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Acta Cryst. (2014). A70, C53
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In the 1970s, a large number of metal iodates compounds were extensively investigated for their nonlinear optics (NLO) properties as well as for their ferroelectric, piezoelectric, and pyroelectric properties. Interest in these compounds resumed in the early 2000s. We have shown that metal iodates are particularly interesting for for quadratic NLO in mid IR, as they possess a large domain of transparency from the visible region to the beginning of the far IR region (12.5 μm), thus covering the three atmospheric transparency windows. The synthesis of metal iodates has so far been mainly investigated by solution chemistry, under hydrothermal conditions or by the flux method. The solid state synthesis of these compounds at high pressure has never been explored. To date, only the structural evolution of α-LiIO3 with pressure has been studied by X-ray powder diffraction [1]. It was shown that, at room temperature, α-LiIO3 is stable up to 75 GPa; only compression of the lattice parameters with pressure was observed. In this work, we present a new phase of silver iodate obtained at high pressure from α-AgIO3 and characterized by X-ray powder diffraction. The α-AgIO3 to β-AgIO3 transition was characterized by differential thermal analysis (DTA) at high pressure [2-3]. The thermal behaviors of α-AgIO3 and β-AgIO3 were studied by differential scanning calorimetry (DSC) at ambient pressure and in situ temperature-dependent X-ray powder diffraction. Structural studies of these two phases were carried out to understand the formation of β-AgIO3.

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Acta Cryst. (2014). A70, C928
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These past few years, many new structures have been solved using electron diffraction methods: zone axis precession electron diffraction (PED) and tomography in reciprocal space. Both methods enable to reduce importantly the multiple scattering, so that the reflection intensities can be used for structure determination by direct methods. The ferrite Sr25Fe30O77 belongs to a family of phases whose structures consist of an intergrowth of m perovskite layers with complex rocksalt type layers [1,2]. The compound of interest is the member m = 4 of this family and its structure has been solved by combining both electron diffraction methods cited above. This oxide crystallizes in an orthorhombic system with the sub-cell parameters a ≍ b ≍ 5.4 Å and c ≍ 42 Å in a F type lattice. The structure exhibits modulation along a axis with a modulation vector q = 2/5 a. The commensurate nature of the modulation enables to describe the structure in a supercell with the cell parameters a ≍ 27 Å, b ≍ 5.4 Å and c ≍ 42 Å. PED patterns were recorded in zone axis with a Spinning Star unit using a precession angle of 20. The intensities were extracted with CRISP software and the resulting dataset was then implemented in SIR2008 for structure solution. The tomography data collection, recorded by tilting manually every 0.5 degree from -30 to +30 degrees, was inserted in a "3D Electron Diffraction Tomography" software, which reconstructs the 3D reciprocal space and extracts automatically the reflection intensities. The intensity file was then used on SIR2008 for structure determination. In order to confirm and refine the structural model, a powder X-ray diffraction pattern was performed on a laboratory diffractometer with Cu Ka1 radiation. Cell parameters were refined with the WinPlotr and FullProf Softwares using both LeBail and Rietveld methods [3]. The structural model obtained with electron diffraction data was tried and confirmed as the correct structure by the Rietveld refinements.
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