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9 protocols using aviii 400 mhz nmr spectrometer

1

Comprehensive Characterization of Organic Compounds

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High-performance liquid chromatography (HPLC) was measured on a Waters 2487 (600E) equipment with a column of Poroshell 120 (EC-C18, 2.7 μm, 4.6 × 150 mm), using acetonitrile/water mixture (ratio = 9:1, v/v) with a flow rate of 1.0 mL/min. Nuclear magnetic resonance (NMR) spectra were carried out on a Bruker AVIII 400 MHz NMR spectrometer equipped with a Dual Probe, using deuterated chloroform (CDCl3) as the solvent. High-resolution mass spectra (HRMS) were measured on a GCT premier CAB048 mass spectrometer manipulated in a GC-TOF module with chemical ionization (CI). Ultraviolet-visible (UV-Vis) spectra were collected on a Varian Cary 50 Conc UV-Visible Spectrophotometer with Peltier. Photoluminescence (PL) spectra and their lifetimes at room temperature and 77 K were recorded on an Edinburgh FLS980 Spectrometer. Absolute quantum yield (QY) was collected on a Hamamatsu Quantum Yield Spectrometer C11347 Quantaurus. Single-crystal X-ray diffraction (XRD) was carried out on a Rigaku Oxford Diffraction (SuperNova) with Atlas diffractometer (Cu Kα (λ = 1.54184 Å)). The single-crystal structures were solved with Olex2 software. Dynamic light scattering (DLS) measurements for the diameter of aggregates were measured on a Malvern Zetasizer Nano ZS equipment at room temperature. All digital photos of crystals and amorphous compounds were recorded on a Canon EOS 60D camera.
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2

Analytical Techniques for Compound Characterization

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Fluorimetry studies were performed on a Photon Technology International fluorimeter with lamp power supply model LPS-220B, motor driver model MD-5020, and shutter control model SC-500. 1H-NMR studies were performed on a Bruker AV-III 400 MHz NMR spectrometer with ICON NMR in automation, while 13C NMR studies were run at 100 MHz. CDCl3 was used as solvent, chemical shifts are reported in ppm, while coupling constants, J, are reported in Hertz. Multiplicities in the spectra are represented by d (doublet), t (triplet), m (multiplet), and b (broad). High-resolution mass spectra (HRMS) were recorded using a Waters Synapt G2; spectra are reported as m/z (relative intensity). 1 μL of saturated LiCl in acetonitrile was added to 50 μL of sample, masses are reported for either [M+] or [M+H+] ion. Millipore water was obtained from a Milli-Q Advantage A-10 water purification system (MilliPore, USA). Microscopy images were captured using a Zeiss Axio Imager A2. Nanoparticle Tracking Analysis was performed on a Malvern NanoSight LM10.
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3

Quantification of Gaseous and Liquid Electrolysis Products

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The gaseous products are quantified every 20 min using a gas chromatograph (GC) (Agilent 7890B) equipped with a ShinCarbon ST column and a HayeSep Q column. A thermal conductivity detector is used to quantify H2 and a flame ionization detector with a methanizer is used to quantify CO, CH4, and C2H4. Ar is used as carrier gas. The analysis results of three GC analyses during the 1 h electrolysis are averaged. The liquid products are quantified using 1H NMR on a Bruker AVIII 400 MHz NMR spectrometer after the whole electrolysis process. The NMR sample is prepared by mixing 500 μL of the electrolyte collected after electrolysis with 100 μL of internal standard solution (1.67 ppm (m/m) dimethyl sulfoxide in D2O). The water signal is suppressed using the presaturation method.
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4

Comprehensive Characterization of Organic Compounds

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NMR measurements of 1H and 13C were conducted on a Bruker AVIII 400 MHz NMR spectrometer equipped with a Dual Probe. High-resolution mass spectra (HRMS) were performed on a CT Premier CAB048 mass spectrometer using a positive ESI-TOF module. Ultraviolet-visible (UV-Vis) spectra were recorded on a Varian Cary 50 UV-Visible Spectrophotometer. Photoluminescence (PL) spectra were carried out on Fluorolog®-3 (HORIBA) spectrofluorometer. Absolute quantum yields (QY) were collected using an integrating sphere on a Hamamatsu Quantum Yield Spectrometer C11347 Quantaurus. Fluorescence lifetime was recorded on an Edinburgh FLS980 Spectrometer. Dynamic light scattering (DLS) of the diameters of aggregates was measured on Malvern Zetasizer Nano ZS equipment at room temperature. Single-crystal structures of four compounds were confirmed through single-crystal X-ray diffraction on a Rigaku Oxford Diffraction (SuperNova) with Atlas diffractometer (Cu Kα (λ = 1.54184 Å) and solved using Olex2 software. All digital photographs of the solution, mixture, and crystalline powder were recorded using a Canon EOS 60D camera.
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5

