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Av 400 instrument

Manufactured by Bruker
Sourced in United States, Switzerland

The AV-400 is a nuclear magnetic resonance (NMR) spectrometer manufactured by Bruker. It is designed to analyze the chemical structure and properties of materials through the detection and measurement of nuclear magnetic resonances.

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18 protocols using av 400 instrument

1

Detailed Chemical Protocols for Synthesis

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General chemical reagents and solvents were obtained from commercial suppliers. All reactions were monitored by thin layer chromatography on plates coated with 0.25 mm silica gel 60 F254 (Qingdao Haiyang Chemicals, Qingdao, China). TLC plates were visualized by UV irradiation (254 nm, Shanghai Peiqing Sci & Tech, Shanghai, China). Flash column chromatography employed silica gel (particle size 32–63 μm, Qingdao Haiyang Chemicals, Qingdao, China). Melting points were determined with a Thomas-Hoover melting point apparatus and uncorrected (Thomas Scientific, Swedesboro, NJ, USA). NMR spectra were obtained with a Bruker AV-400 instrument (Bruker BioSpin, Faellanden, Switzerland) with chemical shifts reported in parts per million (ppm, δ) and referenced to CDCl3 or DMSO-d6. The NMR spectra of compounds 117 and 1921 were provided in Supplementary Materials (Figures S1–S42). IR spectra were recorded on a Bruker Vertex-70 spectrometer (Bruker Optics, Billerica, MA, USA). Low-resolution mass spectra were reported as m/z and obtained with a Bruker amaZon SL mass spectrometer (Bruker Daltonics, Billerica, MA, USA).
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2

Synthetic Procedures and Characterization

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General chemical reagents and solvents were obtained from commercial suppliers. All reactions were monitored by thin layer chromatography on plates coated with 0.25 mm silica gel 60 F254 (Qingdao Haiyang Chemicals, Qingdao, China). TLC plates were visualized by UV irradiation (254 nm, Shanghai Peiqing Sci & Tech, Shanghai, China). Flash column chromatography employed silica gel (particle size 32–63 μm, Qingdao Haiyang Chemicals, Qingdao, China). Melting points were determined with a Thomas-Hoover melting point apparatus (Thomas Scientific, Swedesboro, NJ, USA) and uncorrected. NMR spectra were obtained with a Bruker AV-400 instrument (Bruker BioSpin, Faellanden, Switzerland) with chemical shifts reported in parts per million (ppm, δ) and referenced to CDCl3 or DMSO-d6. The NMR spectra of compounds 11, 15, 16, 2023, 25, and 2729 were provided in Supplementary Materials (Figures S1–S22). IR spectra were recorded on a Bruker Vertex-70 spectrometer (Bruker Optics, Billerica, MA, USA). High-resolution mass spectra were reported as m/z and obtained with a Dalton micrOTOF-Q II spectrometer (Bruker Daltonics, Billerica, MA, USA).
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3

Synthesis and Characterization of Furanose Derivatives

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General chemical reagents and solvents were obtained from commercial suppliers. The Bz-protected furanoses (14) were prepared according to known procedures [27 (link),29 (link),40 (link),41 (link),42 (link)]. Uridine 5′-phosphoropiperidate (14) was prepared according to a previous report [32 (link)]. All reactions were performed under an atmosphere of inert gas and monitored by thin layer chromatography on plates coated with 0.25 mm silica gel 60 F254. TLC plates were visualized by UV irradiation (254 nm). Flash column chromatography employed silica gel (particle size 32–63 μm). All NMR spectra were obtained with a Bruker AV-400 instrument (Billerica, MA, USA) with chemical shifts reported in parts per million (ppm, δ) and referenced to CDCl3, MeOH-d4, or D2O. The NMR spectra of compounds 513 and 1519 were provided in Supplementary Materials (Figures S1–S42). Low- and high-resolution mass spectra were reported as m/z and obtained with a Bruker amaZon SL and a Bruker Dalton microTOFQ II mass spectrometer, respectively. The HPLC traces of 1619 were recorded on an Agilent 1260 instrument equipped with a Waters XTerra MS C18 analytical column (4.6 × 150 mm, 5 μm) [flow rate = 1.0 mL/min; linear gradient of 5% to 100% MeOH in TEAB buffer (10 mM, pH 8.0) over 10 min; UV detection at 254 nm] and provided in Supplementary Materials (Figures S43–S46).
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4

