AN INFRARED STUDY OF TRIMETHYLAMINE OXIDE, ITS HYDRATE, AND ITS HYDROCHLORIDE

1961 ◽  
Vol 39 (6) ◽  
pp. 1214-1220 ◽  
Author(s):  
Paul A. Giguère ◽  
David Chin
Keyword(s):  
Solid State ◽  
Electron Diffraction ◽  
Hydrogen Bonds ◽  
Infrared Spectra ◽  
Diffraction Data ◽  
Electron Diffraction Data ◽  
Infrared Study ◽  
X Ray ◽  
Trimethylamine Oxide ◽  
Molecular Compounds

The infrared spectra of trimethylamine oxide, its hydrate, and its hydrochloride in the solid state were measured over the range 300 to 3500 cm−1 to ascertain the nature of the bonds in these compounds. From the observed stretching frequencies, 937 cm−1 for N—O and 945 cm−1 for C—N, the corresponding bond lengths are calculated to be 1.44 and 1.50 Å in agreement with X-ray and electron diffraction data. Both these frequencies remain unchanged in the hydrate and the hydrochloride as could be expected for molecular compounds. However, in the hydrochloride most of the evidence points to an ionic constitution. In both the hydrate and the hydrochloride the hydrogen bonds are particularly strong presumably because of the formal charges.

A thermal and X-ray investigation of scarbroite

1960 ◽  
Vol 32 (248) ◽  
pp. 353-362 ◽  
Author(s):  
W. J. Duffin ◽  
J. Goodyear
Keyword(s):  
Electron Diffraction ◽  
Chemical Analysis ◽  
Diffraction Data ◽  
Room Temperature ◽  
Layer Structure ◽  
Electron Diffraction Data ◽  
X Ray ◽  
Fine Grained ◽  
The North

SummaryScarbroite, a fine-grained but compact deposit obtained from fissures in the sandstone on the north Yorkshire coast, is shown by chemical analysis to have an idealized formula Al2(CO3)3·12Al(OH)3. X-ray and electron diffraction data indicate a triclinic cell with a 9·94 Å., b 14·88 Å., c 26·47 Å., α 98·7°, β 96·5°, and γ 89·0°. A layer structure consisting of gibbsite-type sheets of Al(OH)3 and sheets of Al2(CO3)3 is proposed. The structure is stable from room temperature to about 125° C.

A complex pseudo-decagonal quasicrystal approximant, Al37(Co,Ni)15.5, solved by rotation electron diffraction

2014 ◽  
Vol 47 (1) ◽  
pp. 215-221 ◽  
Author(s):  
Devinder Singh ◽  
Yifeng Yun ◽  
Wei Wan ◽  
Benjamin Grushko ◽  
Xiaodong Zou ◽  
...  
Keyword(s):  
Electron Diffraction ◽  
Single Crystal ◽  
Diffraction Data ◽  
Three Dimensional ◽  
Basic Structure ◽  
Electron Diffraction Data ◽  
Dimensional Electron ◽  
X Ray Diffraction ◽  
X Ray ◽  
Diffraction Patterns

Electron diffraction is a complementary technique to single-crystal X-ray diffraction and powder X-ray diffraction for structure solution of unknown crystals. Crystals too small to be studied by single-crystal X-ray diffraction or too complex to be solved by powder X-ray diffraction can be studied by electron diffraction. The main drawbacks of electron diffraction have been the difficulties in collecting complete three-dimensional electron diffraction data by conventional electron diffraction methods and the very time-consuming data collection. In addition, the intensities of electron diffraction suffer from dynamical scattering. Recently, a new electron diffraction method, rotation electron diffraction (RED), was developed, which can overcome the drawbacks and reduce dynamical effects. A complete three-dimensional electron diffraction data set can be collected from a sub-micrometre-sized single crystal in less than 2 h. Here the RED method is applied forab initiostructure determination of an unknown complex intermetallic phase, the pseudo-decagonal (PD) quasicrystal approximant Al37.0(Co,Ni)15.5, denoted as PD2. RED shows that the crystal is F-centered, witha= 46.4,b= 64.6,c= 8.2 Å. However, as with other approximants in the PD series, the reflections with oddlindices are much weaker than those withleven, so it was decided to first solve the PD2 structure in the smaller, primitive unit cell. The basic structure of PD2 with unit-cell parametersa= 23.2,b= 32.3,c= 4.1 Å and space groupPnmmhas been solved in the present study. The structure withc= 8.2 Å will be taken up in the near future. The basic structure contains 55 unique atoms (17 Co/Ni and 38 Al) and is one of the most complex structures solved by electron diffraction. PD2 is built of characteristic 2 nm wheel clusters with fivefold rotational symmetry, which agrees with results from high-resolution electron microscopy images. Simulated electron diffraction patterns for the structure model are in good agreement with the experimental electron diffraction patterns obtained by RED.

