scholarly journals X-ray structure of a Ni(ii)–tri-phenoxyl radical complex

2015 ◽  
Vol 44 (41) ◽  
pp. 17924-17926 ◽  
Author(s):  
Laurent Benisvy ◽  
Galina M. Zats ◽  
Ohad Fleker ◽  
Dmitry S. Yufit ◽  
Maylis Orio ◽  
...  
Keyword(s):  
Phenoxyl Radical ◽  
X Ray ◽  
Radical Complex ◽  
Square Planar ◽  
First Time

The diimino-diphenolato neutral square-planar Ni(ii) complex, NiL2, is readily oxidised with 2 equiv. of Ag[SbF6], to produce an unprecedented octahedral Ni(ii) tris(phenoxyl) radical complex, [Ni(L˙)3][SbF6]2. This study reveals, for the first time, the X-ray structure of a metal–tri-phenoxyl radical complex.

High-accuracy X-ray absorption spectra from mMsolutions of nickel (II) complexes with multiple solutions using transmission XAS

2015 ◽  
Vol 22 (4) ◽  
pp. 1008-1021 ◽  
Author(s):  
Christopher T. Chantler ◽  
M. Tauhidul Islam ◽  
Stephen P. Best ◽  
Lachlan J. Tantau ◽  
Chanh Q. Tran ◽  
...  
Keyword(s):  
Multiple Solutions ◽  
High Accuracy ◽  
Hybrid Technique ◽  
Edge Structure ◽  
New Approach ◽  
X Ray ◽  
Square Planar ◽  
Transmission Measurements ◽  
First Time ◽  
X Ray Absorption

A new approach is introduced for determining X-ray absorption spectroscopy (XAS) spectra on absolute and relative scales using multiple solutions with different concentrations by the characterization and correction of experimental systematics. This hybrid technique is a development of standard X-ray absorption fine structure (XAFS) along the lines of the high-accuracy X-ray extended range technique (XERT) but with applicability to solutions, dilute systems and cold cell environments. This methodology has been applied to determining absolute XAS of bis(N-n-propyl-salicylaldiminato) nickel(II) and bis(N-i-propyl-salicylaldiminato) nickel(II) complexes with square planar and tetrahedral structures in 15 mMand 1.5 mMdilute solutions. It is demonstrated that transmission XAS from dilute systems can provide excellent X-ray absorption near-edge structure (XANES) and XAFS spectra, and that transmission measurements can provide accurate measurement of subtle differences including coordination geometries. For the first time, (transmission) XAS of the isomers have been determined from low-concentration solutions on an absolute scale with a 1–5% accuracy, and with relative precision of 0.1% to 0.2% in the active XANES and XAFS regions after inclusion of systematic corrections.

Interaction of ditertiary phosphines with phenyl- and 1-naphthyldithiocarbamatonickel(II)

1985 ◽  
Vol 50 (6) ◽  
pp. 1383-1390
Author(s):  
Aref A. M. Aly ◽  
Ahmed A. Mohamed ◽  
Mahmoud A. Mousa ◽  
Mohamed El-Shabasy
Keyword(s):  
Thermal Analysis ◽  
Powder Diffraction ◽  
Spin Structure ◽  
Magnetic Measurements ◽  
Mixed Ligand ◽  
Mixed Ligand Complexes ◽  
X Ray ◽  
Square Planar

The synthesis of the following mixed ligand complexes is reported: [Ni(phdtc)2(dpm)2], [Ni(phdtc)2(dpe)2], [Ni(phdtc)2(dpp)3], [Ni(1-naphdtc)2(dpm)2], [Ni(1-naphdtc)2], and [Ni(1-naphdtc)2(dpp)2], where phdtc = PhNHCSS-, 1-naphdtc = 1-NaPhNHCSS-, dpm = Ph2PCH2PPh2, dpe = Ph2P(CH2)2PPh2, and dpp = Ph2P(CH2)3PPh2. The complexes are characterised by microanalysis, IR and UV-Vis spectra, magnetic measurements, conductivity, X-ray powder diffraction, and thermal analysis. All the mixed ligand complexes are diamagnetic, and thus a square-planar or square-pyramidal (low-spin) structure was proposed for the present complexes.