Spectroscopic characterization of compounds

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All chemical reagents and solvents were of analytical grade and commercially available. Measurements UV-vis spectra were recorded on Agilent 8453 spectrometer. Fluorescence measurements were carried out using a Jasco FP-6500 spectrophotometer. 1 H NMR spectra were recorded on a Bruker AV III 400 MHz NMR spectrometer. Infrared spectra were recorded using a Bruker Vertex 70 FT-IR spectrometer with KBr pellets.
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6

Quantitative 31P NMR of Lignin

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The 31 P NMR spectrum of the lignin sample was collected using a Bruker AVIII 400 MHz NMR spectrometer (Germany). The sample was subjected to phosphitylation following a published method [31] . Briefly, 20 mg of pre-dried lignin was dissolved in a solution of pyridine/deuterated chloroform (CDCl 3 ) (1.6/1 v/v). Then, cholesterol (internal standard) and chromium acetylacetonate (relaxation agent) were added, followed by adding 2-chloro-4,4,5,5-tetramethyl-1,3,2-dioxaphospholane (TMDP) as a phosphitylating reagent. Then the mixture was shaken for 10 min to ensure thorough mixing and reaction. The 31 P NMR experiment was carried out with a 5-s relaxation delay and 2048 scans at room temperature.
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7

Argon-Atmosphere Synthesis Protocols

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All reactions were carried out under argon atmosphere with standard Schlenk techniques. DMA was purchased from Acros Organics and was not purified before use. . 1 H and 13 C NMR spectra were recorded on Bruker AV III 400 MHz NMR spectrometer equipped with BBFO probehead. Chemical shifts (δ) were reported in parts per million relative to residual chloroform (7.26 ppm for 1 H; 77.0 ppm for 13 C), constants were reported in Hertz. 1 H NMR assignment abbreviations were the following: singlet (s), doublet (d), triplet (t), quartet (q), doublet of doublets (dd), doublet of triplets (dt), and multiplet (m). 13 C NMR spectra were recorded at 100 MHz on the same spectrometer and reported in ppm. All reagents were weighed and handled in air.
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8

Sinomenine Derivatives Synthesis and Characterization

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All regents, including sinomenine, are purchased from Macklin and China National Pharmaceutical Group Corporation and used directly without further purification. All reactions are monitored by thin-layer chromatography (TLC) with GF 254 silica gel plate under an UV lamp (254 nm) or with I 2 detection. Column chromatography purifications are performed on silica gel (300-400 mesh) with CH 2 Cl 2 /CH 3 OH/ NH 3 •H 2 O (200:10:1-400:10:1, v/v) as eluents. Melting points are measured with a Jinke SGWX-4B melting point apparatus and uncorrected. IR spectra are recorded on a Nicolet 6700 FT-IR spectrometer. HRMS spectra are obtained on a ThermoFisher LTQ-Orbitrap XL mass spectrometer, the solvent used for mass spectrometry is H 2 O/CH 3 OH (1:1, v/v), with capillary temperature at 275 ℃, capillary voltage at 35 V, tube lens voltage at 110 V, source voltage at 4 kV, mass range m/z between 200-800, software used for the acquisition is Xcalibur 2.1, and the data are obtained by using ESI source in positive ionization mode. All NMR spectra are recorded on a Bruker AV-III 400 MHz NMR spectrometer using tetramethylsilane as internal standard, CDCl 3 is used as solvent and chemical shifts (δ) are reported in parts per million (ppm).
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9

Synthesis and NMR Characterization of Phenanthroline Ligands

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All the chemicals and RNA sequence were purchased from Sigma-Aldrich. All DNA sequences were purchased from Sangon (Shanghai, China). The synthetic route of N-methyl-N-(1,10-phenanthrolin-2-yl)-1,10-phenanthrolin-2-amine (L1) and N-(1,10-phenanthrolin-2-yl)-N-(2-(piperidin-1-yl)ethyl)-1,10-phenanthrolin-2-amine (L2) were described in supporting information. Milli-Q water was used in all physical measurement experiments. 195 Pt NMR spectra were recorded on a Bruker AVIII 400MHz NMR spectrometer. Chemical shift was referenced externally to K2PtCl4 in D2O (δ -1628 ppm) for 195 Pt NMR spectra.
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