A Search/Match Procedure for Electron Diffraction Data Based on Pattern Matching in Binary Bit Maps

1986 ◽  
Vol 1 (3) ◽  
pp. 226-234 ◽  
Author(s):  
Martin J. Carr ◽  
William F. Chambers ◽  
David Melgaard
Keyword(s):  
Electron Diffraction ◽  
Diffraction Analysis ◽  
Pattern Matching ◽  
Diffraction Data ◽  
Reference Data ◽  
Search Algorithm ◽  
Energy Dispersive ◽  
Electron Diffraction Data ◽  
Electron Diffraction Analysis ◽  
X Ray

AbstractA unique file structure and search algorithm have been developed for the purpose of obtaining matches between experimental electron diffraction and qualitative energy dispersive X-ray compositional data from an unknown crystalline phase and the reference data in the JCPDS Powder Diffraction File. The reference data for over 32,000 inorganic compounds from sets 1–33 were compressed and stored in binary format as bit pattern maps. The entire data set and searching programs require less than 4 Mbyte and retain the precision appropriate for electron diffraction analysis. The search algorithm, written in both RT-11 FORTRAN and Flextran, is based on pattern matching between bit maps obtained for the unknown and reference compounds for both composition and diffraction data. Special attention is given to double diffraction effects commonly encountered in electron diffraction analysis. The programs run on an interactive basis on a microcomputer dedicated to the X-ray energy dispersive spectrometer on an analytical electron microscope. A typical search takes about 15 seconds to run and extracts about 10–15 different compounds.

Nano-scale microstructure of Fe3+-, OH−-bearing crystalline inclusions in experimentally oxidized olivine from a mantle nodule

2000 ◽  
Vol 64 (2) ◽  
pp. 319-335 ◽  
Author(s):  
N. R. Khisina ◽  
K. Langer ◽  
M. Andrut ◽  
A. V. Ukhanov ◽  
R. Wirth
Keyword(s):  
Solid State ◽  
Electron Diffraction ◽  
Diffraction Data ◽  
Uv Spectroscopy ◽  
Electron Diffraction Data ◽  
State Transformation ◽  
Solid State Transformation ◽  
Crystalline Inclusions ◽  
Precursor Phase ◽  
Ir And Uv Spectroscopy

AbstractAn olivine grain from peridotite nodule 9206 (Udachnaya kimberlite) was heated in air at 700°C for 9 h. It was investigated by EMPA, by IR and UV spectroscopy and by TEM. The TEM examination reveals hexagon-like inclusions up to several hundred nm in size with a core and rim structure. The AEM data show that the inclusions contain only Mg, Fe and Si as cations. The rims have almost the same composition as the olivine matrix whereas the cores are enriched in iron and depleted in Mg. Electron diffraction data, SAED and CBED, indicate that the rims are composed of a ‘secondary’ olivine while the cores are composed of coexisting feroxyhite FeOOH, bernalite Fe(OH)3 and β-cristobalite SiO2. The presence of nm-sized inclusions in minerals is expected to influence the interpretation of spectroscopic results if spectroscopy is carried out without knowledge of the microstructure.It is speculated that the complex microstructure of the inclusions is a result of a solid state transformation of a precursor phase, probably a hydrous magnesian silicate, during the experimental heating and oxidation.

