graphene Composites

Advanced Materials Research ◽

10.4028/www.scientific.net/amr.600.174 ◽

2012 ◽

Vol 600 ◽

pp. 174-177 ◽

Cited By ~ 1

Author(s):

Jian Fei Xia ◽

Zong Hua Wang ◽

Yan Zhi Xia ◽

Fei Fei Zhang ◽

Fu Qiang Zhu ◽

...

Keyword(s):

Synthesis And Characterization ◽

Two Dimensional ◽

X Ray Diffraction ◽

X Ray ◽

Graphene Composite ◽

Transmission Electron ◽

One Step ◽

Ft Ir ◽

Xrd Techniques

Zirconia-graphene composite (ZrO2-G) has been successfully synthesized via decomposition of ZrOCl2•6H2O in a water-isopropanol system with dispersed graphene oxide (GO) utilizing Na2S as a precursor could enable the occurrence of the deposition of Zr4+ and the deoxygenation of GO at the same time. Transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD) techniques were used to characterize the samples. It was found that graphene were fully coated with ZrO2, and the ZrO2 existing in tetragonal phase, which resulted in the formation of two-dimensional composite.

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Preparation, Characterization of Nonmetal Doped TiO2 Nanoparticles with their Excellent Photocatalystic Properties

Advanced Materials Research ◽

10.4028/www.scientific.net/amr.183-185.2254 ◽

2011 ◽

Vol 183-185 ◽

pp. 2254-2257

Author(s):

Ying Wei Wang ◽

Yu Fei Li ◽

Pei Han Yang

Keyword(s):

Photoelectron Spectroscopy ◽

Photocatalytic Performance ◽

Anatase Phase ◽

Titania Nanoparticles ◽

X Ray Diffraction ◽

X Ray ◽

One Step ◽

Doped Titania ◽

Nonmetal Doping

Nonmetal (S, P) doped titania nanoparticles were synthesized by a one step hydrothermal method. These samples were calcined with different temperature, the sample exist in anatase phase has much higher photocatalytic activity for methylene blue (MB) degradation. The visible response and the higher UV activity of the different nonmetal doped TiO2make it possible to utilize solar energy efﬁciently to execute photocatalysis processes. The resulting materials were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), etc. It can conclude the nonmetal doping TiO2proves to be more suitable to improve the photocatalytic performance.

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Preparation and Characterization of Vanadium Pentoxide Hollow Microspheres with Tunable Sizes

Key Engineering Materials ◽

10.4028/www.scientific.net/kem.697.706 ◽

2016 ◽

Vol 697 ◽

pp. 706-709

Author(s):

Ming Gong ◽

Chang An Wang

Keyword(s):

Electron Microscopy ◽

Solvothermal Method ◽

Hollow Microspheres ◽

Soft Template ◽

X Ray Diffraction ◽

X Ray ◽

Molecular Weights ◽

Transmission Electron ◽

One Step

V2O5 hollow microspheres were synthesized by a one-step solvothermal method, with the assistance of PVP as the soft template, ethylene glycol (EG) as the solvent, and vanadium (iii) acetylacetonate (acac) as the metal-ions source. The samples were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM). The size of V2O5 hollow microspheres, which can be easily tuned by using PVP of different molecular weights, was about 2.5μm, 4.5μm and 6μm when using PVP-K17, PVP-K30 and PVP-K60 as the template, respectively.

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Characterization of Donut-Like SrMoO4Produced by Microwave-Hydrothermal Process

Journal of Nanomaterials ◽

10.1155/2013/474576 ◽

2013 ◽

Vol 2013 ◽

pp. 1-6 ◽

Cited By ~ 2

Author(s):

Surangkana Wannapop ◽

Titipun Thongtem ◽

Somchai Thongtem

Keyword(s):

Vibration Mode ◽

Energy Gap ◽

Hydrothermal Process ◽

X Ray Diffraction ◽

Hierarchical Nanostructures ◽

X Ray ◽

Microwave Hydrothermal ◽

Stretching Vibration ◽

One Step

SrMoO4hierarchical nanostructures were successfully produced by a one step of 270 W microwave-hydrothermal process of one of the solutions containing three strontium salts [Sr(NO3)2, Sr(CH3CO2)2, and SrCl2·6H2O] and (NH4)6Mo7O24·4H2O for different lengths of time. The as-produced products were characterized by X-ray diffraction, electron microscopy, and spectroscopy. In this research, they were primitive tetragonal structured donut-like SrMoO4, with the main 881cm−1 ν1(Ag)symmetric stretching vibration mode of[MoO4]2−units and 3.92 eV energy gap.

