Single-crystal X-ray data of complexes 1 –4 were collected at 113 K on a Rigaku Saturn CCD diffractometer with graphite monochromated Mo-Kα radiation (λ = 0.71073 Å). The single-crystal structure was solved by SHELXL-2014 [75 ] and SHELXS 2014 [76 ] programs. All non-hydrogen atoms were refined anisotropically, and the H atoms of organic molecules were positioned geometrically. SIMU, DELU, ISOR and other commands were used to correct some disordered C and F atoms. Crystallographic data for complexes 1 –4 are shown in Table 2 . Key bond lengths and angles are listed in Table 3 , Table 4 and Tables S1–S4 , respectively.
Saturn ccd diffractometer
Manufactured by Rigaku
The Saturn CCD diffractometer is a versatile X-ray diffraction instrument designed for crystal structure analysis. It utilizes a CCD (Charge-Coupled Device) detector to collect diffraction data from crystalline samples. The Saturn CCD diffractometer is capable of performing single-crystal and powder X-ray diffraction experiments, providing users with the necessary tools to determine the atomic-level structure of materials.
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3 protocols using saturn ccd diffractometer
1
Single-Crystal X-ray Structural Analysis
2
Single-Crystal X-Ray Diffraction of Uranium Compounds
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Single‐crystal X‐ray diffraction measurements were carried out on a Rigaku Saturn CCD diffractometer at 100(2) K using graphite monochromated CuKα radiation (λ=1.54184 Å). An empirical absorption correction was applied using the SADABS program.[19] All structures were solved by direct methods and refined by full‐matrix least squares on F2 using the SHELXL program package.[20] All the hydrogen atoms were geometrically fixed using the riding model. The crystal data and experimental data for 2 , 5 , 9 , 10 , 12 , 14 , 16 –18 and 20 –23 are summarized in the Supporting Information. Selected bond lengths and angles are listed in Table 1 . It is of note that the structural data of 2 were relatively poor due to crystal twinning, which led to a large positive residual density (9.77 e A−3) close to the uranium atom (0.99 Å) and also to low bond precision within the C−C distances (0.02776 Å). These B level alerts in the checkCIF could not be removed on refinement.
Deposition numbers2054372 (2 ), 2054384 (5 ), 2054379 (9 ), 2054374 (10 ), 2054373 (12 ), 2054376 (14 ), 2054375 (16 ), 2054377 (17 ), 2054382 (18 ), 2054378 (20 ), 2054381 (21 ), 2054383 (22 ), and 2054380 (23 ) contain the supplementary crystallographic data for this paper. These data are provided free of charge by the joint Cambridge Crystallographic Data Centre and Fachinformationszentrum Karlsruhe Access Structures service .
Deposition numbers
3
Structural Characterization of DyCu Compound
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The diffraction data of the coordination precursor [DyCu(3,4-pdc)2(OAc)(H2O)2]•10.5H2O were collected at 296(2) K by a Rigaku Saturn CCD diffractometer equipped with graphite monochromated Mo-Kα radiation using the ω-scan technique. The Data were processed using CrystalClear software and corrected for Lorentz and polarization effects31 (link). Absorption corrections were applied using a multiscan program, and the structures were solved by direct methods then refined by full-matrix least squares based on F2 using SHELXTL program package32 .
XRD patterns were recorded on a D/Max-RB X-ray diffractometer (Rigaku) using Cu Kα irradiation at a scan rate (2θ) of 0.05°/s from 10 to 90°. Powder morphologies were monitored by SEM (Zeiss Supra 55) and HRTEM (FEI Tecnai F30), in addition with the capability of taking energy dispersive X-ray (EDX) spectra. The specific surface areas of the as-prepared samples were measured by N2 adsorption/desorption experiments at 77 K with a Builder SSA-4300 instrument. The XPS measurements were performed on a PHI 5000 C ESCA System with Mg K source operating at 14.0 kV and 25 mA.
XRD patterns were recorded on a D/Max-RB X-ray diffractometer (Rigaku) using Cu Kα irradiation at a scan rate (2θ) of 0.05°/s from 10 to 90°. Powder morphologies were monitored by SEM (Zeiss Supra 55) and HRTEM (FEI Tecnai F30), in addition with the capability of taking energy dispersive X-ray (EDX) spectra. The specific surface areas of the as-prepared samples were measured by N2 adsorption/desorption experiments at 77 K with a Builder SSA-4300 instrument. The XPS measurements were performed on a PHI 5000 C ESCA System with Mg K source operating at 14.0 kV and 25 mA.
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