scholarly journals A Medipix quantum area detector allows rotation electron diffraction data collection from submicrometre three-dimensional protein crystals

2013 ◽  
Vol 69 (7) ◽  
pp. 1223-1230 ◽  
Author(s):  
Igor Nederlof ◽  
Eric van Genderen ◽  
Yao-Wang Li ◽  
Jan Pieter Abrahams
Keyword(s):  
Electron Diffraction ◽  
Data Collection ◽  
Diffraction Data ◽  
Three Dimensional ◽  
Protein Crystal ◽  
Protein Crystals ◽  
Electron Diffraction Data ◽  
Single Shot ◽  
X Ray ◽  
Area Detector

When protein crystals are submicrometre-sized, X-ray radiation damage precludes conventional diffraction data collection. For crystals that are of the order of 100 nm in size, at best only single-shot diffraction patterns can be collected and rotation data collection has not been possible, irrespective of the diffraction technique used. Here, it is shown that at a very low electron dose (at most 0.1 e− Å−2), a Medipix2 quantum area detector is sufficiently sensitive to allow the collection of a 30-frame rotation series of 200 keV electron-diffraction data from a single ∼100 nm thick protein crystal. A highly parallel 200 keV electron beam (λ = 0.025 Å) allowed observation of the curvature of the Ewald sphere at low resolution, indicating a combined mosaic spread/beam divergence of at most 0.4°. This result shows that volumes of crystal with low mosaicity can be pinpointed in electron diffraction. It is also shown that strategies and data-analysis software (MOSFLMandSCALA) from X-ray protein crystallography can be used in principle for analysing electron-diffraction data from three-dimensional nanocrystals of proteins.

On the quality of the continuous rotation electron diffraction data for accurate atomic structure determination of inorganic compounds

2018 ◽  
Vol 51 (4) ◽  
pp. 1094-1101 ◽  
Author(s):  
Yunchen Wang ◽  
Taimin Yang ◽  
Hongyi Xu ◽  
Xiaodong Zou ◽  
Wei Wan
Keyword(s):  
Electron Diffraction ◽  
Single Crystal ◽  
Diffraction Data ◽  
Structural Models ◽  
Electron Diffraction Data ◽  
Data Sets ◽  
X Ray Diffraction ◽  
X Ray ◽  
Continuous Rotation

The continuous rotation electron diffraction (cRED) method has the capability of providing fast three-dimensional electron diffraction data collection on existing and future transmission electron microscopes; unknown structures could be potentially solved and refined using cRED data collected from nano- and submicrometre-sized crystals. However, structure refinements of cRED data using SHELXL often lead to relatively high R1 values when compared with those refined against single-crystal X-ray diffraction data. It is therefore necessary to analyse the quality of the structural models refined against cRED data. In this work, multiple cRED data sets collected from different crystals of an oxofluoride (FeSeO3F) and a zeolite (ZSM-5) with known structures are used to assess the data consistency and quality and, more importantly, the accuracy of the structural models refined against these data sets. An evaluation of the precision and consistency of the cRED data by examination of the statistics obtained from the data processing software DIALS is presented. It is shown that, despite the high R1 values caused by dynamical scattering and other factors, the refined atomic positions obtained from the cRED data collected for different crystals are consistent with those of the reference models refined against single-crystal X-ray diffraction data. The results serve as a reference for the quality of the cRED data and the achievable accuracy of the structural parameters.

Non-planar structures of Et3N and Pri3N: a contradiction between the X-ray, and NMR and electron diffraction data for Pri3N

1998 ◽  
pp. 781-782 ◽  
Author(s):  
Roland Boese ◽  
Dieter Bläser ◽  
Mikhail Y. Antipin ◽  
Roland Boese ◽  
Mikhail Y. Antipin ◽  
...  
Keyword(s):  
Electron Diffraction ◽  
Diffraction Data ◽  
Electron Diffraction Data ◽  
X Ray ◽  
Planar Structures
Sign in / Sign up

Export Citation Format

Share Document