利用多孔材料负载微量样品进行XRD分析.pdfVIP

SUPPLEMENTARY INFORMATION doi:10.1038/nature11990 I. Materials and Methods Chemicals: Solvents and reagents were purchased from TCI Co., Ltd., WAKO Pure Chemical Industries Ltd., and Sigma-Aldrich Co. and used without any further purification except where noted. Glassware: Micro vials for this research were purchased from Waters (Deactivated Clear Glass 12 x 32mm Screw Neck Max Recovery Vial, 1.5 mL Volume). Syringe needle, TERUMO NN-2116R (φ = 0.80 mm), was used as an exhaust outlet for the cap of the micro vial. An incubator Fine FF-12 was used to maintain the temperature during guest inclusion. Equipment: HPLC separation of micro-gram scale natural products was performed on a JASCO UV-970 spectrometer equipped with a JASCO PU-980 pump and an ODS column DEVELOSIL ODS-5, Nomura Chemical Co., LTD. Elemental analysis was performed on a CHN/O/S elemental analyzer CE-440, Exeter Analytical, Inc. Mass spectra were recorded on a Bruker maXis spectrometer. Single crystal X-ray diffraction data were collected on a Bruker APEX-II CCD diffractometer equipped with a focusing mirror (MoKa radiation λ = 0.71073 Å) and a N2 generator (Japan Thermal Eng. Co., Ltd.) or Rigaku VariMax with RAPID (CuKa radiation λ = 1.54187 Å) . Microscopic IR spectra were recorded on a Varian DIGILAB Scimitar instrument. For X-ray diffraction and microscopic IR measurements, fluorolube was used as a protectant for the single crystals. X-ray structural analysis: The structures were solved by direct methods and refined by