Title: Neutron Instruments for Research in Coordination Chemistry

Journal Article · · European Journal of Inorganic Chemistry
 [1]; ORCiD logo [2];  [3]; ORCiD logo [2]; ORCiD logo [2]; ORCiD logo [2];  [2]; ORCiD logo [2]; ORCiD logo [2]; ORCiD logo [2]; ORCiD logo [2]; ORCiD logo [2]
  1. Univ. of Tennessee, Knoxville, TN (United States)
  2. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
  3. National Inst. of Standards and Technology (NIST), Gaithersburg, MD (United States); Univ. of Delaware, Newark, DE (United States)
+ Show Author Affiliations

Here, neutron diffraction and spectroscopies offer unique insight into structures and properties of solids and molecular materials. All neutron instruments located at the various neutron sources are distinct, even if their designs are based on similar principles, and thus, are usually less familiar to the community than commercial X–ray diffractometers and optical spectrometers. Major neutron instruments in the USA, which are open to scientists around the world, and examples of their use in coordination chemistry research are presented here, along with a list of similar instruments at main neutron facilities in other countries. The reader may easily and quickly find from this mini–review an appropriate neutron instrument for research. The instruments include single–crystal and powder diffractometers to determine structures, inelastic neutron scattering (INS) spectrometers to probe magnetic and vibrational excitations, and quasielastic neutron scattering (QENS) spectrometers to study molecular dynamics such as methyl rotation on ligands. Key and unique features of the diffraction and neutron spectroscopies that are relevant to inorganic chemistry are reviewed.

Research Organization:
Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)
Sponsoring Organization:
USDOE
Grant/Contract Number:
AC05-00OR22725
OSTI ID:
1484103
Journal Information:
European Journal of Inorganic Chemistry, Journal Name: European Journal of Inorganic Chemistry Journal Issue: 8 Vol. 2019; ISSN 1434-1948
Publisher:
ChemPubSoc EuropeCopyright Statement
Country of Publication:
United States
Language:
English

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X-ray and Neutron Scattering Study of the Formation of Core–Shell-Type Polyoxometalates journal February 2016
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Reversible Capture and Release of Cl 2 and Br 2 with a Redox-Active Metal–Organic Framework journal April 2017
Optimized Separation of Acetylene from Carbon Dioxide and Ethylene in a Microporous Material journal June 2017
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Neutron Scattering and Spectroscopic Studies of Hydrogen Adsorption in Cr 3 (BTC) 2 —A Metal−Organic Framework with Exposed Cr 2+ Sites journal March 2011
Structural Study of D 2 within the Trimodal Pore System of a Metal Organic Framework journal April 2011
Molecular Insight into the Adsorption and Diffusion of Water in the Versatile Hydrophilic/Hydrophobic Flexible MIL-53(Cr) MOF journal May 2011
Site-Specific CO2 Adsorption and Zero Thermal Expansion in an Anisotropic Pore Network journal December 2011
Probing the Dynamics of the Porous Zr Terephthalate UiO-66 Framework Using 2 H NMR and Neutron Scattering journal May 2012
Diffusion of Xylene Isomers in the MIL-47(V) MOF Material: A Synergic Combination of Computational and Experimental Tools journal March 2013
Noble Gas Adsorption in Copper Trimesate, HKUST-1: An Experimental and Computational Study journal September 2013
Vibrational Density of States of Strongly H-Bonded Interfacial Water: Insights from Inelastic Neutron Scattering and Theory journal May 2014
Kinetic Trapping of D 2 in MIL-53(Al) Observed Using Neutron Scattering journal July 2014
Diffusion of Light Hydrocarbons in the Flexible MIL-53(Cr) Metal–Organic Framework: A Combination of Quasi-Elastic Neutron Scattering Experiments and Molecular Dynamics Simulations journal June 2014
Adsorption and Diffusion of Light Hydrocarbons in UiO-66(Zr): A Combination of Experimental and Modeling Tools journal November 2014
Quasi-Free Methyl Rotation in Zeolitic Imidazolate Framework-8 journal December 2008
