A neutron-diffraction study of the crystal structure of hydrogen-containing compounds at the station MOND NRC KI

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Abstract

Using neutron-diffraction methods implemented at the commissioned MOND experimental station installed on the thermal neutron beam of the IR-8 reactor of the Kurchatov Institute, crystals of hydrogen-contained compounds Cs4(HSO4)3(H2PO4) and NH4Cl∙2H2SeO3 have been studied. The obtained results demonstrate the capabilities of the techniques for localization with high accuracy of hydrogen atoms and characterization of hydrogen bonding systems, information about which is necessary for establishing correlations between atomic, real structure and physicochemical properties of the investigated crystals.

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About the authors

I. P. Makarova

NRC “Kurchatov Institute”

Author for correspondence.
Email: makarova@crys.ras.ru

Shubnikov Institute of Crystallography, Kurchatov Complex of Crystallography and Photonics

Russian Federation, Moscow, 119333

N. N. Isakova

NRC “Kurchatov Institute”

Email: makarova@crys.ras.ru
Russian Federation, Moscow, 123182

A. I. Kalyukanov

NRC “Kurchatov Institute”

Email: makarova@crys.ras.ru
Russian Federation, Moscow, 123182

S. M. Aksenov

Kola Science Centre RAS

Email: makarova@crys.ras.ru
Russian Federation, Apatity, 184209

D. O. Charkin

Kola Science Centre RAS; Lomonosov Moscow State University

Email: makarova@crys.ras.ru

Faculty of Chemistry, Lomonosov Moscow State University

Russian Federation, Apatity, 184209; Moscow, 119991

O. I. Siidra

Lomonosov Moscow State University; St. Petersburg State University

Email: makarova@crys.ras.ru

Faculty of Chemistry, Lomonosov Moscow State University; Institute of Earth Sciences, St. Petersburg State University

Russian Federation, Moscow, 119991; St. Petersburg, 199155

A. L. Tolstikhina

NRC “Kurchatov Institute”

Email: makarova@crys.ras.ru

Shubnikov Institute of Crystallography, Kurchatov Complex of Crystallography and Photonics

Russian Federation, Moscow, 119333

R. V. Gainutdinov

NRC “Kurchatov Institute”

Email: makarova@crys.ras.ru

Shubnikov Institute of Crystallography, Kurchatov Complex of Crystallography and Photonics

Russian Federation, Moscow, 119333

V. A. Komornikov

NRC “Kurchatov Institute”

Email: makarova@crys.ras.ru

Shubnikov Institute of Crystallography, Kurchatov Complex of Crystallography and Photonics

Russian Federation, Moscow, 119333

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Supplementary files

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2. Fig. 1. Single crystal of Cs4(HSO4)3(H2PO4) prepared for neutron diffraction experiment.

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3. Fig. 2. Cs4(HSO4)3(H2PO4) crystals: distribution of the difference nuclear density calculated without taking into account hydrogen atoms. The positions of S, P and O atoms located near the section are shown, as well as the hydrogen bonds connecting the tetrahedral groups. The interval between isolines is 0.3 fm/Å3.

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4. Fig. 3. Cs4(HSO4)3(H2PO4) crystals: a – atomic structure, showing SO4 and (P,S)O4 groups linked by hydrogen bonds, and (100) planes passing through dynamically disordered O4–H3∙∙∙O6 hydrogen bonds; b – cleavage relief of a crystalline sample; c – current-voltage characteristics of the samples measured parallel (1) and perpendicular (2) to the a axis at 296 K.

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5. Fig. 4. NH4Cl∙2H2SeO3 crystals: a – main structural motif; b – distribution of the difference nuclear density calculated without taking into account hydrogen atoms in the section z = 0.41 (near the positions of the H1a, H1c and H1d atoms of the NH4 group). Two orientations of the NH4 group are shown, as well as the positions of the O atoms located near the section and the N–H∙∙∙O hydrogen bonds. Isolines are drawn at 0.5 fm/Å3.

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