Synthesis of ReItricarbonyl complexes with various sulfur- and oxygen-donating ligands: crystal structures of two ReIdinuclear structures bridged by S atoms

2018 ◽  
Vol 74 (10) ◽  
pp. 1116-1122
Author(s):  
Pheello I. Nkoe ◽  
Hendrik G. Visser ◽  
Chantel Swart ◽  
Alice Brink ◽  
Marietjie Schutte-Smith
Keyword(s):  
Hydrogen Bond ◽  
Intermolecular Hydrogen Bond ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Metal Centre ◽  
Pyridine Ligand ◽  
X Ray ◽  
Hydrogen Bond Interactions ◽  
Mononuclear Complexes

The synthesis and characterization of two dinuclear complexes, namelyfac-hexacarbonyl-1κ3C,2κ3C-(pyridine-1κN)[μ-2,2′-sulfanediyldi(ethanethiolato)-1κ2S1,S3:2κ3S1,S2,S3]dirhenium(I), [Re2(C4H8S3)(C5H5N)(CO)6], (1), and tetraethylammoniumfac-tris(μ-2-methoxybenzenethiolato-κ2S:S)bis[tricarbonylrhenium(I)], (C8H20N)[Re2(C7H7OS)3(CO)6], (2), together with two mononuclear complexes, namely (2,2′-bithiophene-5-carboxylic acid-κ2S,S′)bromidotricarbonylrhenium(I), (3), and bromidotricarbonyl(methyl benzo[b]thiophene-2-carboxylate-κ2O,S)rhenium(I), (4), are reported. Crystals of (1) and (2) were characterized by X-ray diffraction. The crystal structure of (1) revealed two Re—S—Re bridges. The thioether S atom only bonds to one of the ReImetal centres, while the geometry of the second ReImetal centre is completed by a pyridine ligand. The structure of (2) is characterized by three S-atom bridges and an Re...Re nonbonding distance of 3.4879 (5) Å, which is shorter than the distance found for (1) [3.7996 (6)/3.7963 (6) Å], but still clearly a nonbonding distance. Complex (1) is stabilized by six intermolecular hydrogen-bond interactions and an O...O interaction, while (2) is stabilized by two intermolecular hydrogen-bond interactions and two O...π interactions.

Oxazoline chemistry — Part IV: Synthesis and characterization of oxazoline complexes of the zinc halides

2003 ◽  
Vol 81 (12) ◽  
pp. 1482-1491 ◽  
Author(s):  
Tosha M Barclay ◽  
Ignacio del Río ◽  
Robert A Gossage ◽  
Sarah M Jackson
Keyword(s):  
Crystal Structure ◽  
Structural Diversity ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Metal Centre ◽  
Zinc Compounds ◽  
X Ray ◽  
H Nmr ◽  
Oxazoline Ligands

The synthesis and characterization of 11 zinc halide derivatives that contain monodentate oxazoline ligands is described. The treatment of ether solutions of [ZnX2] (X = Cl, Br, I) with 2-aryl- or 2-methyl-2-oxazolines results in the formation of mildly hygroscopic complexes of the general formulae [ZnX2(ox)2] (ox = 2-methyl-2-oxazoline (1), 2,4,4-trimethyl-2-oxazoline (2), 2-phenyl-2-oxazoline (3), or 4,4-dimethyl-2-phenyl-2-oxazoline (4)), except in the case of ZnI2, which does not form an isolable complex — likely for steric reasons — with oxazoline 4. Treatment of [ZnBr2(4)2] with 1 reveals (1H NMR) that 1 only sluggishly displaces coordinated 4 at temperatures below 50 °C. The structural characterization, via single crystal X-ray diffraction, of six of the complexes, viz. [ZnI2(1)2], [ZnI2(2)2], [ZnX2(3)2] (X = Cl, Br, or I), and [ZnBr2(4)2], is also reported. All of these structurally characterized complexes are mononuclear zinc compounds with an overall distorted tetrahedral arrangement of the two halide and two oxazoline ligands around the zinc metal centre. The oxazoline series of complexes reported herein show little structural diversity, a facet which is in contrast to their substituted pyridine analogues.Key words: oxazoline, zinc, X-ray crystal structure, coordination complex, NMR spectroscopy, Zn(II).

scholarly journals Preparation and Characterization of a Novel Cocrystal of Atorvastatin Calcium with Succinic Acid Coformer

2019 ◽  
Vol 19 (3) ◽  
pp. 660
Author(s):  
Yudi Wicaksono ◽  
Dwi Setyawan ◽  
Siswandono Siswandono ◽  
Tri Agus Siswoyo
Keyword(s):  
Succinic Acid ◽  
Dissolution Rate ◽  
Intermolecular Hydrogen Bond ◽  
Acid Amide ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Atorvastatin Calcium ◽  
Hydrogen Bond Interactions

