Xtalab pro

Single-crystal data for [OS–(ph)₃–OS] was collected on a Rigaku XtaLAB Pro diffractometer with Cu-Kα radiation (λ = 1.54178 Å). Compound [OS–(ph)₃–OS] crystallized in a monoclinic space group P2₁/n with Z = 1. The empirical absorption corrections were applied using spherical harmonics, implemented in the SCALE3 ABSPACK scaling algorithm⁴⁶ . The structures were solved using direct methods, which yielded the positions of all non-hydrogen atoms. Hydrogen atoms were placed in calculated positions in the final structure refinement. Structure determination and refinement were carried out using the SHELXS-2014 and SHELXL-2014 programs, respectively⁴⁷ .

The crystallographic data of compound 1 obtained in MeOH were collected with a Rigaku XtaLAB PRO single-crystal diffractometer using Cu Kα radiation (λ = 1.54184). Briefly, their X-ray crystal structure was solved using SHELXS97, expanded by difference Fourier techniques, and refined by full-matrix least-squares calculation finally. The non-hydrogen atoms were refined anisotropically, and hydrogen atoms were fixed at calculated positions. The crystallographic data of compound 1 have been deposited in the Cambridge Crystallographic Data Centre.
Crystal Data for adametizine C (1): C₂₁H₃₁ClN₂O₁₂S₃, M_r = 635.11, crystal size 0.1 mm × 0.08 mm × 0.06 mm, orthorhombic, a = 9.16490 (10) Å, b = 11.25800 (10) Å, c = 27.3339 (2) Å, α = β = γ = 90°, V = 2407.9 (4) ų, Z = 4, T = 100.00 (10) K, Space group P2₁2₁2₁, μ = 3.837 mm^–1, ρ_calc = 1.496 g/cm³, 14,343 reflections measured (6.468° ≤ 2Θ ≤ 148.482°), 5,546 unique (R_int = 0.0275, R_sigma = 0.0325). The final R₁ values were 0.0287 [I > 2σ(I)]. The final wR (F²) values were 0.0758 [I > 2σ(I)]. The final R₁ values were 0.0299 (all data). The final wR (F²) values were 0.0764 (all data). The goodness of fit on F² was 1.049. The Flack parameter is 0.002 (6) (CDCC 2130918).

SCXRD measurements of Ag₁₂bpy-NH₂ and Ag₁₂bpy-CH₃ were performed at 150 K and measurements of Ag₁₂bpy-CH₃·O₂ were performed at 80 K on a Rigaku XtaLAB Pro diffractometers with Cu-Kα radiation (λ = 1.54184 Å). Data collection and reduction were performed using the program CrysAlisPro^{51 ,52} . All the structures were solved with direct methods (SHELXS)^{53 (link)} and refined by full-matrix least squares on F² using OLEX2⁵⁴ , which utilizes the SHELXL-2015 module⁵⁵ . All atoms were refined anisotropically, and hydrogen atoms were placed in calculated positions with idealized geometries and assigned fixed isotropic displacement parameters. Detailed information about the X-ray crystal data, intensity collection procedure and refinement results for Ag₁₂bpy-NH₂, Ag₁₂bpy-CH₃, and Ag₁₂bpy-CH₃·O₂ is summarized in Supplementary Table 2.

A powder sample of BaCoSiO₄ was prepared by the direct solid-state reaction from stoichiometric mixtures of BaCO₃, Co₃O₄, and SiO₂ powders all from Alfa Aesar (99.99%). The mixture was calcined at 900 °C in the air for 12 h and then re-grounded, pelletized, and heated at 1200 °C for 20 h and at 1250 °C for 15 h with intermediate grindings to ensure a total reaction. Finally, the sample was rapidly quenched from 1250 °C to room temperature to avoid the decomposition at intermediate temperature. The resulting powder sample is fine and bright blue in color. Large single crystals were grown using a laser-diode heated floating zone technique. The optimal growth conditions were growth speed of 2–4 mm/h, atmospheric air flow of 0.1 L/min and counter-rotation of the feed and seed rods at 15 and 30 r.p.m., respectively. Single-crystal x-ray diffraction data were collected at 95 K using a Rigaku XtaLAB PRO diffractometer with the graphite monochromated Mo K_α radiation (λ = 0.71073 Å) equipped with a HyPix-6000HE detector and an Oxford N-HeliX cryocooler. Peak indexing and integration were done using the Rigaku Oxford Diffraction CrysAlisPro software. An empirical absorption correction was applied using the SCALE3 ABSPACK algorithm as implemented in CrysAlisPro. Structure refinement was done using the FullProf suite^{33 (link)}.

SCXRD analyses of 1 were performed on a Rigaku-CCD diffractometer equipped with a Mo-Kα radiation source. The sample was cooled or warmed under a continuous flow of cold or hot N₂ gas generated using a Rigaku GN₂ low-temperature apparatus. The data from one sample were collected at 123, 173, 223, 273, 293, 313, 333, 353, 373, 393 and 413 K, in sequence. The diffraction data of samples 2, 3, 4 and 5 were collected on a Rigaku XtaLab Pro. The structures were solved by a direct method and refined via full-matrix least-squares on F² using the SHELX program^{38 (link)} with anisotropic thermal parameters for all non-hydrogen atoms. The hydrogen atoms were geometrically added and refined by the riding model. The non-hydrogen atoms in the imidazolium cation were refined with 60% C and 40% N when they are rotated in the ITP and HTP.

Crystals of compounds 1 and 5 were obtained by slow evaporation at 4 °C. A suitable crystal was selected for each of them, mounted on a nylon loop and fixed with oil. Then, X-ray diffraction and crystallographic data were collected at room temperature using redundant ω scans on a Rigaku XtaLabPro single-crystal diffractometer using microfocus Mo Kα radiation and an HPAD PILATUS3 R 200K detector.
Using Olex2 [50 (link)], the structures were readily solved by intrinsic phasing methods (SHELXT [51 (link)]) and by full-matrix least-squares methods on F2 using SHELXL [52 (link)]. The nonhydrogen atoms were refined anisotropically, and most of the hydrogen atoms were identified in difference maps and were treated as riding on their parent atoms.
For each structure, the Flack parameter [53 (link)] was refined. The determination of the absolute structure was confirmed by using Bayesian statistics on Bijvoet differences [54 (link)] based on the Olex2 results.
All the molecular graphics presented here were computed with Mercury 2020.3.0 [55 (link)].
Crystallographic data for the two structures (1 and 5) have been deposited in the Cambridge Crystallographic Data Centre database (the deposition numbers are CCDC 2085749 and CCDC 2085750, respectively). Copies of the data can be obtained free of charge from the CCDC at www.ccdc.cam.ac.uk (accessed on 7 July 2021).