scholarly journals 1,5-Phosphonium betaines from N-triflylpropiolamides, triphenylphosphane, and active methylene compounds

2019 ◽  
Vol 15 ◽  
pp. 2603-2611
Author(s):  
Vito A Fiore ◽  
Chiara Freisler ◽  
Gerhard Maas
Keyword(s):  
Molar Ratio ◽  
Single Bond ◽  
X Ray Diffraction ◽  
Charge Delocalization ◽  
X Ray ◽  
Active Methylene Compounds ◽  
Extended Charge ◽  
Active Methylene ◽  
Crystallization Structure ◽  
Anionic Part

N-Phenyl-N-(trifluoromethylsulfonyl)propiolamides react with triphenylphosphane in the presence of various active methylene compounds CH2XY in a 1:1:1 molar ratio to furnish 1-phosphonium-5-oxabetaines, Ph3P+–C(R)=CH–C(O–)=CXY. These betaines are formed preferentially, but not exclusively, as E-diastereoisomers with respect to the vinylic double bond. In some cases, separation of the two diastereoisomers was achieved by fractionating crystallization. Structure determination by X-ray diffraction analysis revealed marked conformational differences around the CH–C(O–) single bond of E and Z-isomers and extended charge delocalization in the anionic part.

Synthese und Struktur- und Konformationsanalyse von Triphenylphosphonium-bis(diphenylarsino)methylid

1984 ◽  
Vol 39 (11) ◽  
pp. 1456-1462 ◽  
Author(s):  
Hubert Schmidbaur ◽  
Peter Nußstein ◽  
Gerhard Müller
Keyword(s):  
Single Crystal ◽  
Spectroscopic Data ◽  
Heavy Atom ◽  
Lone Pair ◽  
Molar Ratio ◽  
Single Bond ◽  
X Ray Diffraction ◽  
Trans Conformation ◽  
X Ray ◽  
Lone Pairs

Abstract Triphenylphosphonium -diphenylarsinomethylide (1) and -bis-(diphenylarsino)methylide (2) are easily available through transylidation processes using Ph3P = CH2 and Ph2AsCl as the starting materials in the appropriate molar ratio. Analytical and spectroscopic data are presented for both ylides. The structure of 2 was studied in detail by single-crystal X-ray diffraction. The basic PCAs2 skeleton is found to deviate strongly from planarity. The Ph2As-substituents adopt a cis/trans conformation relative to the ylidic P = C bond with the directions of the lone pairs of electrons at the arsenic atoms in the heavy atom plane as expected for a maximum compensation of the electrostatic vectors. For 1, a cis-conformation of the lone pair of electrons and a large PCAs angle are predicted on the basis of NMR analogies with the phosphorus homologues. Single bond rotational barriers appear to be much lower for 1 and 2, however, than for the corresponding phosphino-substituted ylides.

Effect of Hydrated Metal Salts on the Coordination Product of Cobalt(II) halide and PNP Type Ligand, 2,6-bis(di-tertbutylphosphinomethyl) pyridine

2018 ◽  
Author(s):  
Tasneem Siddiquee ◽  
Abdul Goni
Keyword(s):  
Metal Salts ◽  
Molar Ratio ◽  
Pincer Complexes ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
Pincer Ligand ◽  
Tetrahedral Geometry ◽  
X Ray ◽  
Distorted Tetrahedral Geometry ◽  
Cobalt Center

Chemical treatment of CoX<sub>2</sub><b><sup>. </sup></b>6H<sub>2</sub>O (X = Cl, Br, I) with the potentially tridentate PNP pincer ligand 2,6-bis(di-<i>tert</i>-butylphosphinomethyl)pyridine in 1:1 molar ratio results in cobalt(II) halide-PNP pincer complexes. The effect of the hydrated metal source on molecular structure and geometry of the complexes was studied by single crystal X-ray diffraction analysis. The complexes are neutral and the cobalt center adopts a penta-coordinate system with potential atropisomerization. Within the unit cell there are two distinct molecules per asymmetric unit. One of the two phosphorus atoms in the PNP ligand was observed to be partially oxidized to phosphinoxide. Disorder in the structure reflects a mixture of square pyramidal and distorted tetrahedral geometry.

