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Title: Expanding Lorentz and spectrum corrections to large volumes of reciprocal space for single-crystal time-of-flight neutron diffraction. Corrigendum

Abstract

The author list is amended with the addition of Michal Chodkiewicz, Thomas Weber and Hans-Beat Bürgi. Here, the complete list of authors is Tara Michels-Clark, Andrei Savici, Vickie Lynch, Xiaoping Wang, Michal Chodkiewicz, Thomas Weber, Hans-Beat Bürgi and Christina Hoffmann.

Authors:
 [1]; ORCiD logo [2]; ORCiD logo [2]; ORCiD logo [2];  [3];  [4];  [5]; ORCiD logo [2]
  1. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
  2. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
  3. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Warsaw Univ., Warsaw (Poland)
  4. ETH Zurich, Zurich (Switzerland)
  5. ETH Zurich, Zurich (Switzerland); Univ. Bern Freiestrasse, Bern (Switzerland)
Publication Date:
Research Org.:
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1410916
Grant/Contract Number:
AC05-00OR22725
Resource Type:
Journal Article: Accepted Manuscript
Journal Name:
Journal of Applied Crystallography (Online)
Additional Journal Information:
Journal Name: Journal of Applied Crystallography (Online); Journal Volume: 50; Journal Issue: 5; Journal ID: ISSN 1600-5767
Publisher:
International Union of Crystallography
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; modulated diffuse scattering; local structure modeling; Lorentz and spectrum corrections; single-crystal time-of-flight neutron diffraction

Citation Formats

Michels-Clark, Tara M., Savici, Andrei T., Lynch, Vickie E., Wang, Xiaoping, Chodkiewicz, Michal, Weber, Thomas, Bürgi, Hans -Beat, and Hoffmann, Christina M. Expanding Lorentz and spectrum corrections to large volumes of reciprocal space for single-crystal time-of-flight neutron diffraction. Corrigendum. United States: N. p., 2017. Web. doi:10.1107/S1600576717006781.
Michels-Clark, Tara M., Savici, Andrei T., Lynch, Vickie E., Wang, Xiaoping, Chodkiewicz, Michal, Weber, Thomas, Bürgi, Hans -Beat, & Hoffmann, Christina M. Expanding Lorentz and spectrum corrections to large volumes of reciprocal space for single-crystal time-of-flight neutron diffraction. Corrigendum. United States. doi:10.1107/S1600576717006781.
Michels-Clark, Tara M., Savici, Andrei T., Lynch, Vickie E., Wang, Xiaoping, Chodkiewicz, Michal, Weber, Thomas, Bürgi, Hans -Beat, and Hoffmann, Christina M. 2017. "Expanding Lorentz and spectrum corrections to large volumes of reciprocal space for single-crystal time-of-flight neutron diffraction. Corrigendum". United States. doi:10.1107/S1600576717006781. https://www.osti.gov/servlets/purl/1410916.
@article{osti_1410916,
title = {Expanding Lorentz and spectrum corrections to large volumes of reciprocal space for single-crystal time-of-flight neutron diffraction. Corrigendum},
author = {Michels-Clark, Tara M. and Savici, Andrei T. and Lynch, Vickie E. and Wang, Xiaoping and Chodkiewicz, Michal and Weber, Thomas and Bürgi, Hans -Beat and Hoffmann, Christina M.},
abstractNote = {The author list is amended with the addition of Michal Chodkiewicz, Thomas Weber and Hans-Beat Bürgi. Here, the complete list of authors is Tara Michels-Clark, Andrei Savici, Vickie Lynch, Xiaoping Wang, Michal Chodkiewicz, Thomas Weber, Hans-Beat Bürgi and Christina Hoffmann.},
doi = {10.1107/S1600576717006781},
journal = {Journal of Applied Crystallography (Online)},
number = 5,
volume = 50,
place = {United States},
year = 2017,
month = 9
}

