scholarly journals Diferrocenyl Thioketone: Reactions with (Bisphosphane)Pt(0) Complexes—Electrochemical and Computational Studies

Materials ◽  
2019 ◽  
Vol 12 (17) ◽  
pp. 2832 ◽  
Author(s):  
Sebastian Gröber ◽  
Piotr Matczak ◽  
Sławomir Domagała ◽  
Thomas Weisheit ◽  
Helmar Görls ◽  
...  
Keyword(s):  
Quantum Chemical ◽  
Room Temperature ◽  
Electrode Process ◽  
Spectroscopic Methods ◽  
Cyclic Voltammogram ◽  
Computational Studies ◽  
X Ray Diffraction ◽  
X Ray ◽  
Diffusion Controlled ◽  
Bond Character

Diferrocenyl thioketone reacts smoothly with (bisphosphane)Pt(0) complexes in toluene solution at room temperature yielding 1:1 adducts identified as ferrocenyl (Fc) functionalized platinathiiranes. Their structures were unambiguously confirmed by means of spectroscopic methods as well as by X-ray diffraction analysis. A unique, ferrocene-rich platinathiirane, bearing three Fc-units, was prepared starting with [bis(diphenylphosphino)ferrocene] Pt(0(η2-norbornene). For comparison, a similar platinathiirane with one Fc-unit was obtained from the reaction of the latter complex with thiobenzophenone. Quantum-chemical calculations were carried out to describe the bonding pattern and frontier molecular orbitals of the ferrocene-rich platinathiirane complexes. These calculations confirmed that the C=S bond loses its formally double-bond character upon complexation (bisphosphane)Pt(0). Cyclic voltammetry measurements were performed to characterize the obtained platinathiiranes in CH2Cl2 solutions. For comparison, the cyclic voltammogram for diferrocenyl thioketoneas a mixed-valent (FeII-FeIII) compound was also recorded and analyzed. The results point out to a diffusion controlled electrode process in case of differocenyl thioketone and mixed diffusion and adsorption controlled electrode process in the case of the studied platinathiiranes.

Formation of ZnO Doped with Mn Thin Film by Electrodeposition and Magnetic Behaviour.

2005 ◽  
Vol 879 ◽  
Author(s):  
M. Abid ◽  
C. Terrier ◽  
J-P Ansermet ◽  
K. Hjort
Keyword(s):  
Thin Film ◽  
Thin Films ◽  
Room Temperature ◽  
Magnetic Behaviour ◽  
Spectroscopic Methods ◽  
X Ray Diffraction ◽  
X Ray ◽  
Doped Zno ◽  
Mn Doped ◽  
Weak Ferromagnetic

AbstractFollowing the theory, ferromagnetism is predicted in Mn- doped ZnO, Indeed, ferromagnetism above room temperature was recently reported in thin films as well as in bulk samples made of this material. Here, we have prepared Mn doped ZnO by electrodeposition. The samples have been characterized by X-ray diffraction and spectroscopic methods to ensure that the dopants are substitutional. Some samples exhibit weak ferromagnetic properties at room temperature, however to be useful for spintronics this material need additional carriers provided by others means.

Synthesis of a Stable Compound with Fivefold Bonding Between Two Chromium(I) Centers

Science ◽  
2005 ◽  
Vol 310 (5749) ◽  
pp. 844-847 ◽  
Author(s):  
Tailuan Nguyen ◽  
Andrew D. Sutton ◽  
Marcin Brynda ◽  
James C. Fettinger ◽  
Gary J. Long ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Room Temperature ◽  
Computational Studies ◽  
X Ray Diffraction ◽  
Electron Pairs ◽  
Stable Compound ◽  
X Ray ◽  
Slight Excess ◽  
Stable Species ◽  
Moisture Sensitive

Although in principle transition metals can form bonds with six shared electron pairs, only quadruply bonded compounds can be isolated as stable species at room temperature. Here we show that the reduction of {Cr(μ-Cl)Ar′}2 [where Ar′ indicates C6H3-2,6(C6H3-2,6-Pri2)2 and Pr indicates isopropyl] with a slight excess of potassium graphite has produced a stable compound with fivefold chromium-chromium (Cr–Cr) bonding. The very air- and moisture-sensitive dark red crystals of Ar′CrCrAr′ were isolated with greater than 40% yield. X-ray diffraction revealed a Cr–Cr bond length of 1.8351(4) angstroms (where the number in parentheses indicates the standard deviation) and a planar transbent core geometry. These data, the structure's temperature-independent paramagnetism, and computational studies support the sharing of five electron pairs in five bonding molecular orbitals between two 3d5 chromium(I) ions.