Methane Sorption in Nanoporous Metal−Organic Frameworks and First-Order Phase Transition of Confined Methane journal January 2009
Adsorption and Diffusion of H 2 in the MOF Type Systems MIL-47(V) and MIL-53(Cr): A Combination of Microcalorimetry and QENS Experiments with Molecular Simulations journal April 2009
Adsorption Sites and Binding Nature of CO 2 in Prototypical Metal−Organic Frameworks: A Combined Neutron Diffraction and First-Principles Study journal June 2010
Exceptional Mechanical Stability of Highly Porous Zirconium Metal–Organic Framework UiO-66 and Its Important Implications journal March 2013
Increasing the Density of Adsorbed Hydrogen with Coordinatively Unsaturated Metal Centers in Metal−Organic Frameworks journal May 2008
Biomimetic assembly and activation of [FeFe]-hydrogenases journal June 2013
An iron complex with pendent amines as a molecular electrocatalyst for oxidation of hydrogen journal February 2013
Spin-orbit-driven magnetic structure and excitation in the 5d pyrochlore Cd2Os2O7 journal June 2016
Capture of heavy hydrogen isotopes in a metal-organic framework with active Cu(I) sites journal March 2017
Field induced spontaneous quasiparticle decay and renormalization of quasiparticle dispersion in a quantum antiferromagnet journal May 2017
Microporous metal–organic framework with dual functionalities for highly efficient removal of acetylene from ethylene/acetylene mixtures journal June 2015
Quantum-spin-liquid states in the two-dimensional kagome antiferromagnets ZnxCu4−x(OD)6Cl2 journal August 2007
Structural and magnetic phase diagram of CeFeAsO1− xFx and its relation to high-temperature superconductivity journal October 2008
Quasiparticle-continuum level repulsion in a quantum magnet journal November 2015
Higgs amplitude mode in a two-dimensional quantum antiferromagnet near the quantum critical point journal July 2017
Reversible adsorption of nitrogen dioxide within a robust porous metal–organic framework journal June 2018
Complex magnetic incommensurability and electronic charge transfer through the ferroelectric transition in multiferroic Co3TeO6 journal July 2017
Powder Diffraction: Theory and Practice book March 2008
Hydrogen storage properties and neutron scattering studies of Mg2(dobdc)—a metal–organic framework with open Mg2+ adsorption sites journal January 2011
Proton dynamics of two-dimensional oxalate-bridged coordination polymers journal January 2014
Tetragonal vs. cubic phase stability in Al – free Ta doped Li 7 La 3 Zr 2 O 12 (LLZO) journal January 2014
Gate-opening effect in ZIF-8: the first experimental proof using inelastic neutron scattering journal January 2016
Porous metal–organic frameworks with Lewis basic nitrogen sites for high-capacity methane storage journal January 2015
Adsorption of two gas molecules at a single metal site in a metal–organic framework journal January 2016
Hydrogen release reactions of Al-based complex hydrides enhanced by vibrational dynamics and valences of metal cations journal January 2016
The influence of the local structure on proton transport in a solid oxide proton conductor La 0.8 Ba 1.2 GaO 3.9 journal January 2017
Efficient separation of ethylene from acetylene/ethylene mixtures by a flexible-robust metal–organic framework journal January 2017
Gas adsorption in an isostructural series of pillared coordination cages journal January 2018
Effect of magnetic fields on the methyl rotation in a paramagnetic cobalt( ii ) complex. Quasielastic neutron scattering studies journal January 2018
An experimental and computational study of CO 2 adsorption in the sodalite-type M-BTT (M = Cr, Mn, Fe, Cu) metal–organic frameworks featuring open metal sites journal January 2018
Inelastic neutron scattering measurements on [Cu4OCl6L4] (L = pyridine or dimethyl sulfoxide). Observation of zero-field splitting of the cluster ground state  journal January 1997
Crystallography of hydrogen-containing compounds: realizing the potential of neutron powder diffraction journal January 2009
A time-of-flight backscattering spectrometer at the Spallation Neutron Source, BASIS journal August 2011
