Saturn ccd area detector

A needle-shaped single crystal of 3TfAPI, obtained by recrystallization from cyclohexane, was mounted on a fiber loop. Diffraction experiments were performed using a Rigaku Saturn CCD area detector with graphite-monochromated Mo-Kα radiation (λ = 0.71073 Å). Intensity data (6° < 2θ < 55°) were corrected for Lorentz-polarization effects and absorption. The structure solution and refinements were carried out using the CrystalStructure (2000–2018) program package (Rigaku Corp., Tokyo, Japan). The heavy-atom positions were determined by a direct method program (SIR92) and the remaining non-hydrogen atoms were found by subsequent Fourier syntheses and refined by full-matrix least-squares techniques against F² using the SHELXL-2014/7 program [51 (link)]. The position of the NH hydrogen atom was refined, whereas the remaining hydrogen atoms were included in the refinements using a riding model. Crystal data: C₁₆H₁₅N₂O₃F₃, M = 340.30, triclinic, a = 5.1357(13), b = 10.360(3), c = 14.088(4) Å, α = 84.565(7), β = 82.974(9), γ = 89.991(9)°, U = 740.5(3) ų, T = 93 K, space group P $$\overline{1}$$ (no. 2), Z = 2 reflections measured, 9064 unique (R_int = 0.0584), which were used in all calculations. The final wR(F²) was 0.1007 (for all data points). CCDC 2102046 contains supplementary crystallographic data for this study.

Upon crystallization from MeOH/H₂O (10 : 1) using the vapor diffusion method, colorless crystals were obtained for 1a, and a crystal (0.90 × 0.27 × 0.08 mm³) was separated from the sample and mounted on a glass fiber, and data were collected using a Rigaku Saturn CCD area detector with graphite-monochromated Mo Kα radiation, λ = 0.71073 Ǻ at 173(2) K. Crystal data: C₂₆H₃₃F₃O₆·H₂O, M = 516.54, space group orthorhombic, P2₁2₁2₁; unit cell dimensions a = 6.9639 (14) Å, b = 17.211 (3) Å, c = 21.948 (5) Å, V = 2630.5 (9) ų, Z = 4, D_calcd = 1.304 mg/m³,μ = 0.107 mm⁻¹, F(000) = 1096. The structure was solved by direct methods using SHELXL-2016 [19 ] and refined using full-matrix least-squares difference Fourier techniques. All nonhydrogen atoms were refined with anisotropic displacement parameters, and all hydrogen atoms were placed in idealized positions and refined as riding atoms with the relative isotropic parameters. Absorption corrections were applied with the Siemens Area Detector Absorption Program (SADABS) [20 ]. The 14274 measurements yielded 4799 independent reflections after equivalent data were averaged, and Lorentz and polarization corrections were applied. The final refinement gave R₁ = 0.0811 and wR₂ = 0.1232 [I > 2σ(I)].