Structures of Energetic Acetylene Derivatives HC≡CCH2ONO2, (NO2)3CCH2C≡CCH2C(NO2)3 and Trinitroethane, (NO2)3CCH3

2013 ◽  
Vol 68 (5-6) ◽  
pp. 719-731 ◽  
Author(s):  
Thomas M. Klapötke ◽  
Burkhard Krumm ◽  
Richard Moll ◽  
Alexander Penger ◽  
Stefan M. Sproll ◽  
...  
Keyword(s):  
Electron Diffraction ◽  
Gas Phase ◽  
Quantum Chemical ◽  
Room Temperature ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Polar Solvents ◽  
X Ray ◽  
Nmr Study ◽  
Acetylene Derivatives

The molecular structures and relative ratios of the two conformers (anti and gauche) of HCCCH2ONO2 detected in the gas phase at room temperature have been determined by electron diffraction. The results are discussed on the basis of quantum chemical calculations. The molecular structures of (NO2)3CCH2C≡CCH2C(NO2)3 and (NO2)3CCH3 have been determined by X-ray diffraction. A109Ag NMR study was performed for silver trinitromethanide Ag[C(NO2)3] in various polar solvents.

scholarly journals Syntheses, Reactivities, Characterization, and Crystal Structures of Dipalladium Complexes Containing the 1,3-pyrimidinyl Ligand: Structures of [Pd(PPh3)(Br)]2(μ,η2-C4H3N2)2, [Pd(Br)]2(μ,η2-Hdppa)2, and [{Pd(PPh3)(CH3CN)}2(μ,η2-C4H3N2)2][BF4]2

Molecules ◽  
2020 ◽  
Vol 25 (9) ◽  
pp. 2035
Author(s):  
Hsiao-Fen Wang ◽  
Kuang-Hway Yih ◽  
Gene-Hsiang Lee
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Room Temperature ◽  
Palladium Complex ◽  
Chloroform Solution ◽  
Bidentate Ligand ◽  
Tridentate Ligand ◽  
Spectroscopic Methods ◽  
X Ray Diffraction ◽  
X Ray

In a refluxing chloroform solution, the η1-pyrimidinyl {pyrimidinyl = C4H3N2} palladium complex [Pd(PPh3)2(η1-C4H3N2)(Br)], 1 exhibited intermolecular displacement of two triphenylphosphine ligands to form the doubly bridged η2-pyrimidinyl Dipalladium complex [Pd(PPh3)(Br)]2(μ,η2-C4H3N2)2, 3. The treatment of 1 with Hdppa {Hdppa = N,N-bisdiphenyl phosphinoamine} in refluxing dichloromethane yielded the doubly bridged Hdppa dipalladium complex [Pd(Br)]2(μ,η2-Hdppa)2, 4. Complex 1 reacted with the bidentate ligand, NH4S2CNC4H8 and, NaS2COEt, and the tridentate ligand, KTp {Tp = tris(pyrazoyl-1-yl)borate}, to form the η2-dithio η1-pyrimidinyl complex [Pd(PPh3)(η1-C4H3N2)(η2-SS)], (5: SS = S2CNC4H8; 6: SS = S2COEt) and η2-Tp η1-pyrimidinyl complex [Pd(PPh3)(η1-C4H3N2)(η2-Tp)], 7, respectively. Treatment of 1 with AgBF4 in acetonitrile at room temperature resulted in the formation of the doubly bridged η2-pyrimidinyl dipalladium complex [{Pd(PPh3)(CH3CN)}2(μ,η2-C4H3N2)2][BF4]2, 8. All of the complexes were identified using spectroscopic methods, and complexes 3, 4, and 8 were determined using single-crystal X-ray diffraction analyses.