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An Improved Synthesis of 3,6-Dihydro-as-indacene

Synthesis ◽

10.1055/s-0040-1707372 ◽

2020 ◽

Author(s):

Marcelo Preite ◽

Elies Molins ◽

Ivonne Chávez ◽

Mungalimane K. Amshumali ◽

Cesar Morales-Verdejo ◽

...

Keyword(s):

Ammonium Hydroxide ◽

13C Nmr Spectroscopy ◽

X Ray Diffraction ◽

1H And 13C Nmr ◽

Intramolecular Cycloaddition ◽

X Ray ◽

Full Characterization ◽

Mannich Condensation ◽

Acidic Conditions

AbstractThis contribution describes an updated synthetic route to 3,6-dihydro-as-indacene along with full characterization of all intermediates. The title compound is prepared by Mannich condensation of 2-methylfuran with formaldehyde and dimethylamine hydrochloride, quaternization of the resulting amine with methyl iodide, and conversion into the ammonium hydroxide salt by treatment with silver oxide in water. Subsequent Hoffmann elimination and [6,6]-cycloaddition through pyrolysis produces a furanocyclophane, which after photooxidation, intramolecular cycloaddition, and dehydration with sodium carbonate affords 2,3,6,7-tetrahydro-1,8-dione-as-indacene. Reduction of this diketone gives a mixture of alcohols, which after dehydration under slightly basic or acidic conditions produces 3,6-dihydro-as-indacene. The structure is confirmed by X-ray diffraction, and all intermediates are characterized by means of 1H and 13C NMR spectroscopy.

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Polymers of ε-Caprolactone Using New Copper(II) and Zinc(II) Complexes as Initiators: Synthesis, Characterization and X-Ray Crystal Structures

Polymers ◽

10.3390/polym10111239 ◽

2018 ◽

Vol 10 (11) ◽

pp. 1239 ◽

Cited By ~ 5

Author(s):

Andrés Posada ◽

Mario Macías ◽

Santiago Movilla ◽

Gian Miscione ◽

León Pérez ◽

...

Keyword(s):

Single Crystal ◽

Ring Opening ◽

Ring Opening Polymerization ◽

Nmr Analysis ◽

X Ray Diffraction ◽

X Ray ◽

Molecular Weights ◽

Full Characterization ◽

Solvent Free Conditions

Five of six new Zn(II) and Cu(II) complexes were active in the ring-opening polymerization (ROP) of ε-caprolactone (CL) under solvent-free conditions, producing polycaprolactones (PCLs) of high crystallinity with molecular weights between 22,900 and 38,700 g mol−1 and decomposition temperatures above 260 °C. 1H NMR analysis demonstrated that the PCLs obtained were mainly linear, having hydroxymethylene groups at the chain ends. The results obtained indicated a significant improvement in terms of the ratio of monomer:initiator compared to related Cu(II) and Zn(II) complexes. In addition, the structures of the complexes 1 and 4 were determined by single-crystal X-ray diffraction. The synthesis and full characterization of all complexes are described in this paper.

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m-Carborane as a Novel Core for Periphery-Decorated Macromolecules

Molecules ◽

10.3390/molecules25122814 ◽

2020 ◽

Vol 25 (12) ◽

pp. 2814 ◽

Cited By ~ 1

Author(s):

Ines Bennour ◽

Francesc Teixidor ◽

Zsolt Kelemen ◽

Clara Viñas

Keyword(s):

Surface Analysis ◽

Hirshfeld Surface ◽

X Ray Diffraction ◽

Electrophilic Reaction ◽

X Ray ◽

Full Characterization ◽

New Class ◽

Synthetic Procedure ◽

Judicious Choice

Closo m-C2B10H12 can perform as a novel core of globular periphery-decorated macromolecules. To do this, a new class of di and tetrabranched m-carborane derivatives has been synthesized by a judicious choice of the synthetic procedure, starting with 9,10-I2-1,7-closo-C2B10H10. The 2a-NPA (sum of the natural charges of the two bonded atoms) value for a bond, which is defined as the sum of the NPA charges of the two bonded atoms, matches the order of electrophilic reaction at the different cluster bonds of the icosahedral o-and m- carboranes that lead to the formation of B-I bonds. As for m-carborane, most of the 2a-NPA values of B-H vertexes are positive, and their functionalization is more challenging. The synthesis and full characterization of dibranched 9,10-R2-1,7-closo-carborane (R = CH2CHCH2, HO(CH2)3, Cl(CH2)3, TsO(CH2)3, C6H5COO(CH2)3, C6H5COO(CH2)3, N3(CH2)3, CH3CHCH, and C6H5C2N3(CH2)3) compounds as well as the tetrabranched 9,10-R2-1,7-R2-closo-C2B10H8 (R = CH2CHCH2, HO(CH2)3) are presented. The X-ray diffraction of 9,10-(HO(CH2)3)2-1,7-closo-C2B10H10 and 9,10-(CH3CHCH)2-1,7-closo-C2B10H10, as well as their Hirshfeld surface analysis and decomposed fingerprint plots, are described. These new reported tetrabranched m-carborane derivatives provide a sort of novel core for the synthesis of 3D radially grown periphery-decorated macromolecules that are different to the 2D radially grown core of the tetrabranched o-carborane framework.

