Saturn 724 ccd

Manufactured by Rigaku

The Saturn 724+ CCD is a high-performance X-ray detector designed for crystallographic applications. It features a large active area, fast readout, and high signal-to-noise ratio, providing efficient data collection for a wide range of sample types and experimental conditions.

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Lab products found in correlation

Afc12, by Rigaku (1 mentions) D max 2500, by Rigaku (1 mentions) Fv1000 ix81, by Olympus (1 mentions)

6 protocols using saturn 724 ccd

Structural and Electronic Characterization of Mg3Sb2 Crystals

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The single crystals were checked and oriented at room temperature by the white-beam backscattering Laue X-ray diffraction (XRD) method (Rigaku AFC7 plus Saturn 724 + CCD). For the polycrystalline samples, the XRD (Rigaku, Rint 2000, CuK_α) and SEM (Hitachi, S-3400N, 15 kV) analyses were performed along parallel (//P) and vertical (⊥P) to the pressing direction to characterize the texture. To experimentally reveal the valence band structure, we carried out the angle-resolved photoemission spectroscopy (ARPES) measurements of Mg₃Sb₂ single crystals at the UE112-PGM2b beamline of the synchrotron radiation facility BESSY (Berlin) with 1³ and 1² end stations, equipped with DA30L and R800 analyzers, respectively. The total energy resolution is about 15 meV while the angular resolution is 0.2°. The crystals were cleaved in situ and measured at 20 K.

Li A., Hu C., He B., Yao M., Fu C., Wang Y., Zhao X., Felser C, & Zhu T. (2021). Demonstration of valley anisotropy utilized to enhance the thermoelectric power factor. Nature Communications, 12, 5408.

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X-ray Diffraction Analysis of Crystals

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Crystals suitable for X-ray diffraction were mounted, using Paratone oil, onto a nylon loop. Data were collected at 98(2) K using a Rigaku AFC12 / Saturn 724 CCD fitted with MoKα radiation (λ = 71075 Å). Low temperature data collection was accomplished with a nitrogen cold stream maintained by an X-Stream low-temperature apparatus. Data collection and unit cell refinement were performed using CrystalClear software.⁵⁸ Data processing and absorption correction, giving minimum and maximum transmission factors, were accomplished with CrysAlisPro⁵⁹ and SCALE3 ABSPACK,⁶⁰ respectively. The structure was solved with the ShelXT⁶¹ structure solution program within Olex2⁶² using direct methods and refined (on F²) with the ShelXL package⁶³ using full-matrix, least-squares techniques. All non-hydrogen atoms were refined with anisotropic displacement parameters. All hydrogen atom positions were determined by geometry and refined by a riding model. The structure of 1^d-Et was solved in the space group P1, although the true space group is most likely

P \overset{‒}{1}

. Attempts to refine 1^d-Et in

P \overset{‒}{1}

did not produce chemically reasonable structures.

Mahesh Krishnan V., Davis I., Baker T.M., Curran D.J., Arman H.D., Neidig M.L., Liu A, & Tonzetich Z.J. (2018). Backbone Dehydrogenation in Pyrrole-Based Pincer Ligands. Inorganic chemistry, 57(15), 9544-9553.

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Single Crystal Growth and Characterization of DPA

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For single crystal data analysis, large crystals of DPA are grown from saturated solution in chloroform. The crystal analysis was performed on Rigaku Saturn724 CCD at 113(2) K using MoKα with diffraction radiation wavelength of 0.71073 Å and graphite as monochromator. For fluorescence property investigation and device fabrication, single crystals of DPA were grown by a physical vapour transport technique. Samples for laser scanning confocal microscope were grown on a 22 mm × 22 mm cover slip, and FL pictures of the crystals was recorded by laser scanning confocal microscope (Olympus FV-1000-IX81) under mercury lamp with a CCD camera. Samples for XRD characterization was grown on OTS/SiO₂/Si substrates, considering the coverage of crystals on substrates, the substrate was turned four times with each time a different edge facing the sublimation source. X-ray diffraction measurement was performed in reflection mode at 40 kV and 200 mA with Cu Ka radiation using a 2 kW Rigaku D/max-2500 X-ray diffractometer. Samples for TEM test were prepared by scratching crystals from OTS/SiO₂/Si and then transferred to copper grid with supporting carbon membrane. TEM and SAED measurements were carried out on a JEOL 2010 (Japan).