Formation of meso-1,2-Bis(dimethylamino)-1,2-diphenylethane by Oxidative C-C Coupling Reaction

2005 ◽  
Vol 60 (10) ◽  
pp. 1083-1087 ◽  
Author(s):  
Holger Fleischer ◽  
Dieter Schollmeyer
Keyword(s):  
Molecular Structure ◽  
Quantum Chemical ◽  
Phenyl Ring ◽  
Room Temperature ◽  
Negative Charge ◽  
Coupling Reaction ◽  
X Ray Diffraction ◽  
Dft Methods ◽  
Butyl Lithium ◽  
X Ray

The title compound was obtained from the reaction of N,N-dimethylbenzylamine with n-butyl lithium and sulfur in tetrahydrofuran at room temperature. Its molecular structure was investigated by means of single crystal X-ray diffraction and quantum chemical DFT methods. The formation of meso-1,2-bis(dimethylamino)-1,2-diphenylethane is likely to be due to an unusual α-deprotonation of N,N-dimethylbenzylamine, instead of the well known ortho-lithiation, with a subsequent oxidative C-C coupling of the anions. Ab initio calculations of the corresponding α- and o-deprotonated anions of N,N-dimethylbenzylamine showed the former to be more stable than the latter, due to delocalisation of the negative charge over the π-system of the phenyl ring. The choice of solvent and temperature is seen as the main reason for the unusual course of the reaction.

Electron Microscopy of Human Gallstones

1971 ◽  
Vol 29 ◽  
pp. 296-297
Author(s):  
C. Wolpers ◽  
R. Blaschke
Keyword(s):  
Electron Microscopy ◽  
Room Temperature ◽  
Bile Pigment ◽  
X Ray Diffraction ◽  
Triclinic Crystal System ◽  
X Ray ◽  
Follow Up Study ◽  
Infra Red ◽  
Main Components

Scanning microscopy was used to study the surface of human gallstones and the surface of fractures. The specimens were obtained by operation, washed with water, dried at room temperature and shadowcasted with carbon and aluminum. Most of the specimens belong to patients from a series of X-ray follow-up study, examined during the last twenty years. So it was possible to evaluate approximately the age of these gallstones and to get information on the intensity of growing and solving.Cholesterol, a group of bile pigment substances and different salts of calcium, are the main components of human gallstones. By X-ray diffraction technique, infra-red spectroscopy and by chemical analysis it was demonstrated that all three components can be found in any gallstone. In the presence of water cholesterol crystallizes in pane-like plates of the triclinic crystal system.

A TEM investigation of a hyper-eutectic lead-tin alloy

1988 ◽  
Vol 46 ◽  
pp. 562-563
Author(s):  
John A. Sutliff
Keyword(s):  
Volume Diffusion ◽  
Eutectic Mixture ◽  
Precipitation Reaction ◽  
Directionally Solidified ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Diffusion Controlled ◽  
Discontinuous Precipitation Reaction ◽  
Controlled Precipitation

Near-eutectic Pb-Sn alloys are important solders used by the electronics industry. In these solders, the eutectic mixture, which solidifies last, is the important microstructural consituent. The orientation relation (OR) between the eutectic phases has previously been determined for directionally solidified (DS) eutectic alloys using x-ray diffraction or electron chanelling techniques. In the present investigation the microstructure of a conventionally cast, hyper-eutectic Pb-Sn alloy was examined by transmission electron microscopy (TEM) and the OR between the eutectic phases was determined by electron diffraction. Precipitates of Sn in Pb were also observed and the OR determined. The same OR was found in both the eutectic and precipitation reacted materials. While the precipitation of Sn in Pb was previously shown to occur by a discontinuous precipitation reaction,3 the present work confirms a recent finding that volume diffusion controlled precipitation can also occur.Samples that are representative of the solder's cast microstructure are difficult to prepare for TEM because the alloy is multiphase and the phases are soft.

Electron Microscope study of commensurate-incommensurate phase transition in BaZnGeO4

1990 ◽  
Vol 48 (4) ◽  
pp. 172-173
Author(s):  
Naoki Yamamoto ◽  
Makoto Kikuchi ◽  
Tooru Atake ◽  
Akihiro Hamano ◽  
Yasutoshi Saito
Keyword(s):  
Phase Transition ◽  
Electron Microscope Study ◽  
Room Temperature ◽  
Hexagonal Lattice ◽  
Ferroelectric Materials ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Periodic Arrays ◽  
Modulation Wave Vector

BaZnGeO4 undergoes many phase transitions from I to V phase. The highest temperature phase I has a BaAl2O4 type structure with a hexagonal lattice. Recent X-ray diffraction study showed that the incommensurate (IC) lattice modulation appears along the c axis in the III and IV phases with a period of about 4c, and a commensurate (C) phase with a modulated period of 4c exists between the III and IV phases in the narrow temperature region (—58°C to —47°C on cooling), called the III' phase. The modulations in the IC phases are considered displacive type, but the detailed structures have not been studied. It is also not clear whether the modulation changes into periodic arrays of discommensurations (DC’s) near the III-III' and IV-V phase transition temperature as found in the ferroelectric materials such as Rb2ZnCl4.At room temperature (III phase) satellite reflections were seen around the fundamental reflections in a diffraction pattern (Fig.1) and they aligned along a certain direction deviated from the c* direction, which indicates that the modulation wave vector q tilts from the c* axis. The tilt angle is about 2 degree at room temperature and depends on temperature.

