Xcalibur atlas gemini ultra diffractometer

Yellow crystals of 1 was obtained from MeOH. X-ray diffraction analysis was carried out on an Xcalibur Atlas Gemini Ultra diffractometer (Agilent Technologies) with Cu Kα radiation (λ = 1.54184 Å) at 293 (2) K. Crystal data for compound 1: C₄₂H₄₄N₆O₆, M = 728.83; needle crystal (0.48 × 0.29 × 0.18 mm³), orthorhombic system, space group P 2(1), a = 9.3167 (2) Å, b = 19.4360 (3) Å, c = 21.0342 (3) Å, α = 90°, β = 90°, γ = 90°, V = 3808.86 (11) ų, Z = 4, d = 1.271 g/cm³, F(000) = 1544. A total of 6701 reflections were collected in the range 6.2 ≤ 2θ ≤ 134.0, of which 5935 unique reflections with I > 2σ(I) were collected for the analysis. The structure was refined by full-matrix least squares on F² using SHELXL-2015 package software. The final reliability factors are: R = 0.0526, wR₂ = 0.1451, Flack parameter = 0.07 (16), and the goodness of fit on F² was equal to 1.037. Crystallographic data for the structure reported in this paper have been deposited at the Cambridge Crystallographic Data Centre under the reference number CCDC 1819264. Copies of the data can be obtained, free of charge, on application to CCDC, 12 Union Road, Cambridge CB2 1EZ, UK (fax: +44-(0)1223–336033 or email: deposit@ccdc.cam.ac.Uk).

Optical rotation was measured on an Autopol I polarimeter (Rudolph Research Analytical, Hackettstown, NJ, USA). The ultraviolet (UV) absorption spectra were measured in MeOH on a METASH UV-8000 spectrophotometer (Shanghai METASH Instruments Co. Ltd., Shanghai, China). The electronic circular dichroism (ECD) was measured on a JASCO J-815 spectropolarimeter (JASCO Co. Tokyo, Japan). The infrared (IR) spectra were recorded using a Bruker Vector 32 spectrometer (Brucker, Karlsruhe, Germany). NMR spectra were recorded in CDCl₃ (ALDRICH, St. Louis, MO, USA) or MeOH-d₄ (ALDRICH, St. Louis, MO, USA) with tetramethylsilane (TMS) as an internal standard, using a Bruker AV III 500 MHz NMR spectrometer. HR-ESIMS data were obtained on an Agilent 6224 TOF LC/MS. Single crystal X-ray crystallography was determined on an Xcalibur Atlas Gemini Ultra diffractometer (Agilent Technologies). Column chromatography (CC) was performed with silica (100–200 and 200–300 mesh, Qingdao Haiyang Chemical Co., Ltd., Qingdao, China).