Diphosphinoazine Rhodium(I) and Iridium(I) Complexes

2006 ◽  
Vol 71 (2) ◽  
pp. 197-206 ◽  
Author(s):  
Martin Pošta ◽  
Jan Čermák ◽  
Pavel Vojtíšek ◽  
Ivana Císařová
Keyword(s):  
Rhodium Complexes ◽  
Iridium Complexes ◽  
X Ray ◽  
First Time

The first rhodium complexes of diphosphinoazines [{RhCl(1,2-η:5,6-η-CH=CHCH2CH2CH=CHCH2CH2)}2 {μ-R2PCH2C(But)=NN=C(But)CH2PR2] (R = Ph, Cy, Pri) were prepared by cleavage of the bridge in chloro(cycloocta-1,5-diene)rhodium(I) dimer, the analogous iridium(I) complexes were also prepared for the first time. The X-ray structures of isostructural rhodium and iridium complexes with bis(dicyclohexylphosphino)pinacoloneazine were determined. Diphosphinoazine ligands in the complexes remained in (Z,Z) configuration bridging two RhCl(C8H12) units.

Synthesis and Structure of a Clathrated Two-Dimensional Metal-Organic Framework: [Cd(4,4'-bpy)2(H2O)2](ClO4)2·(L)2·H2O (L = Bis(1-pyrazinylethylidene)hydrazine)

2008 ◽  
Vol 73 (1) ◽  
pp. 24-31
Author(s):  
Dayu Wu ◽  
Genhua Wu ◽  
Wei Huang ◽  
Zhuqing Wang
Keyword(s):  
Metal Organic Framework ◽  
Channel Structure ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Guest Molecules ◽  
X Ray ◽  
Square Planar ◽  
Metal Organic ◽  
Aqueous Meoh ◽  
Organic Framework

The compound [Cd(4,4'-bpy)2(H2O)2](ClO4)2·(L)2 was obtained by the reaction of Cd(ClO4)2, bis(1-pyrazinylethylidene)hydrazine (L) and 4,4'-bipyridine in aqueous MeOH. Single-crystal X-ray diffraction has revealed its two-dimensional metal-organic framework. The 2-D layers superpose on each other, giving a channel structure. The square planar grids consist of two pairs of shared edges with Cd(II) ion and a 4,4'-bipyridine molecule each vertex and side, respectively. The square cavity has a dimension of 11.817 × 11.781 Å. Two guest molecules of bis(1-pyrazinylethylidene)hydrazine are clathrated in every hydrophobic host cavity, being further stabilized by π-π stacking and hydrogen bonding. The results suggest that the hydrazine molecules present in the network serve as structure-directing templates in the formation of crystal structures.

scholarly journals Quartz Crystallite Size and Moganite Content as Indicators of the Mineralogical Maturity of the Carboniferous Chert: The Case of Cherts from Eastern Asturias (Spain)

Minerals ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 611
Author(s):  
Celia Marcos ◽  
María de Uribe-Zorita ◽  
Pedro Álvarez-Lloret ◽  
Alaa Adawy ◽  
Patricia Fernández ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Crystallite Size ◽  
Archaeological Sites ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Infrared And Raman Spectroscopy ◽  
First Time ◽  
Geological Formations

Chert samples from different coastal and inland outcrops in the Eastern Asturias (Spain) were mineralogically investigated for the first time for archaeological purposes. X-ray diffraction, X-ray fluorescence, transmission electron microscopy, infrared and Raman spectroscopy and total organic carbon techniques were used. The low content of moganite, since its detection by X-ray diffraction is practically imperceptible, and the crystallite size (over 1000 Å) of the quartz in these cherts would be indicative of its maturity and could potentially be used for dating chert-tools recovered from archaeological sites. Also, this information can constitute essential data to differentiate the cherts and compare them with those used in archaeological tools. However, neither composition nor crystallite size would allow distinguishing between coastal and inland chert outcrops belonging to the same geological formations.

scholarly journals First Report on the Geologic Occurrence of Natural Na–A Zeolite and Associated Minerals in Cretaceous Mudstones of the Paja Formation of Vélez (Santander), Colombia