Liu J., Zhang H., Dong H., Meng L., Jiang L., Jiang L., Wang Y., Yu J., Sun Y., Hu W, & Heeger A.J. (2015). High mobility emissive organic semiconductor. Nature Communications, 6, 10032.

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Solving Disordered Crystal Structures

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The X-ray intensity data for the three compounds were collected on a Rigaku Saturn 724+ CCD diffractometer with graphite monochromatized Mo Kα radiation (λ = 0.71073 Å). The crystal structures were solved by direct methods using difference Fourier synthesis with SHELXTS24 , and refined by full-matrix least-squares method using the SHELXL-97 program25 . The non-hydrogen atoms were refined with anisotropic displacement parameters. Hydrogen atoms except for those of guest molecules were added according to theoretical models. To Dy-DDQ and Eu-DDQ, the solvent molecules and anion part of the structures were highly disordered and impossible to been found in the Fourier maps and fixed in the ideal position26 . To resolve this issue, the contribution of solvent and anionic electron density was removed by SQUEEZE routine in PLATON27 . The molecules removed were determined with elemental analysis and TG data. Crystal data and details of the structure determination for the three compounds are listed in Table S1.

Zhu Y., Zhu M., Xia L., Wu Y., Hua H, & Xie J. (2016). Lanthanide Metal-Organic Frameworks with Six-Coordinated Ln(III) Ions and Free Functional Organic Sites for Adsorptions and Extensive Catalytic Activities. Scientific Reports, 6, 29728.

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X-ray Diffraction Structural Analysis of Ni2 and Ni5

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X-ray
diffraction studies
were conducted for the suitable single-crystal of Ni2 and Ni5. Crystals were grown by the layering of heptane
into the solution of the corresponding complex in dichloromethane
at ambient temperature. The X-ray structural determination was carried
out on a Rigaku Saturn 724+ CCD diffractometer provided with graphite
monochromatic Mo Kα radiation (λ = 0.71073 Å) at
173(2) K. The cell parameters were obtained by a global refinement
of the positions of all the collected reflections. The intensities
for Lorentz and polarization effects were corrected out and an empirical
absorption was applied. The structures were resolved by the direct
methods and refined by full-matrix least-squares on F². All hydrogen atoms were placed in the calculated positions.
Structure solution and refinement were conducted by using SHELXT-97.^{21 (link)} The free solvent molecules were squeezed with
PLATON software.^{22 (link)} The details of the X-ray
structure determination data and structural refinements for Ni2 and Ni5 are provided in Table 7.

Zada M., Vignesh A., Guo L., Zhang R., Zhang W., Ma Y., Sun Y, & Sun W.H. (2020). Sterically and Electronically Modified Aryliminopyridyl-Nickel Bromide Precatalysts for an Access to Branched Polyethylene with Vinyl/Vinylene End Groups. ACS Omega, 5(18), 10610-10625.

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X-ray Diffraction Analysis of Crystalline Complexes

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Crystals of L2, L4, and L5 suitable for X-ray diffraction analyses were obtained from their heptane solution at room temperature overnight. Crystals of the complex Al1 suitable for the X-ray diffraction analyses were obtained from its toluene solution. X-ray studies were carried out on a Rigaku Saturn724 + CCD with graphite-monochromatic Mo Kα radiation (λ = 0.71073 Å) at 173 (2) K. Cell parameters were obtained by global refinement of the positions of all collected reflections. Intensities were corrected for Lorentz and polarization effects and empirical absorption. The structures were solved by direct methods and refined by full-matrix least squares on F². All hydrogen atoms were placed in calculated positions. Structure solution and refinement were performed by using the SHELXL-2014 package.^{21 (link)} Within the structure refinement of complex Al1, there were free solvent molecules that had no influence on the geometry of the main compounds. Therefore, the SQUEEZE option of the crystallographic program PLATON^{22 (link)} was used to remove these free solvents from the structure. Details of the X-ray structure determinations and refinements are provided in Table S1.† Details of the hydrogen-bonding interactions of ligands (L2, L4 and L5) are listed in Table S2.†

Yue E., Cao F., Zhang J., Zhang W., Jiang Y., Liang T, & Sun W.H. (2021). Bimetallic aluminum complexes bearing novel spiro-phenanthrene-monoketone/OH derivatives: synthesis, characterization and the ring-opening polymerization of ε-caprolactone. RSC Advances, 11(22), 13274-13281.

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