D8 venture diffractometer

¹H and ¹³C NMR spectra were tested using Bruker Avance NEO 400 MHz spectrometer (400 and 100 MHz, respectively) in d-DMSO. Chemical shifts are reported as δ values relative to internal standard d-DMSO (δ 2.50 for ¹H NMR and 39.52 for ¹³C NMR) using Bruker TopSpin 4.0.9. Infrared spectra (IR) were obtained on a PerkinElmer Spectrum BX FT-IR instrument equipped with an ATR unit at 25 °C using an Omnic software. Elemental analyses of C/H/N were investigated on a Vario EL III Analyzer. The onset decomposition temperature was measured using a TA Instruments discovery DSC25 differential scanning calorimeter at a heating rate of 5 °C min⁻¹ under dry nitrogen atmosphere. Densities were determined at room temperature by a Micromeritics AccuPyc 1345 gas pycnometer. Impact and friction sensitivities were tested by a BAM fallhammer and friction tester. X-ray diffractions of all single crystals were carried out on a Bruker D8 VENTURE diffractometer using Mo-Kα radiation (λ = 0.71073 Å). The crystal structures were produced employing Mercury 2021.1.0 software and XP. All reagents used in the experiment were purchased from Aladdin manufacturers.

The elemental analyses (C, H, and N) were carried with a Vario EL CHNOS elemental analyzer. The powder X-ray diffraction (PXRD) patterns were collected from 3° to 50° with a step of 0.02° and 0.5 s on a Bruker D8 Advance diffractometer with Cu–Kα radiation (λ = 1.54056 Å) and a Lynxeye one-Dimensional detector. Thermalgravimetric analysis (TGA) was performed on a NETZSCH STA 449F3 instrument in 30–900 °C under a nitrogen flow at a rate of 10 °C min⁻¹. TGA sample was prepared by heating SCU-8 solid in an oven at 60 °C for 12 h before analysis. A Quantachrome Autosorb Gas Sorption analyzer IQ2 was used to perform N₂ adsorption measurements. Scanning electron microscopy/energy-dispersive spectroscopy (SEM/EDS) images and data were collected using FEI Quanta 200 FEG. The concentration analysis of Re was completed using a Thermo Finnigan high resolution magnetic sector Element 2 ICP-MS instrument. HPLC-MS/MS analysis of PFOS concentration in solution was conducted using a Waters Xevo TQ_S instrument. The UV–vis spectroscopy was collected by using a Thermo Scientific GENESYS 10 s UV–vis Spectrophotometer. Single-crystal X-ray analysis was accomplished on a Bruker D8-Venture diffractometer with a Turbo X-ray Source (Mo–Kα radiation, λ = 0.71073 Å) adopting the direct-drive rotating anode technique and a CMOS detector at 273 K.

The crystal was measured on the Bruker D8 Venture diffractometer (Bruker AXS, Inc., Madison, WI, USA) at 130.0(5) K [78 ,79 ,80 ]. The structure was solved and refined using SHELXTL Software Package (Bruker AXS, Inc., Madison, WI, USA) [81 (link),82 (link)] based on atomic scattering factors taken from the International Tables [83 ]. The Molecular graphics was prepared using Mercury CSD 2020 program [84 (link)]. The details concerning X-ray diffraction experiment and crystal structure refinement are located in Table 3. Cambridge Crystallographic Data Centre (CCDC) 2038741 contains the supplementary crystallographic data for this paper. The data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/structures.

X-ray reflections for Compounds-A (Form I and Form II), -B (Form I and Form II), -C (Form I), -D and -E were collected on a Bruker D8 Quest CCD diffractometer equipped with a graphite monochromator and an Mo Kα fine-focus sealed tube (λ = 0.71073 Å) at 298 K. High-temperature data for Compound-A Form III and Compound-C Form II were collected on a Bruker D8 Venture diffractometer at 338 and 368 K, respectively. Data reduction was performed using Bruker APEX2 software. Intensities were corrected for absorption using SADABS (Sheldrick, 1997a ▸ ) and the structures were solved and refined using SHELX97 (SMART 2000 ▸ ; Sheldrick, 1997b ▸ ). All non-H atoms were refined anisotropically. H atoms on hetero atoms were located from difference electron-density maps and all C-bound H atoms were fixed geometrically. ORTEP plots are shown in Fig. S3 in the supporting information. Hydrogen-bond geometries were determined using PLATON (Spek, 2002 ▸ ). X-Seed (Barbour, 1999 ▸ ) was used to prepare packing diagrams. The crystal structures have been deposited with the Cambridge Structural Database (CCDC Numbers 1548278–1548285). Compound-A Form I is reported in the CCDC as No. 824932.

Experimental reflection intensity data for compounds I and II were collected on a Bruker D8 Venture diffractometer (Bruker AXS GmbH, Karlsruhe, Germany; graphite monochromatized MoK_α radiation, λ = 0.71073 Å) using ω-scan mode at 100 K. Absorption corrections based on measurements of equivalent reflections were applied [40 ]. The structures were solved by direct methods and refined by full-matrix least-squares on F² with anisotropic thermal parameters for all non-hydrogen atoms [41 (link)]. Hydrogen atoms were located from different Fourier syntheses and refined isotropically. Selected atom distances and bond angles are collected in Table S4. Selected crystallographic data for I and II are provided in Table 2. Atomic coordinates and anisotropic displacement parameters are given in Supplementary Materials (Tables S6–S9). CCDC 2215218 and 2215219 contain the supplementary crystallographic data for this paper. These data can be obtained free of charge via http://www.ccdc.cam.ac.uk/conts/retrieving.html (accessed on 30 November 2022) (or from the CCDC, 12 Union Road, Cambridge CB2 1EZ, U.K.; fax: +44 1223 336033; e-mail: [email protected]).