Preparation and characterization of a novel cocrystal of atorvastatin calcium with succinic acid coformer were successfully performed. This research aims to modify the crystalline form of atorvastatin calcium through cocrystallization with succinic acid coformer. The cocrystal was prepared by a solvent evaporation method and characterized by Powder X-Ray Diffraction (PXRD), Differential Scanning Calorimetry (DSC), Fourier Transform Infrared Spectroscopy (FTIR) and Scanning Electron Microscopy (SEM). The atorvastatin calcium-succinic acid cocrystal has new crystalline peaks at 2θ of 12.9, 18.2 and 26.7° indicating the formation of a new crystalline phase. The cocrystal showed the melting point at 205.7 °C with an enthalpy of fusion 30.2 J/g which is different from the initial components. The FTIR spectra of cocrystal showed the shifting of absorption peaks of groups of initial components indicating of formation of atorvastatin calcium-succinic acid cocrystal through acid–amide intermolecular hydrogen bond interactions. The solubility and dissolution test showed that the cocrystal has solubility and dissolution rate significantly higher than the solubility and dissolution rate of pure atorvastatin calcium.

Synthesis and characterization of TiN / Ti / AISI 410 coatings

2018 ◽  
Vol 2 (1) ◽  
pp. 7
Author(s):  
S Chirino ◽  
Jaime Diaz ◽  
N Monteblanco ◽  
E Valderrama
Keyword(s):  
Synthesis And Characterization ◽  
Photoemission Spectroscopy ◽  
X Ray Diffraction ◽  
X Ray ◽  
Columnar Grains ◽  
Tin Thin Films ◽  
Steel Aisi ◽  
Interacting Surfaces ◽  
Stainless Steel Aisi

The synthesis and characterization of Ti and TiN thin films of different thicknesses was carried out on a martensitic stainless steel AISI 410 substrate used for tool manufacturing. The mechanical parameters between the interacting surfaces such as thickness, adhesion and hardness were measured. By means of the scanning electron microscope (SEM) the superficial morphology of the Ti/TiN interface was observed, finding that the growth was of columnar grains and by means of EDAX the existence of titanium was verified.  Using X-ray diffraction (XRD) it was possible to observe the presence of residual stresses (~ -3.1 GPa) due to the different crystalline phases in the coating. Under X-ray photoemission spectroscopy (XPS) it was possible to observe the molecular chemical composition of the coating surface, being Ti-N, Ti-N-O and Ti-O the predominant ones.

Synthesis and characterization of photothermal antibacterial hydrogel with enhanced mechanical properties

2021 ◽  
Author(s):  
Shu bin Li ◽  
Xiao Wang ◽  
Jiang Zhu ◽  
Zhenyu Wang ◽  
Lu Wang
Keyword(s):  
Mechanical Properties ◽  
Hydrogen Bond ◽  
Fe3o4 Nanoparticles ◽  
Intermolecular Hydrogen Bond ◽  
Amide Bond ◽  
Synthesis And Characterization

In this work, using carboxyl-modified Fe3O4 nanoparticles as a photothermal agent, combining the chemical amide bond and intermolecular hydrogen bond crosslinking force, a photothermal hydrogel with enhanced mechanical properties was...

scholarly journals Synthesis and Characterization of Clay Polymer Nanocomposites of P(4VP-co-AAm) and Their Application for the Removal of Atrazine

Polymers ◽  
2019 ◽  
Vol 11 (4) ◽  
pp. 721 ◽  
Author(s):  
Jorge A. Ramírez-Gómez ◽  
Javier Illescas ◽  
María del Carmen Díaz-Nava ◽  
Claudia Muro-Urista ◽  
Sonia Martínez-Gallegos ◽  
...  
Keyword(s):  
Polymer Nanocomposites ◽  
Nanocomposite Materials ◽  
Synthesis And Characterization ◽  
Cross Linking ◽  
X Ray Diffraction ◽  
Numerous Species ◽  
X Ray ◽  
Different Types ◽  
Synthesized Materials

Atrazine (ATZ) is an herbicide which is applied to the soil, and its mechanism of action involves the inhibition of photosynthesis. One of its main functions is to control the appearance of weeds in crops, primarily in corn, sorghum, sugar cane, and wheat; however, it is very toxic for numerous species, including humans. Therefore, this work deals with the adsorption of ATZ from aqueous solutions using nanocomposite materials, synthesized with two different types of organo-modified clays. Those were obtained by the free radical polymerization of 4-vinylpyridine (4VP) and acrylamide (AAm) in different stoichiometric ratios, using tetrabutylphosphonium persulfate (TBPPS) as a radical initiator and N,N′-methylenebisacrylamide (BIS) as cross-linking agent. The structural, morphological, and textural characteristics of clays, copolymers, and nanocomposites were determined through different analytical and instrumental techniques, i.e., X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA). Adsorption kinetics experiments of ATZ were determined with the modified and synthesized materials, and the effect of the ratio between 4VP and AAm moieties on the removal capacities of the obtained nanocomposites was evaluated. Finally, from these sets of experiments, it was demonstrated that the synthesized nanocomposites with higher molar fractions of 4VP obtained the highest removal percentages of ATZ.

