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21 protocols using eca 600

1

Comprehensive Analytical Characterization

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NMR spectra were acquired on an ECA-600 (JEOL, Tokyo, Japan) using dimethyl sulfoxide (DMSO)-d6 as a solvent. UV spectra were measured on a U-2910 spectrometer (Hitachi, Tokyo, Japan) in MeCN−0.1% (vol vol−1) formic acid aq. (7:1) or MeOH−0.1% (vol vol−1) formic acid aq. (21:4) at a concentration of 50 µM. A mass spectrum was obtained on a micrOTOF-Q II−ESI-Qq-TOF spectrometer (Bruker, Billerica, MA, USA) using ESI-L Low Concentration Tuning Mix (Agilent Technologies, Santa Clara, CA, USA) as the internal standards. The sample was dissolved in MeCN−0.1% (vol vol−1) formic acid aq. (7:1) for the mass analysis. IR spectrum was measured on a FT/IR-4100 type A spectrometer (JASCO, Tokyo, Japan) using the KBr method. A fluorescence spectrum was acquired on a F-2500 spectrometer (Hitachi, Tokyo, Japan) as a solution in MeCN−0.1% (vol vol−1) formic acid aq. (7:1).
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2

Instrumental Analysis for Chemical Characterization

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JEOL ECA600, ECZ400 and ECZ600 were used for recording spectra of nuclear magnetic resonance (NMR) spectra. JASCO FT/IR-4700 spectrometer was used for recording IR spectra. JEOL AccuTOF LC-plus JMS-T100LP mass spectrometer was used for obtaining HRMS spectra. JASCO an LC-2000 Plus series were used for high-performance liquid chromatography (HPLC).
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3

Comprehensive Spectroscopic Characterization Methods

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UV–vis
spectra were recorded
using a Shimadzu UV3100PC at room temperature. The XPS measurements
were carried out on a Quantera-SXM spectrometer at room temperature.
Binding energies were measured relative to the C 1s peak (284.8 eV)
of an internal hydrocarbon. The diffuse reflectance spectra were recorded
on a Hitachi U-4000 spectrophotometer over the range from 200 to 2500
nm at room temperature. The infrared spectra were recorded on a PerkinElmer
Spectrum 400 over the range from 400 to 4000 cm–1 at room temperature. Cyclic voltammetric measurements were conducted
at room temperature using a BAS CV-50W or BAS 617E electrochemical
analyzer. Cyclic voltammograms were recorded with CH3CN
or CH2Cl2 solutions containing 0.1 M Bu4NPF6 as the supporting electrolyte. Conventional
three-electrode arrangement consisting of glassy carbon or Pt working
electrode, Ag/Ag+ reference electrode, and Pt wire counter
electrode was used. EPR spectra were measured on a JEOL TE-200 spectrometer. 1H NMR were conducted on a JEOL ECA-600.
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4

Spectroscopic Analysis of Compounds

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Melting points were measured on a Yanagimoto micro apparatus without correction. Measurement of optical rotation was carried out on a JASCO P-2300 in CHCl3 solution at 23 °C. IR spectra were recorded using a Perkin-Elmer Model Spectrum 100. 1H (400 or 600 MHz)- and 13C (100 or 150 MHz)-NMR spectra were recorded on a JEOL AL-400 or ECA-600 spectrometer using tetramethylsilane as an internal standard. The chemical shifts are expressed on the δ scale. EI-MS and HREI-MS were measured at 30–60 eV (direct inlet) with a JEOL Model JMS-700 and the relative intensities of peaks are reported with reference to the most intense peak higher than m/z 100. TLC was carried out on pre-coated silica gel 60 (Merck 5554) with n-hexane-EtOAc or CHCl3-MeOH as the developing phase. Detection was carried out by spraying with concentrated H2SO4 followed by heating. HPLC was performed on a Hitachi L-6000 equipped with a Hitachi L-7490 RI detector. The following column and solvents were used for elution: Mightysil, RP-18 GP 250–10 (25 cm x 10 mm i.d., 5μm) with MeOH-H2O or CH3CN-H2O.
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5

Biophysical Characterization of Molecular Interactions

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The experiments were performed following the methods reported in the literature.11 Fluorescence spectra were recorded on a Hitachi High-Tech F7000 spectrometer equipped with a thermostatic cell holder and a stirrer, UV-vis spectra were recorded on a JASCO V-670 spectrophotometer equipped with a JASCO ETC-717 temperature controller, and NMR spectra were recorded on a Bruker AVANCE 400 (400 MHz for 1H) or JEOL ECA-600 (600 MHz for 1H) spectrometer. ITC analysis was performed using a GE Healthcare MicroCal iTC200 microcalorimeter.
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6