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

Catalysts ◽  
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.

Application of vermiculite and limestone to desulphurization and to the removal of dust during briquette combustion

2003 ◽  
Vol 67 (6) ◽  
pp. 1243-1251 ◽  
Author(s):  
A. Lu ◽  
D. Zhao ◽  
J. Li ◽  
C. Wang ◽  
S. Qin
Keyword(s):  
Electron Microscopy ◽  
Coal Combustion ◽  
Combustion Temperature ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Retention Ratio ◽  
X Ray ◽  
Major Factors ◽  
Chemical Reactant ◽  
Scanning Electron

AbstractSmall domestic cooking furnaces are widely used in China. These cooking furnaces release SO2 gas and dust into the atmosphere and cause serious air pollution. Experiments were conducted to investigate the effects of vermiculite, limestone or CaCO3, and combustion temperature and time on desulphurization and dust removal during briquette combustion in small domestic cooking furnaces. Additives used in the coal are vermiculite, CaCO3 and bentonite. Vermiculite is used for its expansion property to improve the contact between CaCO3 and SO2 and to convey O2 into the interior of briquette; CaCO3 is used as a chemical reactant to react with SO2 to form CaSO4; and bentonite is used to develop briquette strength. Expansion of vermiculite develops loose interior structures, such as pores or cracks, inside the briquette, and thus brings enough oxygen for combustion and sulphation reaction. Effective combustion of the original carbon reduces amounts of dust in the fly ash. X-ray diffraction, optical microscopy, and scanning electron microscopy with energy dispersive X-ray analysis show that S exists in the ash only as anhydrite CaSO4, a product of SO2 reacting with CaCO3 and O2. The formation of CaSO4 effectively reduces or eliminates SO2 emission from coal combustion. The major factors controlling S retention are vermiculite, CaCO3 and combustion temperature. The S retention ratio increases with increasing vermiculite amount at 950°C. The S retention ratio also increases with increasing Ca/S molar ratio, and the best Ca/S ratio is 2-3 for most combustion. With 12 g of the original coal, 1 to 2 g of vermiculite, a molar Ca/S ratio of 2.55 by adding CaCO3, and some bentonite, a S retention ratio >65% can be readily achieved. The highest S retention ratio of 97.9% is achieved at 950°C with addition of 2 g of vermiculite, a Ca/S ratio of 2.55 and bentonite.

Synthese und Kristallstrukturen einiger Tetramethylstibonium-Hydrogendicarboxylate / Synthesis and Crystal Structures of Some Tetramethylstibonium Hydrogendicarboxylates

1982 ◽  
Vol 37 (11) ◽  
pp. 1393-1401 ◽  
Author(s):  
Beatrix Milewski-Mahrla ◽  
Hubert Schmidbaur
Keyword(s):  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Spectroscopic Data ◽  
Molar Ratio ◽  
Ionic Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Carboxylate Oxygen ◽  
Donor Acceptor ◽  
New Compounds

Reactions of pentamethylantimony (CH3)5Sb with carboxylic acids in the molar ratio 1:2 afford one equivalent of methane and essentially quantitative yields of crystalline tetramothylstibonium hydrogendicarboxylates. Six new compounds of this series have been synthesized using benzoic, o-phthalic, salicylic, 4-ethoxy-salicylic, oxalic, and malic acid, and characterized by analytical and spectroscopic data. An ionic structure with strong hydrogen bonds in the anionic components is proposed.The crystal structures of the hydrogen-dibenzoato (1), hydrogen-ortho-plithalato (2) and 4-ethoxy-hydrogen-salicylate (3) were determined by single crystal X-ray diffraction. The compounds can be described as having ionic lattices with some donor-acceptor inter­actions between the stibonium centers and the carboxylate oxygen atoms. The anions are characterized by strong hydrogen bonds O...H...O. Thus, the (CH3)4Sb-tetrahedron in 1 is distorted by two benzoate oxygon atoms (at 304(2) and 340(2) pin). The cation in 2 is largely undistorted and the anion has a hydrogenphthalate hydrogen bond of d(O...H...O) = 232 pm. The cation-anion contact in 3 is as short as d(Sb-O) = 289 pm rendering the Sb atom pentacoordinate.