The new cold neutron chopper spectrometer at the Spallation Neutron Source: Design and performance journal August 2011
A comparison of four direct geometry time-of-flight spectrometers at the Spallation Neutron Source journal April 2014
High pressure floating zone growth and structural properties of ferrimagnetic quantum paraelectric BaFe 12 O 19 journal June 2015
The cold neutron chopper spectrometer at the Spallation Neutron Source—A review of the first 8 years of operation journal September 2016
Manipulation of ionized impurity scattering for achieving high thermoelectric performance in n-type Mg 3 Sb 2 -based materials journal September 2017
Neutron powder diffraction – new opportunities in hydrogen location in molecular and materials structure journal March 2014
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Wish: The New Powder and Single Crystal Magnetic Diffractometer on the Second Target Station journal April 2011
The D20 instrument at the ILL: a versatile high-intensity two-axis neutron diffractometer journal January 2008
MACS—a new high intensity cold neutron spectrometer at NIST journal January 2008
Powder diffraction with spin polarized neutrons journal March 2010
Hydrogen adsorption in HKUST-1: a combined inelastic neutron scattering and first-principles study journal April 2009
SEQUOIA: A Newly Operating Chopper Spectrometer at the SNS journal November 2010
IN1-LAGRANGE – the new ILL instrument to explore vibration dynamics of complex materials journal November 2014
Detection of Antiferromagnetism by Neutron Diffraction journal October 1949
Noncollinear antiferromagnetic structure of the molecule-based magnet Mn [ N ( CN ) 2 ] 2 journal September 2000
Massive triplet excitations in a magnetized anisotropic Haldane spin chain journal October 2003
Magnetic structure, magnetostriction, and magnetic transitions of the Laves-phase compound Nd Co 2 journal February 2005
Neutron scattering from a coordination polymer quantum paramagnet journal September 2006
Dynamics of quantum spin liquid and spin solid phases in IPA − Cu Cl 3 under an applied magnetic field studied with neutron scattering journal August 2007
Origin of the exceptional negative thermal expansion in metal-organic framework-5 Zn 4 O ( 1 , 4 − benzenedicarboxylate ) 3 journal August 2008
Neutron scattering evidence for isolated spin- 1 2 ladders in ( C 5 D 12 N ) 2 CuBr 4 journal September 2009
Neutron scattering study of a quasi-two-dimensional spin- 1 2 dimer system: Piperazinium hexachlorodicuprate under hydrostatic pressure journal November 2010
Magnetic neutron scattering of thermally quenched K-Co-Fe Prussian blue analog photomagnet journal August 2012
Magnetic properties of the S = 1 2 quasisquare lattice antiferromagnet CuF 2 (H 2 O) 2 (pyz) (pyz = pyrazine) investigated by neutron scattering journal August 2012
Origin of the phase transition in IrTe 2 : Structural modulation and local bonding instability journal September 2013
Magnetic ordering induced by interladder coupling in the spin- 1 2 Heisenberg two-leg ladder antiferromagnet C 9 H 18 N 2 CuBr 4 journal May 2014
Anharmonicity and atomic distribution of SnTe and PbTe thermoelectrics journal December 2014
Finite-temperature scaling of spin correlations in a partially magnetized Heisenberg S = 1 2 chain journal September 2015
Magnetic structure and phase stability of the van der Waals bonded ferromagnet Fe 3 − x GeTe 2 journal January 2016
Coupled antiferromagnetic spin- 1 2 chains in green dioptase Cu 6 [ Si 6 O 18 ] · 6 H 2 O journal February 2016
Pressure effect on hydrogen tunneling and vibrational spectrum in α -Mn journal October 2016
Combining microscopic and macroscopic probes to untangle the single-ion anisotropy and exchange energies in an S = 1 quantum antiferromagnet journal April 2017
Interplay of spin-orbit coupling and hybridization in Ca 3 LiOsO 6 and Ca 3 LiRuO 6 journal November 2017
Effect of chemical pressure on the crystal electric field states of erbium pyrochlore magnets journal January 2018
Low-temperature vibrational dynamics of fused silica and binary silicate glasses journal February 2018
Excitations in a Four-Leg Antiferromagnetic Heisenberg Spin Tube journal January 2008