Crystals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 218
Author(s):  
Carlos Alberto Ríos-Reyes ◽  
German Alfonso Reyes-Mendoza ◽  
José Antonio Henao-Martínez ◽  
Craig Williams ◽  
Alan Dyer
Keyword(s):  
Natural Zeolite ◽  
Scanning Electron Micrographs ◽  
Total Sulfur ◽  
Zeolite A ◽  
X Ray Diffraction ◽  
X Ray ◽  
Mineral Phases ◽  
The World ◽  
Porosity And Permeability ◽  
First Time

This study reports for the first time the geologic occurrence of natural zeolite A and associated minerals in mudstones from the Cretaceous Paja Formation in the urban area of the municipality of Vélez (Santander), Colombia. These rocks are mainly composed of quartz, muscovite, pyrophyllite, kaolinite and chlorite group minerals, framboidal and cubic pyrite, as well as marcasite, with minor feldspar, sulphates, and phosphates. Total organic carbon (TOC), total sulfur (TS), and millimeter fragments of algae are high, whereas few centimeters and not biodiverse small ammonite fossils, and other allochemical components are subordinated. Na–A zeolite and associated mineral phases as sodalite occur just beside the interparticle micropores (honeycomb from framboidal, cube molds, and amorphous cavities). It is facilitated by petrophysical properties alterations, due to processes of high diagenesis, temperatures up to 80–100 °C, with weathering contributions, which increase the porosity and permeability, as well as the transmissivity (fluid flow), allowing the geochemistry remobilization and/or recrystallization of pre-existing silica, muscovite, kaolinite minerals group, salts, carbonates, oxides and peroxides. X-ray diffraction analyses reveal the mineral composition of the mudstones and scanning electron micrographs show the typical cubic morphology of Na–A zeolite of approximately 0.45 mμ in particle size. Our data show that the sequence of the transformation of phases is: Poorly crystalline aluminosilicate → sodalite → Na–A zeolite. A literature review shows that this is an unusual example of the occurrence of natural zeolites in sedimentary marine rocks recognized around the world.

scholarly journals The Effect of Surfactant-Modified Montmorillonite on the Cross-Linking Efficiency of Polysiloxanes

Materials ◽  
2021 ◽  
Vol 14 (10) ◽  
pp. 2623
Author(s):  
Monika Wójcik-Bania ◽  
Jakub Matusik
Keyword(s):  
Total Pore Volume ◽  
Cross Linking ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
The Cross ◽  
Chain Lengths ◽  
First Time ◽  
Substituent Influence ◽  
Benzyl Substituent

Polymer–clay mineral composites are an important class of materials with various applications in the industry. Despite interesting properties of polysiloxanes, such matrices were rarely used in combination with clay minerals. Thus, for the first time, a systematic study was designed to investigate the cross-linking efficiency of polysiloxane networks in the presence of 2 wt % of organo-montmorillonite. Montmorillonite (Mt) was intercalated with six quaternary ammonium salts of the cation structure [(CH3)2R’NR]+, where R = C12, C14, C16, and R’ = methyl or benzyl substituent. The intercalation efficiency was examined by X-ray diffraction, CHN elemental analysis, and Fourier transform infrared (FTIR) spectroscopy. Textural studies have shown that the application of freezing in liquid nitrogen and freeze-drying after the intercalation increases the specific surface area and the total pore volume of organo-Mt. The polymer matrix was a poly(methylhydrosiloxane) cross-linked with two linear vinylsiloxanes of different siloxane chain lengths between end functional groups. X-ray diffraction and transmission electron microscopy studies have shown that the increase in d-spacing of organo-Mt and the benzyl substituent influence the degree of nanofillers’ exfoliation in the nanocomposites. The increase in the degree of organo-Mt exfoliation reduces the efficiency of hydrosilylation reaction monitored by FTIR. This was due to physical hindrance induced by exfoliated Mt particles.

scholarly journals Homopiperazine (Hexahydro-1,4-diazepine)