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Late transition metal complexes of oxypyriporphyrin and the platinum(II) complex of oxybenziporphyrin

Journal of Porphyrins and Phthalocyanines ◽

10.1142/s1088424617500535 ◽

2017 ◽

Vol 21 (07n08) ◽

pp. 493-501 ◽

Cited By ~ 1

Author(s):

Komal Pokharel ◽

Gregory M. Ferrence ◽

Timothy D. Lash

Keyword(s):

Acetic Acid ◽

Coordination Chemistry ◽

Transition Metal Complexes ◽

Potassium Acetate ◽

Late Transition Metal ◽

Coordination Core ◽

X Ray ◽

X Ray Crystallography ◽

Anionic Species ◽

Late Transition

Even though oxypyriporphyrin, a pyridone-containing porphyrinoid system, has the equivalent coordination core to true porphyrins, its coordination chemistry has been little explored. In this study, the first examples of palladium(II), platinum(II) and silver(II) oxypyriporphyrins have been synthesized. Conventional conditions failed to result in the formation of a platinum(II) complex, but moderate yields were obtained when oxypyriporphyrin was reacted with platinum(II) chloride in refluxing mixtures of DMF and acetic acid containing potassium acetate. The palladium(II) and platinum(II) derivatives were characterized by X-ray crystallography. The structurally analogous carbaporphyrinoid system oxybenziporphyrin was also shown to react with platinum(II) chloride under the same conditions to give a platinum(II) hydroxybenziporphyrin complex. Unlike oxybenziporphyrin, this complex is only weakly diatropic. In the presence of base, the diatropic character was reasserted to afford an aromatic anionic species.

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Synthesis and characterization of crystalline poly(N-(2-hydroxyethyl)aniline) microspheres

High Performance Polymers ◽

10.1177/0954008316638135 ◽

2016 ◽

Vol 29 (2) ◽

pp. 227-236 ◽

Cited By ~ 7

Author(s):

HM Abd El-Salam ◽

HG Askalany

Keyword(s):

Initial Rate ◽

Polymerization Rate ◽

Proton Nuclear Magnetic Resonance ◽

Polymerization Reaction ◽

Synthesis And Characterization ◽

X Ray Diffraction ◽

Ammonium Persulphate ◽

X Ray ◽

One Step

Poly( N-(2-hydroxyethyl)aniline) microsphere was prepared in aqueous hydrochloric acid (HCl) in one step, using ammonium persulphate as an oxidant. The effect of monomer, oxidant, HCl concentrations and temperature on polymerization rates was investigated. The data show that polymerization rate increases with increasing reactant concentrations. In addition, the initial rate increases with raising the temperature. The apparent activation energy found was 57.4319 kJ/mole. Also, Δ H* and Δ S* found were 55.0691 kJ/mole and 78.3662 J/mole K respectively. Infrared and proton nuclear magnetic resonance spectroscopies, thermogravimetric analysis, X-ray diffraction, scanning electron microscopy and elemental analysis characterize the obtained polymer sample to confirm the suggested structure. The mechanism of the polymerization reaction are discussed.

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Synthesis and characterization of Cu3SbS4 thin films grown by co-sputtering metal precursors and subsequent sulfurization

Materials Advances ◽

10.1039/d0ma00574f ◽

2020 ◽

Vol 1 (9) ◽

pp. 3333-3338

Author(s):

A Azizur Rahman ◽

Emroj Hossian ◽

Hetal Vaishnav ◽

Jayesh B. Parmar ◽

Arnab Bhattacharya ◽

...

Keyword(s):

Thin Films ◽

Synthesis And Characterization ◽

Optical Absorption Spectra ◽

X Ray Diffraction ◽

Diffraction Profile ◽

X Ray ◽

Metal Precursors ◽

Phase Pure ◽

Pure Cu

X-ray diffraction profile, Raman and optical absorption spectra, and surface morphology of phase-pure Cu3SbS4 films grown at 425 °C by co-sputtering metal precursors and subsequent sulfurization.

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