Controlled Synthesis of Different Morphologies of SrWO4 Crystals via a Surfactant-Assisted Hydrothermal Precipitation Method

2013 ◽  
Vol 785-786 ◽  
pp. 449-454
Author(s):  
Yan Zhao ◽  
Chun Yan Wu ◽  
Dan Qin ◽  
Xin Lai ◽  
Si Wu ◽  
...  
Keyword(s):  
Ph Value ◽  
Precipitation Method ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
X Ray ◽  
Experimental Parameters ◽  
Infrared Spectrometer ◽  
Luminescent Spectra ◽  
Hydrothermal Precipitation ◽  
Surfactant Assisted

SrWO4 octahedrons, flowers, bundles, ellipsoids and dendrites had been successfully synthesized via surfactant-assisted method. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), photo-luminescent spectra techniques (PL) and fourier transrform infrared spectrometer (FTIR). By through various comparison experiments, it can be found that some related experimental parameters including the reagent concentration, [Sr2+]/[WO42-] molar ratio (R), aging temperature and the pH value had great influences on morphology of the products.

Synthesis, crystal structure and molecular conformation of (±)-1-oxoferruginol and (±)-shonanol

2004 ◽  
Vol 219 (10) ◽  
Author(s):  
Swastik Mondal ◽  
Monika Mukherjee ◽  
Arnab Roy ◽  
Debabrata Mukherjee
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Diffraction Data ◽  
Molecular Conformation ◽  
Membered Ring ◽  
Methyl Groups ◽  
Single Bond ◽  
X Ray Diffraction ◽  
X Ray ◽  
Chemical Structures

Abstract(±)-1-oxoferruginol and (±)-shonanol, two potential intermediates in the synthesis of tricyclic diterpenoid ferruginol, have been prepared and crystal structures of the compounds have been investigated using single-crystal X-ray diffraction data. The methyl groups of the isopropyl moiety in (±)-shonanol are disordered over two positions with occupation factors 0.65(1) and 0.35(1), respectively. Although the chemical structures of two compounds are very similar, a C—C single bond in the terminal six-membered ring of (±)-1-oxoferruginol is replaced by a C=C bond in (±)-shonanol, the quantitative isostructurality index calculations indicate that the structures are not isostructural. Intermolecular O—H…O hydrogen bonds between pairs of molecules in the compounds related by center of inversion lead to characteristic dimers forming R

scholarly journals Effect of Mg/Al molar ratio on the basicity of Mg-Al mixed oxide derived from Mg-Al hydrotalcite

2020 ◽  
Vol 10 (6) ◽  
pp. 625
Author(s):  
Said Arhzaf ◽  
Mohammed Naciri Bennani ◽  
Sadik Abouarnadasse ◽  
Hamid Ziyat ◽  
Omar Qabaqous
Keyword(s):  
Thermal Analysis ◽  
Mixed Oxide ◽  
Mixed Oxides ◽  
Molar Ratio ◽  
Acid Molecule ◽  
X Ray Diffraction ◽  
Phenol Adsorption ◽  
X Ray ◽  
Maximum Quantity ◽  
Uv Visible