Molbank ◽  
10.3390/m1200 ◽  
2021 ◽  
Vol 2021 (2) ◽  
pp. M1200
Author(s):  
R. Alan Aitken ◽  
Dheirya K. Sonecha ◽  
Alexandra M. Z. Slawin
Keyword(s):  
13C Nmr ◽  
Title Compound ◽  
Coupling Constants ◽  
15N Nmr ◽  
Time Data ◽  
Nmr Spectrum ◽  
X Ray ◽  
First Time

The X-ray structure of the title compound has been determined for the first time. Data on its 1H–13C-NMR coupling constants and 15N-NMR spectrum are also given.

scholarly journals A novel and potentially scalable CVD-based route towards SnO2:Mo thin films as transparent conducting oxides

2021 ◽  
Author(s):  
Tianlei Ma ◽  
Marek Nikiel ◽  
Andrew G. Thomas ◽  
Mohamed Missous ◽  
David J. Lewis
Keyword(s):  
Thin Films ◽  
Photoelectron Spectroscopy ◽  
Mixed Valence ◽  
Chemical Vapour ◽  
X Ray Diffraction ◽  
X Ray ◽  
Conducting Oxides ◽  
Valence States ◽  
3 Omega ◽  
First Time

AbstractIn this report, we prepared transparent and conducting undoped and molybdenum-doped tin oxide (Mo–SnO2) thin films by aerosol-assisted chemical vapour deposition (AACVD). The relationship between the precursor concentration in the feed and in the resulting films was studied by energy-dispersive X-ray spectroscopy, suggesting that the efficiency of doping is quantitative and that this method could potentially impart exquisite control over dopant levels. All SnO2 films were in tetragonal structure as confirmed by powder X-ray diffraction measurements. X-ray photoelectron spectroscopy characterisation indicated for the first time that Mo ions were in mixed valence states of Mo(VI) and Mo(V) on the surface. Incorporation of Mo6+ resulted in the lowest resistivity of $$7.3 \times 10^{{ - 3}} \Omega \,{\text{cm}}$$ 7.3 × 10 - 3 Ω cm , compared to pure SnO2 films with resistivities of $$4.3\left( 0 \right) \times 10^{{ - 2}} \Omega \,{\text{cm}}$$ 4.3 0 × 10 - 2 Ω cm . Meanwhile, a high transmittance of 83% in the visible light range was also acquired. This work presents a comprehensive investigation into impact of Mo doping on SnO2 films synthesised by AACVD for the first time and establishes the potential for scalable deposition of SnO2:Mo thin films in TCO manufacturing. Graphical abstract

scholarly journals Reactive Dual Magnetron Sputtering: A Fast Method for Preparing Stoichiometric Microcrystalline ZnWO4 Thin Films

Surfaces ◽  
2021 ◽  
Vol 4 (2) ◽  
pp. 106-114
Author(s):  
Yannick Hermans ◽  
Faraz Mehmood ◽  
Kerstin Lakus-Wollny ◽  
Jan P. Hofmann ◽  
Thomas Mayer ◽  
...  
Keyword(s):  
Thin Films ◽  
Magnetron Sputtering ◽  
Photoelectron Spectroscopy ◽  
Fast Method ◽  
X Ray Diffraction ◽  
X Ray ◽  
Glass Substrates ◽  
Post Annealing ◽  
Rf Signal ◽  
First Time

Thin films of ZnWO4, a promising photocatalytic and scintillator material, were deposited for the first time using a reactive dual magnetron sputtering procedure. A ZnO target was operated using an RF signal, and a W target was operated using a DC signal. The power on the ZnO target was changed so that it would match the sputtering rate of the W target operated at 25 W. The effects of the process parameters were characterized using optical spectroscopy, X-ray diffraction, and scanning electron microscopy, including energy dispersive X-ray spectroscopy as well as X-ray photoelectron spectroscopy. It was found that stoichiometric microcrystalline ZnWO4 thin films could be obtained, by operating the ZnO target during the sputtering procedure at a power of 55 W and by post-annealing the resulting thin films for at least 10 h at 600 °C. As FTO coated glass substrates were used, annealing led as well to the incorporation of Na, resulting in n+ doped ZnWO4 thin films.

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