R axis rapid area detector diffractometer

A suitable single crystal of compound 5j (CCDC 1909489) was obtained by dissolving the compound in a solution of ethyl acetate, and the solvent was placed at room temperature to slowly evaporate the solvent in air for several days. Bright white crystals of 5j (0.13 mm × 0.12 mm × 0.10 mm) were selected and mounted on a Rigaku R-AXIS RAPID area detector diffractometer equipped with graphite-monochromated Mo-Kα radiation (λ = 0.71073Å); θmax = 27.58. The crystal was kept at 293 K during data collection. Direct methods were used for structure solving by the SHELXS-97 program. A total of 28,327 integrated reflections were collected, and of those, 5128 were unique in the range with R_int = 0.0392 and Rsigma = 0.0457. Full-matrix least-squares refinement based on F² employing the weight of ω = 1/[ δ²(F₀²) + (0.0470P)² + 2.0812P] gave final values of R₁ = 0.0334, ωR₂ = 0.0981 and GOF(F) = 1.066 for 309 variables, 309 parameters and 2363 contributing reflections. Maximum shift/error = 0.003, maximum/minimum residual electron density = 0.396/−0.428 eÅ⁻³.

All the solvents and reactants were analytical pure and applied without purification. Analytical thin-layer chromatography (TLC) was exercised in silica gel GF₂₅₄. Column chromatographic purification was carried out using silica gel. Yields were not optimized. The melting point was gauged on a Beijing Taike point instrument (X-4) and was uncorrected. The infrared (IR) spectra were collected on a Bruker ALPHA-T spectrometer (in KBr pallets). The nuclear magnetic resonance (NMR) spectrum were collected on a Bruker AV-400 spectrometer using CDCl₃ as solvent and tetramethylsilane (TMS) as internal standard. The high-resolution mass spectrum was collected on a high resolution mass spectrometer (HRMS) of Bruker. Crystallographic data of the compound was measured on a Rigaku R-AXIS RAPID area-detector diffractometer.

Compound 3a was recrystallized from EtOAc/n-hexane to afford a suitable single crystal. The cell dimensions and strength of compound 3a were gauged (298 K) using a Rigaku R-AXIS RAPID area detector diffractometer (Japan) with graphite monochromated Mo-Kα radiation (λ = 0.71073 Å). 17827 measured reflections and 3651 independent reflections (R_int = 0.0247) were obtained in the range of 2.78° < 𝜃 < 28.29° (h, -14 to 14; k, -19 to 19; l, -11 to 12), and 2917 observed reflections with I > 2σ (I) were used in the refinement on F². The structure was solved by direct methods and refined utilizing SHELXS-97 (Sheldrick, 1997 ). The crystallographic data have been deposited at the Cambridge Crystallographic Data Centre (CCDC) as supplementary publication number CCDC 1856348. Copies of the data can be obtained, free of charge, upon application to CCDC, 12 Union Road, Cambridge CB2 1EZ, United Kingdom (fax: +44(1223)336033; e-mail: deposit@ccdc.cam.ac.uk).