Eine elektrochemische und strukturelle Studie an den Eisensilylamiden Fe[N(SiMe3)2]2 und Fe[N(SiMe3)2]3 / An Electrochemical and Structural Study of the Iron Silylamides Fe[N(SiMe3)2]2 and Fe[N(SiMe3)2]3

2012 ◽  
Vol 67 (6) ◽  
pp. 549-556 ◽  
Author(s):  
Günter Margraf ◽  
Frauke Schödel ◽  
Inge Sänger ◽  
Michael Bolte ◽  
Matthias Wagner ◽  
...  
Keyword(s):  
Cyclic Voltammogram ◽  
X Ray Diffraction ◽  
Amido Complexes ◽  
X Ray ◽  
Redox Transition ◽  
Transfer Processes ◽  
Irreversible Oxidation ◽  
Reaction Solution ◽  
Reversible Redox ◽  
Electron Transfer Processes

The bis(trimethyl)silylamido complex Na(THF){Fe[N(SiMe3)2]3} and the disilane tBu3SiSitBu3 were obtained from the reaction of Fe[N(SiMe3)2]3 with the sodium silanide Na(THF)2[SitBu3] in a mixture of benzene and THF. Single crystals of Na(THF){Fe[N(SiMe3)2]3} suitable for X-ray diffraction were grown from the reaction solution at ambient temperature (orthorhombic, C2221, Z = 4). The solid-state structure features a contact-ion pair with two short N-Na contacts. The THF adducts {M(THF)2[N(SiMe3)2]2} reacted with 2,2´-bipyridine to give the corresponding complexes {M(2,2´bipy)[N(SiMe3)2]2} (M= Mn; Fe). Their structures (M= Fe: orthorhombic, Pca21, Z = 8; M = Mn: orthorhombic, Pbca, Z = 8) feature monomeric units. The cyclic voltammogram of Fe[N(SiMe3)2]3 revealed a reversible redox transition with the potential of -0;523 V (E½), which was assigned to the Fe(III)[N(SiMe3)2]3 → Fe(II)[N(SiMe3)2]-3 redox transition, whereas the compounds {Fe(THF)2[N(SiMe3)2]2} (Eox = -0;379 V) and {Fe(2,2´bipy)[N(SiMe3)2]2} (Eox = -0;436 V) featured irreversible oxidation waves. The related manganese bis(trimethylsilyl)amido complexes {Mn(THF)2[N(SiMe3)2]2} (Eox = -0;458 V) and {Mn(2,2´bipy)[N(SiMe3)2]2} (Eox = -0513 V) also underwent irreversibile electron transfer processes.

Optical properties and energy transfer processes in Tb3+-doped ZnSe quantum dots

2021 ◽  
Author(s):  
Nguyen Ca ◽  
N. D Vinh ◽  
Phan Van Do ◽  
N. T. Hien ◽  
Xuan Hoa Vu ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Quantum Dots ◽  
Chemical Method ◽  
X Ray Diffraction ◽  
Wet Chemical Method ◽  
X Ray ◽  
Transfer Processes ◽  
Transmission Electron ◽  
Wet Chemical

Tb3+-doped ZnSe quantum dots (QDs) with Tb content in the range of 0.5 - 7% were successfully synthesized by a wet chemical method. X-ray diffraction (XRD) and transmission electron microscopy...

Structural, Optical, Photocatalytic and Electrochemical Studies of PbS Nanoparticles

2020 ◽  
Vol 61 ◽  
pp. 18-31 ◽  
Author(s):  
Peter A. Ajibade ◽  
Abimbola E. Oluwalana
Keyword(s):  
Particle Sizes ◽  
X Ray Diffraction ◽  
Lead Sulphide ◽  
Electron Transfer Process ◽  
Sem Images ◽  
Pbs Nanoparticles ◽  
X Ray ◽  
Diffusion Controlled ◽  
Reversible Redox ◽  
Diffraction Patterns

Oleic acid (OA) and octadecylamine (ODA) capped lead sulphide (PbS) nanoparticles were prepared at 150, 190 and 230 °C. X-ray diffraction patterns indicates that the synthesized PbS nanoparticles were in the rock cubic salt crystalline phase. The particle sizes of the as-prepared PbS nanoparticles are in the range 2.91–10.05 nm for OA-PbS(150), 24.92–39.98 nm for ODA-PbS(150), 9.26 – 29.08 nm for OA-PbS(190), 34.54 – 48.04 nm for ODA-PbS(190), 17.96–88.07 nm for OA-PbS(230) and 53.60 – 94.42 nm for ODA-PbS(230). SEM images revealed flaky and agglomerated spherical like morphology for the nanoparticles. The energy bandgap of the PbS nanoparticles are in the range 4.14 – 4.25 eV, OA-PbS(230) have the lowest bandgap of 4.14 eV while ODA-PbS(150) have the highest bandgap of 4.25 eV. The PbS nanoparticles were used as photocatalyst for the degradation of Rhodamine B and OA-PbS(150) showed efficiency of 44.11% after 360 mins. Cyclic voltammetry of the PbS nanoparticles showed a reversible redox reaction and linear Randles-Sevcik plots indicates electron transfer process is diffusion controlled.