Spectroscopic Characterization of Compounds

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NMR measurements were performed on a JEOL ECA-600. Mass spectra were measured using a JEOL JMS-S3000. The absorption spectra and fluorescence spectra were recorded on a JASCO V-760 spectrophotometer and a JASCO FP-8500 spectrofluorimeter, respectively. The absolute fluorescence quantum yields were determined by a Hamamatsu C9920–02. CD spectra were measured using a JASCO J-725 spectropolarimeter. SEM images were obtained using an ultra-high resolutions SEM SU9000 (Hitachi High-Tech, Corp) operated at 15–25 kV. Unstained specimens for SEM were prepared by dropping solutions of compounds onto carbon-coated copper grids. The XRD profiles were recorded using a Rigaku SmartLab X-ray diffractometer with Cu Kα radiation (λ = 0.154 nm).
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7

Synthesis and Characterization of Propionylated Hydroxypropyl Cellulose

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HPC (10 g) and DMAP (1 g) were dissolved in 200 mL of pyridine at 40 °C. 150 mL of propionic anhydride was added into the solution and the reaction was carried out at 40 °C for 24 h. After the reaction, 300 mL of methanol was added to the solution in an ice water bath and it was stirred, followed by dialysis of the mixture in ethanol for 3 days. The dialyzed sample, then, was concentrated by heating on a hot plate thermoregulated at 100 °C and dried in vacuum oven at 40 °C for 24 h to obtain PHPC. The 1H NMR measurement (600 MHz) of this sample in CDCl3 was performed using ECA 600 (JEOL Ltd.) and obtained signals were assigned as shown in Fig. S1. DSPr, an average number of introduced propionyl groups per repeating unit of HPC, was calculated from where Ic, Iring, and Ia are the integrals for the areas of signals c, ring proton, and a, respectively. DSPr of PHPC used in this work was 3.
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8

Analytical Techniques for Natural Products

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Analytical TLC was performed on silica gel 60F254 and RP-18F254S (Merck). Column chromatography was carried out on silica gel 60 (70–230 mesh, Merck) and COSMOSIL 75C18-OPN (Nacalai Tesque, Inc.). NMR spectra were recorded on JEOL ECA-600 and AL-400. Chemical shifts for 1H and 13C NMR are given in parts per million (δ) relative to tetramethylsilane (δH 0.00) and residual solvent signals (δC 77.0) as internal standards. Mass spectra were measured on JEOL JMS-700, JMS-DX303, and JMS-T 100 GC. Optical rotations were measured on JASCO P-1030.
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9

Characterization of Organometallic Complexes

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NMR spectra were recorded at room temperature using a JEOL ECA-600, ECA-500, or ECA-400 NMR spectrometer. Infrared (IR) spectra were measured using a Thermo Nicolet Avatar FT-IR spectrometer with diamond ATR. UV-vis absorption spectra were recorded in THF, toluene, and MeOH solutions in screw-capped 1 cm quartz cuvettes using an Agilent Cary 8454 UV-vis spectrophotometer. Cyclic voltammetry (CV) measurements were performed with a CH Instruments 602E potentiostat interfaced with a nitrogen glovebox via wire feedthroughs. Samples were dissolved in dichloromethane (CH2Cl2) with 0.1 M TBAPF6 as a supporting electrolyte. A 3 mm diameter glassy carbon working electrode, a platinum wire counter electrode, and a silver wire pseudo-reference electrode were used. Potentials were referenced to an internal standard of ferrocene. The bulk purity for all complexes is established by elemental analysis, performed by Atlantic Microlab, Inc.
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10

Analytical Techniques for Compound Characterization

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Analytical TLC was performed on silica gel 60 F254 (Merck). Silica gel column chromatography was carried out on silica gel 60 (70–230 mesh, Merck). Octadecyl silica gel column chromatography was carried out on Cosmosil 140C18-OPN (NACALAI TESQUE, Inc., Kyoto Japan). NMR spectra were recorded on JEOL ECA-600. Chemical shifts for 1H and 13C NMR are given in parts per million (δ) relative to tetramethylsilane (δH 0.00) and residual solvent signals (δC 77.0) as internal standards. Mass spectra were measured on JEOL JMS-700 and JMS-DX303.
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