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Acta Cryst. (1996). A52, C386
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Acta Cryst. (2002). A58, c23
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Acta Cryst. (2014). A70, C151
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Study of multiferroics, materials simultaneously having more than one primary ferroic order parameter, is a hot topic of material sciences. The most extensively studied class of these compounds is the family of magnetoelectric multiferroics, where ferroelectricity can be induced by various types of magnetic orderings via the relativistic spin-orbit interaction. As a consequence of the cross coupling between spins and electric polarization, the spectacular control of the ferroelectric polarization by external magnetic field and the manipulation of the magnetic order via electric field can often be realized in these systems. Depending on the symmetry and microscopic mechanism of the multiferroicity the coupling energy between magnetic and electric ordering parameters can significantly vary. Classical neutron diffraction often fails in the precise determining of the complex magnetic structure in the multiferroics due to the presence of the statistically distributed domains in the macroscopic sample. Using spherical neutron polarimetry (SNP), known also as 3D polarization analysis, it is possible not only to precisely determine the complex magnetic structure, but also to investigate in-situ its evolution with external parameters and to control the magnetic domains distribution under the influence of the external electric or/and magnetic field. Here we will present some SNP results on few different multiferroic materials. In some of them, e.g. square lattice 2D antiferromagnet Ba2CoGe2O7, even strong electric field does not change the magnetic order. However rater week magnetic field is sufficient to create a mono-domain structure and to rotate spins in the plane. In other e.g. incommensurate (spiral) magnetic structure of the TbMnO3, solely electric field is sufficient to fully control the chirality of the magnetic structure. In the case of Cr2O3 both electric and magnetic fields should be applied in parallel in order to switch between the different antiferromagnetic domains.

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Acta Cryst. (2002). A58, c251
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Acta Cryst. (2008). A64, C575-C576
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Acta Cryst. (2014). A70, C553
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Supramolecular ferroelectric cocrystal of phenazine (Phz) with chloranilic acid (H2ca), which exhibits three successive phase transitions, have been characterized by the interplay between their structural transformations and solid-state acid-base (proton transfer) reactions (Figure) [1]. This material undergoes a ferroelectric phase (FE-I phase) transition of displacive-type at 253 K followed by successive phase transitions to the lattice modulated phases with incommensurate periodicities and with commensurate 2-fold periodicity (FE-II phase) at lower temperature [2]. To elucidate the origin of the ferroelectricity in the FE-I phase, it is crucial to study the crystal structure using single crystals. The synchrotron x-ray diffraction experiment was carried out on the imaging-plate diffractometer at BL-8A of Photon Factory in KEK. Superstructure reflections with the modulation wave vector q=(1/2 1/2 1/2) were clearly observed below 103 K. Considering the preserved 2/m Laue symmetry, the lattice can be transformed to a C-centered monoclinic lattice, which is related by (-2a, -2b, a + c) or (2a, -2b, -a - c) with the FE-I structure. Although the lattice distortion and the intensities of the superlattice reflections are consistent with the 2/m Laue symmetry, the space group C1 is deduced from the polar nature and a subgroup symmetry of the FE-I structure. Moreover, we performed single-crystal neutron diffraction experiments at SENJU of MLF/J-PARC in order to determine the displacement of the hydrogen atom. The crystal structure analysis at 10 K was carried out using the reflections measured in a half-sphere of reciprocal space at d > 0.4. The structure analysis was performed on the basis of the space group C1, where four Phz and four H2ca become crystallographically inequivalent. Finally, all the structural parameters including all hydrogen atoms were successfully refined. In the FE-II phase, the neutral and ionic molecules alternately align along the [pi]-molecular stack.

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The title compound, C18H10O4, has been isolated as an impurity in commercially available 6,11-dihydr­oxy-5,12-naphth­acenedione. The title compound exhibits yellow fluorescence in the solid state. The mol­ecule has crystallographic inversion symmetry and is planar, with an r.m.s. deviation of 0.031 (1) Å. The crystal structure is stabilized by C-H...O hydrogen bonds and [pi]-[pi] stacking inter­actions between 3-methyl­eneisobenzofuran-1(3H)-one units [inter­planar distance 3.43 (1) Å].

