scholarly journals Characterization of a Reactive Rh2 Nitrenoid by Crystalline Matrix Isolation

2019 ◽  
Author(s):  
Anuvab Das ◽  
Yu-Sheng Chen ◽  
Joseph Reibenspies ◽  
David Powers
Keyword(s):  
Transient Species ◽  
Reactive Metal ◽  
Data Set ◽  
High Resolution Data ◽  
X Ray ◽  
Organic Azide ◽  
Crystal Matrix ◽  
Azide Ligand ◽  
Crystalline Matrix

Here we report the first X-ray crystal structure of a reactive Rh<sub>2</sub> nitrenoid, enabled by N<sub>2</sub> elimination from an organic azide ligand within a single-crystal matrix. The resulting high-resolution data set demonstrates a long Rh–N bond, consistent with a triplet electronic structure. The demonstration of facile access to reactive metal nitrenoids within a crystalline matrix provides a platform for structural characterization of the elusive transient species at the heart of C–H functionalization.

scholarly journals Characterization of a Reactive Rh2 Nitrenoid by Crystalline Matrix Isolation

2019 ◽  
Author(s):  
Anuvab Das ◽  
Yu-Sheng Chen ◽  
Joseph Reibenspies ◽  
David Powers
Keyword(s):  
Transient Species ◽  
Reactive Metal ◽  
Data Set ◽  
High Resolution Data ◽  
X Ray ◽  
Organic Azide ◽  
Crystal Matrix ◽  
Azide Ligand ◽  
Crystalline Matrix

Here we report the first X-ray crystal structure of a reactive Rh<sub>2</sub> nitrenoid, enabled by N<sub>2</sub> elimination from an organic azide ligand within a single-crystal matrix. The resulting high-resolution data set demonstrates a long Rh–N bond, consistent with a triplet electronic structure. The demonstration of facile access to reactive metal nitrenoids within a crystalline matrix provides a platform for structural characterization of the elusive transient species at the heart of C–H functionalization.

Difference Fourier Analysis of Glucose Embedded and Frozen Hydrated Purple Membrane

1982 ◽  
Vol 40 ◽  
pp. 74-75
Author(s):  
Jules S. Jaffe ◽  
Robert M. Glaeser
Keyword(s):  
Purple Membrane ◽  
Data Set ◽  
High Resolution Data ◽  
X Ray ◽  
X Ray Crystallography ◽  
Fourier Techniques ◽  
Versus Protein ◽  
The Difference ◽  
Difference Fourier ◽  
Ideal Method

Although difference Fourier techniques are standard in X-ray crystallography it has only been very recently that electron crystallographers have been able to take advantage of this method. We have combined a high resolution data set for frozen glucose embedded Purple Membrane (PM) with a data set collected from PM prepared in the frozen hydrated state in order to visualize any differences in structure due to the different methods of preparation. The increased contrast between protein-ice versus protein-glucose may prove to be an advantage of the frozen hydrated technique for visualizing those parts of bacteriorhodopsin that are embedded in glucose. In addition, surface groups of the protein may be disordered in glucose and ordered in the frozen state. The sensitivity of the difference Fourier technique to small changes in structure provides an ideal method for testing this hypothesis.

scholarly journals BINoculars: data reduction and analysis software for two-dimensional detectors in surface X-ray diffraction

2015 ◽  
Vol 48 (4) ◽  
pp. 1324-1329 ◽  
Author(s):  
Sander Roobol ◽  
Willem Onderwaater ◽  
Jakub Drnec ◽  
Roberto Felici ◽  
Joost Frenken
Keyword(s):  
Data Reduction ◽  
Modular Design ◽  
Reciprocal Lattice ◽  
Measurement Techniques ◽  
Three Dimensional ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Data Set ◽  
High Resolution Data ◽  
X Ray

BINocularsis a tool for data reduction and analysis of large sets of surface diffraction data that have been acquired with a two-dimensional X-ray detector. The intensity of each pixel of a two-dimensional detector is projected onto a three-dimensional grid in reciprocal-lattice coordinates using a binning algorithm. This allows for fast acquisition and processing of high-resolution data sets and results in a significant reduction of the size of the data set. The subsequent analysis then proceeds in reciprocal space. It has evolved from the specific needs of the ID03 beamline at the ESRF, but it has a modular design and can be easily adjusted and extended to work with data from other beamlines or from other measurement techniques. This paper covers the design and the underlying methods employed in this software package and explains howBINocularscan be used to improve the workflow of surface X-ray diffraction measurements and analysis.

scholarly journals Electrodeposition and Characterization of Lanthanide Elements on Carbon Sheets

Coatings ◽  
2021 ◽  
Vol 11 (1) ◽  
pp. 100
Author(s):  
Min Hee Joo ◽  
So Jeong Park ◽  
Sung-Min Hong ◽  
Choong Kyun Rhee ◽  
Dongsoo Kim ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Full Data ◽  
Data Set ◽  
X Ray ◽  
Thin Film Fabrication ◽  
Lanthanide Elements ◽  
Fundamental Information ◽  
Electrochemical Coating ◽  
Carbon Sheet

Electrochemical coating and recovery by electrodeposition have been invaluably employed for facial thin film fabrication and the recycling of used materials. Herein, we have established a full data set of lanthanide (Ln: La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, and Yb) elements electrodeposited on carbon sheets. Cyclic voltammetry was performed for 10 mM Ln(III) ions in a 0.1 M NaClO4 electrolyte over a carbon sheet between +0.5 V and −1.7 V (vs. Ag/AgCl). Amperometry was performed at a given potential to electrodeposit the Ln element on the carbon sheet. Their physicochemical properties were fully investigated by scanning electron microscopy, Fourier-transform infrared spectroscopy, energy-dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy. The newly established full data set for Ln(III) ions over carbon electrodes provides useful fundamental information for the development of coating and recovery methods of Ln elements.

