Jes x320

The reaction progress was monitored using thin-layer chromatography (TLC) on silica gel 60 F₂₅₄ (0.25 mm, Merck, Darmstadt, Germany). Column chromatography was performed using silica gel 60 (0.04–0.063 mm, Merck). Melting points were determined using a Yanaco (Tokyo, Japan) micro-melting point apparatus without correction. The LC system used was equipped with an LC-6 AD pump (Shimadzu, Kyoto, Japan), a UVDEC-100 V spectrometric detector (JASCO, Tokyo, Japan), a YRD-880 IR detector (Shimamura Tech. Co. Ltd., Tokyo, Japan), or a SPD-20A (Shimadzu), and a Capcell pack RP-18 column (Shiseido, Tokyo, Japan). NMR spectra were recorded with a JEOL JNM-LA400 spectrometer (Tokyo, Japan). The chemical shifts were expressed as ppm downfield from TMS. The mass spectra were measured on a JEOL JMS-SX102A mass spectrometer. The ESR spectra were collected on a JEOL JES-X320.

The QuadraSorb SI is used in order to analyze the specific surface area, pore size, and CO₂ adsorption quantity. UV–vis diffuse reflection absorption spectra of samples are obtained by the UV2600 spectrophotometer equipped with an integrating sphere accessory and Teflon as a reference material. The morphologies and microstructures are inspected by transmission electron microscopy (TEM, HT-7700, accelerating voltage 100 kV) and scanning electron microscope (FE-SEM, ZEISS SUPRATM 55). Elemental characterization including HAADF and EDS images are carried out by using STEM (FEI Tecnai G2 TF20). Powder X-ray diffraction (PXRD) is recorded using a Bruker D8 DISCOVER X-ray power diffractometer. Time-resolved fluorescence decay is measured by time-correlated-single photon counting (Edinburgh Instruments, FLS 920). Electron paramagnetic resonance (EPR) signals are recorded using JEOL JES-X320. Photoluminescence (PL) measurements are performed at room temperature using a F-320 fluorescence spectrophotometer.

A quartz ESR tube containing DTBDTCN powder (2.0 mg, 1.923 × 10⁻⁶ mol) was evacuated for 4 h, and then flame sealed. VT‐ESR measurements of DTBDTCN were performed on an ESR spectrometer (JES‐X320, JEOL) equipped with a variable temperature controller (ES‐13060DVT5, JEOL). A TEMPOL solution (3.309 × 10⁻⁶m) in anhydrous toluene with the spin number of 1.094 × 10¹⁵ was used as a standard sample. The integration of the ESR signals was calibrated with Mn marker peaks. The double integral of the DTBDTCN signal at variable temperatures relative to the TEMPOL signal was used to quantify the spin concentrations in DTBDTCN. Fitting of the VT ESR data was performed with the Bleaney‐Bowers equation reported in the literature.^[58] The ESR sample of DTTTCN was prepared and measured with the same methods as those for DTBDTCN.

Low-magnification transmission electron microscopy (TEM) was performed on a HITACHI HT7700 at 120 kV. High-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) and HRTEM was recorded on a FEI Talos F200X S/TEM with a field-emission gun at 200 kV. ESR spectra were collected on JEOL JES-X320. XPS was performed on SSI S-Probe XPS Spectrometer. Powder X-ray diffraction (PXRD) patterns were collected on X’Pert-Pro MPD diffractometer (Netherlands PANalytical) with a Cu Kα X-ray source (λ = 1.540598 Å).