scholarly journals Direct Preparation and Characterization of Copper Pentacyanonitrosylferrate Nanoparticles

2015 ◽  
Vol 2015 ◽  
pp. 1-6 ◽  
Author(s):  
D. R. Do Carmo ◽  
M. M. Souza ◽  
U. O. Bicalho ◽  
V. S. Dos Santos ◽  
J. P. Souza ◽  
...  
Keyword(s):  
Charge Transfer Band ◽  
Cyclic Voltammogram ◽  
X Ray Diffraction ◽  
X Ray ◽  
Peak Broadening ◽  
Vis Spectroscopy ◽  
Intervalence Charge Transfer ◽  
Direct Preparation ◽  
Graphite Paste Electrode ◽  
Paste Electrode

The present work describes the preparation of nanoparticles of copper pentacyanonitrosyl complexes starting from the compound sodium nitroprusside. Copper pentacyanonitrosylferrate (NCuNP) nanoparticles were successfully synthesized by using deionized water and formamide as solvent. The material was characterized by Fourier-transforming infrared spectroscopy (FT-IR), X-ray diffraction (XRD), ultraviolet-visible (UV-Vis) spectroscopy, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and cyclic voltammetry (CV). The results revealed that the electronic spectra of NCuNP exhibited a broad intervalence charge transfer band at 685 nm. An XRD peak broadening pattern of the NCuNP was verified, indicating a particle decrease when formamide is used. The particle size of NCuNP is estimated to be 80 nm. The cyclic voltammogram of the modified graphite paste electrode with NCuNP showed two redox pairs with formal potentialsEθ′=0.36 V andEθ′=0.78 V (ν=20 mV s−1; KCl 1.0 M), attributed to the redox processCuI/CuIIand [FeII(CN)5NO]/[FeIII(CN)5NO], respectively. The graphite paste electrode with NCuNP presents electrocatalytic response for Sulfite determination.

Formation and decomposition of the Sb(III)/Li cage [{Sb(P-t-Bu)3}2Li6·6THF]

2002 ◽  
Vol 80 (11) ◽  
pp. 1421-1427 ◽  
Author(s):  
Alan Bashall ◽  
Felipe García ◽  
Gavin T Lawson ◽  
Mary McPartlin ◽  
Alexander Rothenberger ◽  
...  
Keyword(s):  
Solid State ◽  
Low Temperature ◽  
Spectroscopic Studies ◽  
X Ray Diffraction ◽  
Initial Formation ◽  
X Ray ◽  
Cage Complex ◽  
Reaction Solution

The heterometallic Sb(III)/Li cage complex [{Sb(P-t-Bu)3}2Li6·6THF] (1) is obtained by the low-temperature (<0°C) reaction of Sb(NMe2)3 with t-BuPHLi (1:3 equiv) in THF. Thermolysis of this reaction solution leads to the formation of the bicyclic distibane [(t-BuP)3Sb]2 (2). 31P NMR spectroscopic studies reveal that this process involves initial formation of [(t-BuP)3Sb]– and [t-Bu(H)PP-t-Bu]– anions. Complexes 1 and 2 have been characterized in the solid state by X-ray diffraction studies.Key words: antimony, lithium, cage.

Phosphanhaltige Palladium(II)-, Platin(II)-und Gold(I)-Komplexe mit dem Di-tbutyliminodicarboxylat-Anion N(C O2tBu)2− / Phosphine Palladium(II), Platinum(II) and Gold(I) Complexes of the Di-tbutyliminocarboxylate Anion N(C O2tBu)2−

1997 ◽  
Vol 52 (10) ◽  
pp. 1203-1206 ◽  
Author(s):  
Markus Prem ◽  
Kurt Polbom ◽  
Wolfgang Beck
Keyword(s):  
X Ray Diffraction ◽  
Amido Complexes ◽  
X Ray

The amido complexes L2M(Cl)N(Boc)2 (M = Pd, Pt; L = PPh3, PnBu3, PEt3; 2 L = COD) and Ph3PAuNBoc2 were prepared from Na+N(CO2tBu)2− and L2MCl2 or Ph3PAuNO3, respectively. The structure of cis-(Ph3P)2Pt(Cl)NBoc2 was determined by X-ray diffraction.

