Axs smart apex ccd 2

All chromatographic separations were carried out on Sortech’s silica gel (Premium Rf, 60 Å, 40–75 µm). The 1D (¹H and ¹³C) and 2D (gCOSY, gHSQC, gHMBC, NOESY) data were collected on a 500 MHz (13C: 125 MHz) Varian INOVA spectrometer operated with Vnmrj. Chloroform-d was used as solvent, and tetramethylsilane (TMS) as internal standard in the solvent. The mass spectra were obtained on a Synapt G2 HDMS instrument (Waters; Milford, MA, USA) operated in positive ESI mode. Elemental analysis was carried out on a Costech’s ECS 4010 (Valencia, CA, USA). The infrared spectra were obtained on a Perkin Elmer Spectrum 100 FT-IR spectrometer (Waltham, MA, USA) using an ATR accessory. Please see Figures S1, S2 and S4–S7 in Supplementary File 1 for NMR, IR, Anal, and MS spectra as well as the crystal structure.
Crystals of 1 were obtained by slow evaporation of a chloroform solution of 1. X-ray diffraction data were collected on a Bruker AXS Smart APEX CCD II [Mo Kα (λ = 0.71073 Å)] (Madison, WI, USA) at 295 K. The structure was solved by Olex2 using SHELXTL and was refined by full-matrix least-squares procedure (Figure S6) Non-hydrogen atoms were refined anisotropically. Hydrogen atoms were added in calculated positions and were refined. Melting points were recorded on a MEL-TEMP 1101D apparatus (Dubuque, IA, USA). The melting point values are uncorrected.