Journal Article:
Free Publicly Available Full Text
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  • Evidence is mounting that potentially exploitable properties of technologically and chemically interesting crystalline materials are often attributable to local structure effects, which can be observed as modulated diffuse scattering (mDS) next to Bragg diffraction (BD). BD forms a regular sparse grid of intense discrete points in reciprocal space. Traditionally, the intensity of each Bragg peak is extracted by integration of each individual reflection first, followed by application of the required corrections. In contrast, mDS is weak and covers expansive volumes of reciprocal space close to, or between, Bragg reflections. For a representative measurement of the diffuse scattering, multiple sample orientationsmore » are generally required, where many points in reciprocal space are measured multiple times and the resulting data are combined. The common post-integration data reduction method is not optimal with regard to counting statistics. A general and inclusive data processing method is needed. In this contribution, a comprehensive data analysis approach is introduced to correct and merge the full volume of scattering data in a single step, while correctly accounting for the statistical weight of the individual measurements. Lastly, development of this new approach required the exploration of a data treatment and correction protocol that includes the entire collected reciprocal space volume, using neutron time-of-flight or wavelength-resolved data collected at TOPAZ at the Spallation Neutron Source at Oak Ridge National Laboratory.« less
  • The intensity of single crystal Bragg peaks obtained by mapping neutron time-of-flight event data into reciprocal space and integrating in various ways are compared. These include spherical integration with a fixed radius, ellipsoid fitting and integrating of the peak intensity and one-dimensional peak profile fitting. In comparison to intensities obtained by integrating in real detector histogram space, the data integrated in reciprocal space results in better agreement factors and more accurate atomic parameters. Furthermore, structure refinement using integrated intensities from one-dimensional profile fitting is demonstrated to be more accurate than simple peak-minus-background integration.
  • A single-crystal time-of-flight neutron diffraction structure of hydrogen cis-diacetyltetracarbonylrhenate, (cis-(OH)/sub 4/Re(CH/sub 3/CO)/sub 2/)H, is reported. This is one of the first successful structure determinations reported by using this technique. The diffraction data were collected at the Argonne Intense Pulsed Neutron Source with the unique time-of-flight single-crystal diffractometer. Complete experimental details are provided. The positions of all hydrogen atoms are determined, and the enolic hydrogen atom is shown to participate in an intramolecular O...H...O hydrogen bond. Although large thermal motion of the enolic hydrogen atom prevents a precise definition of the symmetry of this hydrogen bond, most of the results aremore » consistent with an asymmetric O...H...O bond and a localized ..pi..-electron system within the rhena chelate ring.« less
  • This paper describes a single crystal diffractometer (SCD) which uses a position-sensitive area detector for collecting time-of-flight (TOF) neutron diffraction data at Argonne's Intense Pulsed Neutron Source (IPNS). The analysis of data obtained during operation of the prototype ZING-P' pulsed neutron source is also presented.
  • The crystal and molecular structure of the unusual complex Tl/sub 4/(Pt(CN)/sub 4/)CO/sub 3/, obtained by mixing Tl/sub 2/(Pt(CN)/sub 4/) and Tl/sub 2/CO/sub 3/ in aqueous solution at 95/sup 0/C, was determined by both single-crystal and time-of-flight powder neutron diffraction. The complex is not a partially oxidized tetracyanoplatinate (POTCP) salt and contains Pt in an integral (2.0) oxidation state. The lustrous metallic green complex crystallizes in the tetragonal space group, with unit cell constants a = b = 9.911 (4) A (9.908 (3) A, powder study), c = 6.490 (3) A (6.487 (2) A), and V/sub c/ = 637.5 A/sup 3/more » at 298/sup 0/K. In the single-crystal study diffracted intensities of 267 independent reflections were measured to a (sin theta)/lambda limit of 0.438 A/sup -1/, and of these 202 had F/sub 0//sup 2/ > sigma(F/sub 0//sup 2/). Full-matrix least-squares refinement of all structural parameters resulted in a final R(F/sub 0//sup 2/) = 0.075 (all data) and R(F/sub 0//sup 2/) = 0.068. It is important to note that the structural parameters derived with use of the time-of-flight neutron diffraction and single-crystal methods are, in this case, virtually identical. The most pertinent structural feature in Tl/sub 4/(Pt(CN)/sub 4/)CO/sub 3/ is that the Pt atoms form perfectly linear chains with Pt-Pt separations crystallographically constrained to a value of (c/2) = 3.245 (3) A. The intrachain Pt-Pt separation is much longer than in the partially oxidized salts (2.80 to 2.96 A) and accounts for the low electrical conductivity in this salt. The structure is composed of square-planar Pt(CN)/sub 4//sup 2 -/ groups linked by Tl/sup +/ cations, all of whichoccupy the same molecular plane, and carbonate groups which lie between the Pt(CN)/sub 4//sup 2 -/ groups. The CO/sub 3//sup 2 -/ group oxygen atoms are clearly disordered among at least two positions, creating six partially occupied oxygen atom sites per group. The Tl/sup +/ and O separations are approx. 0.2 A shorter than the sum of the ionic radii which is probably an artifact of disorder.« less