<p>The fundamental character of the Mg-Al mixed oxide (Mg<sub>n</sub>(Al)O), derived from the Mg-Al hydrotalcite (Mg<sub>n</sub>Al-CO<sub>3</sub>-HT), where n corresponds to the Mg/Al molar ratio (n: 2, 2.5, 3, 3.5 and 4), was studied by using the adsorption of phenol as a probe acid molecule. The hydrotalcite precursors were prepared by the coprecipitation method. Their derived mixed oxides were obtained by thermal treatment at 450°C in a flow of air. The resulting solids were characterized by X-ray fluorescence spectroscopy (XRF), X-ray diffraction (XRD), infrared spectroscopy (FTIR), thermogravimetric and differential thermal analysis             (TG-DTA), nitrogen physisorption (BET) and phenol chemisorption. The phenol adsorption followed by UV-Visible spectrophotometry shows that the basicity increases with the Mg/Al molar ratio, such that maximum quantity of phenol adsorbed (Q<sub>ads</sub> = 0.54 mmol/g <sub>cat</sub>) was obtained with the mixed oxide derived from the Mg-Al hydrotalcite of Mg/Al molar ratio equal to 3.5.</p>

Notizen: Bridging of Trigoldsulfonium Clusters by a Silver(I) Ion

1997 ◽  
Vol 52 (2) ◽  
pp. 301-304 ◽  
Author(s):  
Alexander Sladek ◽  
Hubert Schmidbaur
Keyword(s):  
Crystal Structure ◽  
Silver Atom ◽  
Metal Cluster ◽  
Phosphine Ligands ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
X Ray ◽  
Site Exchange ◽  
Mixed Metal Cluster ◽  
Short Contacts

Abstract Treatment of tris[(triphenylphosphine)gold(I)]-sulfonium tetrafluoroborate with AgBF4 (molar ratio 2:1) in tetrahydrofuran affords a hepta-nuclear mixed-metal cluster trication {[(Ph3P)6Au6AgS2](thf)}3+ as the tetrafluorobor­ate salt. The crystal structure of the compound has been determined by X-ray diffraction. The sil­ver atom is found in a bridging position between the two Au3S units with short contacts to both sulfur atoms and to three out of six gold atoms. The coordination sphere of the silver atom is complemented by a tetrahydrofuran molecule. In di(tri)chlorom ethane solutions there is rapid site exchange of the silver coordination as shown by virtual equivalence of the phosphine ligands on the NMR time scale at ambient temperature.

Photocatalytic Activity of CuO/ZnO Heterostructure Nanocrystals under UV-Visible Light Irradiation

2014 ◽  
Vol 787 ◽  
pp. 35-40 ◽  
Author(s):  
Xiao Yan Zhou ◽  
Peng Wei Zhou ◽  
Hao Guo ◽  
Bo Yang ◽  
Ru Fei Ren
Keyword(s):  
Photocatalytic Activity ◽  
Visible Light ◽  
Visible Light Irradiation ◽  
Cuo Nanoparticles ◽  
Light Irradiation ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
X Ray ◽  
Vis Spectroscopy ◽  
Uv Visible

The p-n junction photocatalysts, p-CuO (at. 0-25%)/n-ZnO nanocomposite were prepared through hydrothermal method without using any organic solvent or surfactant. The as-prepared samples were characterized by X-ray diffraction, scanning electron microscopy, energy dispersive X-Ray spectroscopy, and UV-vis spectroscopy. The results demonstrated that the CuO/ZnO nanocomposite presented a two-dimensional morphology composed of sheet-like ZnO nanostructures adorned with CuO nanoparticles. The photocatalytic activity of CuO/ZnO with different Cu/Zn molar rations and pure ZnO synthesized by the identical synthetic route were evaluated by degrading methylene blue (MB) dye under UV-visible light irradiation. The CuO/ZnO with Cu/Zn molar ratio of 4% exhibits the highest photocatalytic activity compared that of the other photocatalysts under the identical conditions. It is mainly attributed to the increased charge separation rate in the nanocomposite and the extended photo-responding range.

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