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Measuring conditions of MS MS was measured with a JEOL JMS-01SG and a JEOL JMS-700 by the electron impact method where an electronic accelerating voltage of 70eV or 75 eV and an ion accelerating voltage of 8-10 kV. The direct or reservoir inlet systems were used. The dynamic range for the peak intensities was 3 digits, and the accuracy of the mass number was 0.5. If the Sample Temperature was recorded as “0˚C”, it means that the temperature could not be measured. Measuring conditions of 1H NMR 1H NMR was measured with a JEOL FX-90Q (89.56 MHz), a JEOL GX-400 (399.65 MHz), or a JEOL AL-400 (399.65 MHz). The measuring conditions for the most of the spectra were as follows: flip angle of 22.5-30.0 degrees, pulse repetition time of 30 s. The long pulse repetition time and small flip angle is used to ensure precise relative intensities. The measured temperature is set at 30 degrees centigrade. Solvent, reference, and impurity peaks were removed prior to open to the public Digital resolutions for the most of the spectra were 0.0625 Hz, 0.125 Hz, and 0.0625 Hz for the FX-90Q, GX-400, and AL-400, respectively. When peaks exist outside the standard spectral width, a wider spectral width was adopted. A sample condition was indicated in each data. The 1H NMR chemical shifts were referred to TMS in organic solvents and TSP in D2O. When the spectral assignment was difficult, additional measurements are performed such as 1H-1H and/or 13C-1H COSY, HMQC and HMBC, or by increasing the temperature or adding water. Sometimes LAOCN calculations were also carried out to confirm spectral assignments. When assignments had ambiguity, we indicated these with asterisks. The spectra with whose spectral code begins with “HPM” were generated spectra at 300 MHz from chemical shifts and coupling constants. The shifts and coupling constants for HPM-00 were extracted from spectra measured for HSP; these for HPM-01 were obtained from our publication data; those for HPM-02/03/04 were recorded from references. Measuring conditions of 13C NMR 13C NMR was measured with a NEVA NV-14 (15.087 MHz), a JEOL FX-90Q (22.530 MHz), a Varian XL-100 (25.160 MHz), a Bruker AC-200 (50.323 MHz), a JEOL FX-200 (50.183 MHz), a JEOL GX-400 (100.535 MHz) or a JEOL AL-400 (100.40 MHz). The measuring conditions for the most of the spectra were as follows: a pulse flip angle of 22.5 - 45 degrees, a pulse repetition time of 4-7 seconds, and a resolution of 0.025-0.045 ppm. The measured temperature is set at 30 degrees centigrade. The spectra whose spectral codes started with “CDS” were reconstructed from peak positions, intensities, and line widths by assuming all resonance peaks were Lorenz lines. Other spectra were the original spectra whose solvent, reference, and impurity peaks were removed prior to open to the public. A sample condition was indicated in each data. The chemical shift was referred to a TMS for all solvents. Although we acquired13C-1H COSY, HMQC, HMBC, GASPE, DEPT, and 1H coupled spectra for making the assignments unambiguous, when the assignments were not clear, symbols * and # are attached to the assignments that indicated ambiguity in the assignments. Measuring conditions of FT-IR All the IR spectra were measured in our institute using a Nicolet 170SX or a JASCO FT/IR-410. The spectral resolution for the Nicolet 170SX was 0.25 cm-1, and the spectral data were stored in the database at intervals of 0.5 cm-1 at 4000-2000 cm-1, and of 0.25 cm-1 at 2000-400 cm-1. On the other hand, the spectral resolution and the interval were 0.5 cm-1 for the JASCO FT/IR-410. Liquid samples were measured with liquid film method, and solid samples were measured by using KBr disc and Nujol paste methods. Measuring conditions of Raman All the Raman spectra were observed with a laser-Raman spectrometer in the region of 4000-0 cm-1 with an excitation wavelength of 4800 nm. The slit width was 100-200 micrometer. The states of the samples were liquid, powder or grain. The activity had ended. ESR The data source, sample conditions, and measuring conditions of ESR spectra were described to each data. The activities of ESR ended in 1987.
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