One-electron transfer processes in the reaction of elemental gallium, indium, and tin with tetrahalogeno-ortho-benzoquinones

1989 ◽  
Vol 67 (11) ◽  
pp. 1807-1814 ◽  
Author(s):  
Theodore A. Annan ◽  
Dennis G. Tuck
Keyword(s):  
Electron Transfer ◽  
Reaction Mechanism ◽  
Paramagnetic Species ◽  
X Ray ◽  
Transfer Processes ◽  
Electron Transfer Processes ◽  
Derivatives Of

Tin reacts with tetrahalogeno-o-benzoquinones X4C6O2 (X = Cl, Br) in refluxing toluene to give the tin(IV) catecholato species Sn(O2C6X4)2, and neutral and anionic derivatives have also been obtained. A mixture of Sn + X4C6O2-o + I2 + 1,10-phenanthroline (phen) yields SnI2(O2C6X4)phen. With gallium or indium (= M), the corresponding experiments give derivatives of MII (e.g., [M(O2C6X4)phen]2), or MIII (e.g., MI(O2C6X4)phen). Intermediate paramagnetic species were detected in the case of [Formula: see text], and a reaction mechanism involving one-electron transfer processes is proposed on the basis of these results. Solvated crystals of the compound InCl(O2C6Cl4)(C6H7N)3 were obtained from CH2Cl2 solution, and the structure of this molecule has been determined by X-ray crystallographic methods. Keywords: gallium, indium, tin, benzoquinones, oxidation.

Axially substituted phosphorous(v) corrole with polycyclic aromatic hydrocarbons: syntheses, X-ray structures, and photoinduced energy and electron transfer studies

2018 ◽  
Vol 42 (10) ◽  
pp. 8230-8240 ◽  
Author(s):  
B. Shivaprasad Achary ◽  
A. R. Ramya ◽  
Jagadeesh Babu Nanubolu ◽  
Sairaman Seetharaman ◽  
Gary N. Lim ◽  
...  
Keyword(s):  
Electron Transfer ◽  
Excited State ◽  
Aromatic Hydrocarbons ◽  
State Energy ◽  
Excited State Energy ◽  
X Ray ◽  
Transfer Processes ◽  
Energy And Electron Transfer ◽  
Polycyclic Aromatic ◽  
Electron Transfer Processes

Excited state energy and electron transfer processes in naphthalene and pyrene appended phosphorous(v) corroles.

scholarly journals Dihydrogen Bonds in Salts of Boron Cluster Anions [BnHn]2− with Protonated Heterocyclic Organic Bases

Crystals ◽  
2019 ◽  
Vol 9 (7) ◽  
pp. 330 ◽  
Author(s):  
Varvara V. Avdeeva ◽  
Anna V. Vologzhanina ◽  
Elena A. Malinina ◽  
Nikolai T. Kuznetsov
Keyword(s):  
Cluster Anions ◽  
X Ray Diffraction ◽  
X Ray ◽  
Boron Cluster ◽  
Organic Bases ◽  
Dihydrogen Bonds ◽  
Reaction Solution ◽  
Ft Ir ◽  
Hydrolysis Of ◽  
Ft Ir Spectroscopy

Dihydrogen bonds attract much attention as unconventional hydrogen bonds between strong donors of H-bonding and polyhedral (car)borane cages with delocalized charge density. Salts of closo-borate anions [B10H10]2− and [B12H12]2− with protonated organic ligands 2,2’-dipyridylamine (BPA), 1,10-phenanthroline (Phen), and rhodamine 6G (Rh6G) were selectively synthesized to investigate N−H...H−B intermolecular bonding. It was found that the salts contain monoprotonated and/or diprotonated N-containing cations at different ratios. Protonation of the ligands can be implemented in an acidic medium or in water because of hydrolysis of metal cations resulting in the release of H3O+ cations into the reaction solution. Six novel compounds were characterized by X-ray diffraction and FT-IR spectroscopy. It was found that strong dihydrogen bonds manifest themselves in FT-IR spectra that allows one to use this technique even in the absence of crystallographic data.

Electrochemical Synthesis and Characterization of NaCuO2

1994 ◽  
Vol 346 ◽  
Author(s):  
Gerald L. Roberts ◽  
Susan M. Kauzlarich
Keyword(s):  
Potassium Hydroxide ◽  
Reference Electrode ◽  
Room Temperature Resistivity ◽  
Cyclic Voltammogram ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hydroxide Melt ◽  
Black Plate ◽  
Temperature Resistivity

ABSTRACTNaCuO2 has been prepared via electrodeposition from a sodium hydroxide/potassium hydroxide melt and characterized by single crystal and powder X-ray diffraction, magnetic susceptibility, and resistivity. Clusters of blue-black plate-like and needle crystals are grown at positive potentials on a platinum anode with a platinum or a zirconium crucible serving as the cathode and a platinum reference electrode. Details of the electrochemical procedure are described, along with a cyclic voltammogram. NaCuO2 exhibits temperature independent paramagnetism over the temperature range 30 – 300 K. Its room temperature resistivity is greater than 106 Ω-cm.

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