External Magnetic Field Effects on a Distorted Kagome Antiferromagnet journal September 2008
Observation of Magnetoelectric Multiferroicity in a Cubic Perovskite System: LaMn 3 Cr 4 O 12 journal August 2015
Quantum Tunneling of Water in Beryl: A New State of the Water Molecule journal April 2016
Candidate Elastic Quantum Critical Point in LaCu 6 − x Au x journal November 2016
Bound Spinons in an Antiferromagnetic S = 1 / 2 Chain with a Staggered Field journal July 2004
Néel-Vector Tunneling in Antiferromagnetic Molecular Clusters journal July 2005
Direct Observation of Hydrogen Adsorption Sites and Nanocage Formation in Metal-Organic Frameworks journal November 2005
Dynamics of Composite Haldane Spin Chains in IPA − CuCl 3 journal February 2006
Spin Waves in the Frustrated Kagomé Lattice Antiferromagnet KFe 3 ( OH ) 6 ( SO 4 ) 2 journal June 2006
Spin Dynamics of the Spin- 1 / 2 Kagome Lattice Antiferromagnet ZnCu 3 ( OH ) 6 Cl 2 journal March 2007
Quantum Oscillations of the Total Spin in a Heterometallic Antiferromagnetic Ring: Evidence from Neutron Spectroscopy journal April 2007
High-temperature magnetostructural transition in van der Waals-layered α − MoCl 3 journal November 2017
Four-circle single-crystal neutron diffractometer at the High Flux Isotope Reactor journal May 2011
GSAS-II : the genesis of a modern open-source all purpose crystallography software package journal March 2013
A profile refinement method for nuclear and magnetic structures journal June 1969
Unit-cell refinement from powder diffraction scans journal December 1981
Integration of neutron time-of-flight single-crystal Bragg peaks in reciprocal space journal May 2014
SENJU: a new time-of-flight single-crystal neutron diffractometer at J-PARC journal February 2016
TOPAS and TOPAS-Academic : an optimization program integrating computer algebra and crystallographic objects written in C++ journal February 2018
Neutron Scattering in Condensed Matter Physics book May 2009
Vibrational Spectroscopy with Neutrons book June 2005
Whole powder pattern decomposition methods and applications: A retrospection journal December 2005
DEMAND, a Dimensional Extreme Magnetic Neutron Diffractometer at the High Flux Isotope Reactor journal December 2018
External magnetic field effects on a distorted kagome antiferromagnet text January 2008
Structural and magnetic phase diagram of CeFeAsO1-xFx and its relationship to high-temperature superconductivity text January 2008
High pressure floating zone growth and structural properties of ferrimagnetic quantum paraelectric BaFe$_{12}$O$_{19}$ text January 2015
Bound spinons in an antiferromagnetic S=1/2 chain with a staggered field text January 2003
Neutron scattering from a coordination polymer quantum paramagnet text January 2006
DAVE: A Comprehensive Software Suite for the Reduction, Visualization, and Analysis of Low Energy Neutron Spectroscopic Data
  • Azuah, Richard Tumanjong; Kneller, Larry R.; Qiu, Yiming
  • Journal of Research of the National Institute of Standards and Technology, Vol. 114, Issue 6 https://doi.org/10.6028/jres.114.025
journal November 2009
Double-Focusing Thermal Triple-Axis Spectrometer at the NCNR journal January 2012
Combining microscopic and macroscopic probes to untangle the single-ion anisotropy and exchange energies in an S = 1 quantum antiferromagnet text January 2017

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Spectroscopic Studies of the Magnetic Excitation and Spin‐Phonon Couplings in a Single‐Molecule Magnet journal November 2019
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Thermodynamic and kinetic studies of H 2 and N 2 binding to bimetallic nickel-group 13 complexes and neutron structure of a Ni(η 2 -H 2 ) adduct journal January 2019
Ferromagnetic Ising chains in frustrated LnODCO 3 : the influence of magnetic structure in magnetocaloric frameworks journal January 2019

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46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND TECHNOLOGY
Inelastic Neutron Scattering (INS)
Neutron Instruments
Powder Diffractometers
Quasielastic Neutron Scattering (QENS)
Single-Crystal Diffractometers