The Use of Advanced Analytical Techniques for Characterization of the Chemical, Physical, and Crystallographic Nature of a Surface

1973 ◽  
Vol 31 ◽  
pp. 132-133 ◽  
Author(s):  
R. E. Herfert
Keyword(s):  
Surface Characterization ◽  
Analytical Techniques ◽  
X Ray Diffraction ◽  
Depth Of Penetration ◽  
X Ray ◽  
The Past ◽  
Transmission Electron ◽  
Scanning Electron

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.

High Resolution Replication of Organoclay Surfaces

1982 ◽  
Vol 40 ◽  
pp. 576-577
Author(s):  
W. W. Barker ◽  
W. E. Rigsby ◽  
V. J. Hurst ◽  
W. J. Humphreys
Keyword(s):  
Clay Mineral ◽  
Organic Molecule ◽  
Organic Molecules ◽  
X Ray Diffraction ◽  
Xrd Pattern ◽  
X Ray ◽  
Naturally Occurring ◽  
Silicate Layers ◽  
Mineral Identification

Experimental clay mineral-organic molecule complexes long have been known and some of them have been extensively studied by X-ray diffraction methods. The organic molecules are adsorbed onto the surfaces of the clay minerals, or intercalated between the silicate layers. Natural organo-clays also are widely recognized but generally have not been well characterized. Widely used techniques for clay mineral identification involve treatment of the sample with H2 O2 or other oxidant to destroy any associated organics. This generally simplifies and intensifies the XRD pattern of the clay residue, but helps little with the characterization of the original organoclay. Adequate techniques for the direct observation of synthetic and naturally occurring organoclays are yet to be developed.

Digital x-ray mapping of nanometer-size supported bimetallic catalysts

1988 ◽  
Vol 46 ◽  
pp. 530-531
Author(s):  
L. T. Germinario
Keyword(s):  
Background Radiation ◽  
Metal Cluster ◽  
Single Element ◽  
Beam Diameter ◽  
X Rays ◽  
X Ray ◽  
Major Interest ◽  
Induced Changes

Understanding the role of metal cluster composition in determining catalytic selectivity and activity is of major interest in heterogeneous catalysis. The electron microscope is well established as a powerful tool for ultrastructural and compositional characterization of support and catalyst. Because the spatial resolution of x-ray microanalysis is defined by the smallest beam diameter into which the required number of electrons can be focused, the dedicated STEM with FEG is the instrument of choice. The main sources of errors in energy dispersive x-ray analysis (EDS) are: (1) beam-induced changes in specimen composition, (2) specimen drift, (3) instrumental factors which produce background radiation, and (4) basic statistical limitations which result in the detection of a finite number of x-ray photons. Digital beam techniques have been described for supported single-element metal clusters with spatial resolutions of about 10 nm. However, the detection of spurious characteristic x-rays away from catalyst particles produced images requiring several image processing steps.

Plant Pathology Diagnosed by X-Ray Microanalysis

1987 ◽  
Vol 45 ◽  
pp. 974-975
Author(s):  
J. H. Resau ◽  
N. Howell ◽  
S. H. Chang
Keyword(s):  
Electron Microscopy ◽  
Plant Pathology ◽  
Biochemical Characterization ◽  
Nutrient Deficiency ◽  
Green Leaf ◽  
Parasitic Infestation ◽  
X Ray

Spinach grown in Texas developed “yellow spotting” on the peripheral portions of the leaves. The exact cause of the discoloration could not be determined as there was no evidence of viral or parasitic infestation of the plants and biochemical characterization of the plants did not indicate any significant differences between the yellow and green leaf portions of the spinach. The present study was undertaken using electron microscopy (EM) to determine if a micro-nutrient deficiency was the cause for the discoloration.Green leaf spinach was collected from the field and sent by express mail to the EM laboratory. The yellow and equivalent green portions of the leaves were isolated and dried in a Denton evaporator at 10-5 Torr for 24 hrs. The leaf specimens were then examined using a JEOL 100 CX analytical microscope. TEM specimens were prepared according to the methods of Trump et al.

EXELFS Studies of Carbon Fibers

1990 ◽  
Vol 48 (2) ◽  
pp. 72-73
Author(s):  
V. Serin ◽  
K. Hssein ◽  
G. Zanchi ◽  
J. Sévely
Keyword(s):  
Carbon Fibers ◽  
Energy Analysis ◽  
Electron Excitation ◽  
Complex Structures ◽  
High Modulus ◽  
Promising Technique ◽  
X Ray ◽  
Fine Structures ◽  
X Ray Absorption

The present developments of electron energy analysis in the microscopes by E.E.L.S. allow an accurate recording of the spectra and of their different complex structures associated with the inner shell electron excitation by the incident electrons (1). Among these structures, the Extended Energy Loss Fine Structures (EXELFS) are of particular interest. They are equivalent to the well known EXAFS oscillations in X-ray absorption spectroscopy. Due to the EELS characteristic, the Fourier analysis of EXELFS oscillations appears as a promising technique for the characterization of composite materials, the major constituents of which are low Z elements. Using EXELFS, we have developed a microstructural study of carbon fibers. This analysis concerns the carbon K edge, which appears in the spectra at 285 eV. The purpose of the paper is to compare the local short range order, determined by this way in the case of Courtauld HTS and P100 ex-polyacrylonitrile carbon fibers, which are high tensile strength (HTS) and high modulus (HM) fibers respectively.

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