Xenon Trioxide Adducts of O-Donor Ligands; [(CH3)2CO]3XeO3, [(CH3)2SO]3(XeO3)2, (C5H5NO)3(XeO3)2, and [(C6H5)3PO]2XeO3

2018 ◽  
Author(s):  
Katherine Marczenko ◽  
James Goettel ◽  
Gary Schrobilgen
Keyword(s):  
Room Temperature ◽  
Triphenylphosphine Oxide ◽  
Donor Ligands ◽  
Mechanical Shock ◽  
X Ray Diffraction ◽  
X Ray ◽  
Oxygen Coordination ◽  
Xenon Trioxide ◽  
Distorted Octahedra ◽  
Coordination Spheres

Oxygen coordination to the Xe(VI) atom of XeO<sub>3</sub> was observed in its adducts with triphenylphosphine oxide, dimethylsulfoxide, pyridine-N-oxide, and acetone. The crystalline adducts were characterized by low-temperature, single-crystal X-ray diffraction and Raman spectroscopy. Unlike solid XeO<sub>3</sub>, which detonates when mechanically or thermally shocked, the solid [(C<sub>6</sub>H<sub>5</sub>)<sub>3</sub>PO]<sub>2</sub>XeO<sub>3</sub>, [(CH<sub>3</sub>)<sub>2</sub>SO]<sub>3</sub>(XeO<sub>3</sub>)<sub>2</sub>,<sub> </sub>and (C<sub>5</sub>H<sub>5</sub>NO)<sub>3</sub>(XeO<sub>3</sub>)<sub>2</sub> adducts are insensitive to mechanical shock, but undergo rapid deflagration when ignited by a flame. Both [(C<sub>6</sub>H<sub>5</sub>)<sub>3</sub>PO]<sub>2</sub>XeO<sub>3 </sub>and (C<sub>5</sub>H<sub>5</sub>NO)<sub>3</sub>(XeO<sub>3</sub>)<sub>2</sub> are air-stable whereas [(CH<sub>3</sub>)<sub>2</sub>SO]<sub>3</sub>(XeO<sub>3</sub>)<sub>2</sub> slowly decomposes over several days and [(CH<sub>3</sub>)<sub>2</sub>CO]<sub>3</sub>XeO<sub>3</sub> undergoes adduct dissociation at room temperature. The xenon coordination sphere of [(C<sub>6</sub>H<sub>5</sub>)<sub>3</sub>PO]<sub>2</sub>XeO<sub>3</sub> is a distorted square pyramid which provides the first example of a five-coordinate XeO<sub>3</sub> adduct. The xenon coordination spheres of the remaining adducts are distorted octahedra comprised of three Xe---O secondary contacts that are approximately trans to the primary Xe–O bonds of XeO<sub>3</sub>. Quantum-chemical calculations were used to assess the Xe---O adduct bonds, which are predominantly electrostatic σ-hole bonds between the nucleophilic oxygen atoms of the bases and the σ-holes of the xenon atoms.

Effect of trytophan as dopant on potassium acid phthalate single crystals

2019 ◽  
Author(s):  
Chem Int
Keyword(s):  
Single Crystals ◽  
Room Temperature ◽  
Visible Region ◽  
X Ray Diffraction ◽  
X Ray ◽  
Slow Evaporation Technique ◽  
Absorption Studies ◽  
Evaporation Technique ◽  
Potassium Acid Phthalate ◽  
Acid Phthalate

Optically transparent single crystals of potassium acid phthalate (KAP, 0.5 g) 0.05 g and 0.1 g (1 and 2 mol %) trytophan were grown in aqueous solution by slow evaporation technique at room temperature. Single crystal X- ray diffraction analysis confirmed the changes in the lattice parameters of the doped crystals. The presence of functional groups in the crystal lattice has been determined qualitatively by FTIR analysis. Optical absorption studies revealed that the doped crystals possess very low absorption in the entire visible region. The dielectric constant has been studied as a function of frequency for the doped crystals. The thermal stability was evaluated by TG-DSC analysis.

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