scholarly journals High-pressure synthesis and characterization of the non-centrosymmetric scandium borate ScB6O9(OH)3

2020 ◽  
Vol 75 (6-7) ◽  
pp. 597-603
Author(s):  
Birgit Fuchs ◽  
Hubert Huppertz
Keyword(s):  
High Pressure ◽  
High Temperature ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
High Pressure High Temperature ◽  
Structure Solution ◽  
Temperature Experiment ◽  
Pressure Synthesis

AbstractThe non-centrosymmetric scandium borate ScB6O9(OH)3 was obtained through a high-pressure/high-temperature experiment at 6 GPa and 1473 K. Single-crystal X-ray diffraction revealed that the structure is isotypic to InB6O9(OH)3 containing borate triple layers separated by scandium layers. The compound crystallizes in the space group Fdd2 with the lattice parameters a = 38.935(4), b = 4.4136(4), and c = 7.6342(6) Å. Powder X-ray diffraction and vibrational spectroscopy were used to further characterize the compound and verify the proposed structure solution.

One Step Synthesis and Characterization of Zirconia-Graphene Composites

2012 ◽  
Vol 600 ◽  
pp. 174-177 ◽  
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.

Synthesis and Characterization of Multiferroic NiFe2O4/BiFeO3 Nanocomposites by Modified Pechini Method

2011 ◽  
Vol 197-198 ◽  
pp. 456-459
Author(s):  
Xian Ming Liu ◽  
Wen Liang Gao
Keyword(s):  
Pechini Method ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Magnetic Bias ◽  
Field Frequency ◽  
Magnetic Field Frequency ◽  
X Ray ◽  
Structure And Morphology ◽  
Modified Pechini Method

Spinel-perovskite multiferroics of NiFe2O4/BiFeO3 nanoparticles were prepared by modified Pechini method. The structure and morphology of the composites were examined by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results showed that the composites consisted of spinel NiFe2O4 and perovskite BiFeO3 after annealed at 700°C for 2h, and the particle size ranges from 40 to 100nm. VSM and ME results indicated that the nanocomposites exhibited both tuning magnetic properties and a ME effect. The ME effect of the nanocomposites strongly depended on the magnetic bias and magnetic field frequency.

Hydrothermal Synthesis and Characterization of BiFeO3 Polyhedral Crystallites

2012 ◽  
Vol 174-177 ◽  
pp. 508-511
Author(s):  
Lin Lin Yang ◽  
Yong Gang Wang ◽  
Yu Jiang Wang ◽  
Xiao Feng Wang
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Xrd Pattern ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Electron

BiFeO3 polyhedrons had been successfully synthesized via a hydrothermal method. The as-prepared products were characterized by power X-ray diffraction (XRD) pattern, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The possible mechanisms for the formation of BiFeO3 polyhedrons were discussed. Though comparison experiments, it was found that the kind of precursor played a key role on the morphology control of BiFeO3 crystals.

Synthesis and Characterization of a Fluorescent Dianthraceno­indacene

Synlett ◽  
2018 ◽  
Vol 29 (19) ◽  
pp. 2562-2566 ◽  
Author(s):  
Michael Haley ◽  
Conerd Frederickson ◽  
Joshua Barker ◽  
Justin Dressler ◽  
Zheng Zhou ◽  
...  
Keyword(s):  
Neutral Molecule ◽  
Conical Intersection ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Irreversible Reduction ◽  
Inside Out

A freely soluble dianthracenoindacene derivative has been synthesized using an ‘inside-out’ Friedel–Crafts alkylation method and is the first fluorescent diacenoindacene reported. Linear fusion of the anthracenes is confirmed by X-ray diffraction studies on the neutral molecule as well as its dianion. Based on predictions from our previous studies, this is also the least antiaromatic diacenoindacene derivative yet to be prepared, which is reflected in its highly negative and irreversible reduction. With its paratropicity essentially eliminated, we posit that the molecule is no longer deactivated by a conical intersection, typical of antiaromatic molecules, and therefore fluorescence is restored. This follows the trend shown in the related dianthracenopentalenes, with the reappearance of fluorescence when the outer acene groups are extended to linearly-fused anthracene moieties.

Sign in / Sign up

Export Citation Format

Share Document