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Acta Cryst. (2009). A65, s69-s70
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Acta Cryst. (2014). A70, C280
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It might not be well recognized, most reflections are contaminated by multiple diffractions (MD). Therefore high redundancy data could not coincide with high accuracy data when MDs are not avoided. We collected both data set of MD-avoided and no MD-avoided ones and investigated its effectiveness in electron density measurement. For data collection, four-circle diffractometer at KEK-PF BL14A (Tsukuba, Japan) was used. In MD-avoided measurement, each reflection is collected at angle setting of least of MD contamination which calculated by psi-scan simulation software MDC [1]. In no MD-avoided measurement, usual bisect setting were used. In no MD-avoided measurement, intensities of forbidden reflections of YMn2O5 are more than 10 times largely observed than for MD-avoided one, and resulting residual density map is also highly contaminated reflecting the tendency of Fo>>Fc which is typical for reflections of weak intensity. Figure 1 shows this situation. Figure 2 is the deformation density of YTiO3 for MD-avoided data. Where model density of without Ti-3d1 valence electrons is subtracted from experimentally observed electron density. In the figure, quenching of angular momentum of Ti-3d1 electron is clearly observed. Although Rint could not be an ideal indicator of data accuracy since it cannot perceive Fo>>Fc, Rint(F) of MD-avoided measurement for YTiO3 is significantly reduced to ~0.5%. For no MD-avoided one, Rint(F) is ~1.2%. Since accuracy of MD-avoidance technique is confirmed, the next step is to exploit informations of only a few numbers of valence electrons among F(000) electrons. To accomplish this, wave function based refinement such as XAO [2] should be applied and studied.

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Acta Cryst. (2014). A70, C387
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Incommensurate helical (or cycloidal) magnetic structure may have left- and right-wound states (helicity), which are in principle equally populated in a magnet with inversion symmetry. In addition, for a Heisenberg triangular antiferromagnet, clockwise and counter-clockwise rotations of the 120 degree spin structure provide another intriguing degree of freedom. Hence, a triangular magnet that has incommensurate helical ordering along the stacking direction will show intriguing interplay of the helicity (of the helical structure) and chirality (in the triangular plane). Such phenomenon is, however, rarely studied in the past since only one example, the Ba3NbFe3Si2O14 langathite, has been known to date [1]. In this work, we study MnSb2O6, which consists of distorted triangular lattice stacking along the c-axis [2,3]. MnSb2O6 belongs to the space group P321, and hence lacks inversion symmetry. Due to this fact, unique selection of the helicity and chirality may be expected. However, the earlier studies were carried out using unpolarized neutron diffraction with mostly the powder sample, and thus helicity and chirality selection cannot be concluded. Here, we have performed single-crystal diffraction experiment using polarized neutrons in addition to the unpolarized ones, and have succeeded in determination of the magnetic structure of MnSb2O6. The resulting magnetic structure is nearly cycloidal with the magnetic modulation vector q = (0, 0, 0.182) (see figure below). The spin rotation plane is, however, inclined from the ac-plane toward the b-axis for approximately 30 degrees. Polarization analysis indicates that both the helicity of the (nearly-) cycloidal structure and chirality of the in-plane 120 degree structure are uniquely selected. The 30 degree inclination from the ac-plane is a key finding of this work, allowing new kind of multiferroicity in this material.

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Diffraction measurements on multiferroic Ba2CoGe2O7 at room temperature with both hot and cold neutrons show that the scattered intensities detected at the positions of reflections forbidden in the tetragonal space group P\overline{4}2_{1}m are entirely due to multiple diffraction (the Renninger effect).


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The crystal structure of the multiferroic melilite Ca2CoSi2O7 is determined by means of single-crystal neutron diffraction at 10 K.




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Acta Cryst. (2011). A67, C512-C513
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Acta Cryst. (2008). A64, C524
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