Synthesis and Characterization of (R3P)AuCl Complexes

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All reactions were performed under an atmosphere of argon by using standard Schlenk or dry box techniques; solvents were dried over Na metal or CaH2 under nitrogen atmosphere. (R3P)AuCl (R = Me, Et) were synthesized using literature procedures66 (link)–68 (link). 1H, 13C, 29Si, and 31P NMR spectra were obtained with a Bruker AV 400 instrument at 400 MHz (1H NMR), 101 MHz (13C NMR) and 162 MHz (31P NMR), as well as Bruker AV 500 instrument at 500 MHz (1H NMR), 126 MHz (13C NMR), 99 MHz (29Si NMR), 202 MHz (31P NMR) at 298 K. Unless otherwise noted, the NMR spectra were recorded in benzene-d6 at ambient temperature. The 1H and 13C NMR chemical shifts were referenced to residual 1H and 13C signals of the solvents. NMR multiplicities are abbreviated as follows: s = singlet, d =  doublet, t = triplet, dt = doublet of triplets, m = multiplet, and brs = broad singlet. Coupling constants J are given in Hz. Electrospray ionization (ESI) mass spectra were obtained at the Mass Spectrometry Laboratory at Hangzhou Normal University with a Bruker Daltonics MicroQtof spectrometer. Melting points were measured with a BUCHI Melting Point M-560. Sampling of air-sensitive compounds was carried out using a MBRAUN’s MB-10-G glove box. UV–Vis spectra were recorded on a Shimadzu UV-1800 spectrophotometer.
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5

Synthesis and Characterization of HACD

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APTES and glutaraldehyde were purchased from Sigma-Aldrich. All other reagents were purchased from Aladdin. HACD was synthesized by means of an amide condensation reaction between HA sodium salt and mono-6-deoxyl-6-ethylenediamino-β-CD, according to a previously reported procedure (17 (link)). NMR spectra were recorded on a Bruker AV400 instrument in D2O. DLS analysis was performed on a laser light scattering spectrometer (BI-200SM) equipped with a digital correlator (TurboCorr) at 636 nm at a scattering angle of 90°.
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6

Analytical Characterization of Organic Compounds

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All solvents were analytical reagents (ARs), commercially available, and used without further purification. The reaction systems were monitored by thin-layer chromatography with silica gel precoated glass and fluorescent indicator, and the removal of solvent was carried out with a rotary evaporator and vacuum pump. As previously reported, proton (1H) and carbon (13C) NMR spectra were recorded on a Bruker AV-400 instrument and are reported in ppm relative to tetramethylsilane (TMS) and referenced to the solvent in which the spectra were collected. Low-resolution and high-resolution mass spectral (MS) data were determined on an Agilent 1100 Series LC-MS with UV detection at 254 nm and a low-resonance electrospray mode (ESI). All target compounds were purified to >95% purity, as determined by high-performance liquid chromatography (HPLC). The HPLC analysis was performed on a Waters 2695 HPLC system equipped with a Kromasil C18 column (4.6 mm × 250 mm, 5 μm).
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7

Characterization of Organic Compounds

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Reagents were
purchased from commercial
sources and were used as received unless mentioned otherwise. Commercially
available compounds were used without further purification, unless
otherwise stated. Melting points were determined on a Stuart SMP30
melting point apparatus (Bibby Scientific Ltd, U.K.). Infrared (IR)
spectra were recorded on a Simex FT-801 Fourier transform infrared
spectrometer in KBr pellets or in liquid film. 1H and 13C nuclear magnetic resonance (NMR) spectra were recorded
on a Bruker AV-400 instrument (Bruker Corporation) at 400 and 100
MHz. Chemical shifts are expressed in ppm (δ). Elemental analysis
was performed on a Thermo Fisher FlashEA 1112 elemental analyzer (Thermo
Fisher).
During the experiments, the starting reagents and the
reaction products were weighed on an analytical balance. The syntheses
were run in round-bottom flasks fitted with a magnetic stirrer. Silicon
bath was used for the heat-up.
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8

Characterization of Ag and S-P Complexes

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All reactions were performed using standard Schleck techniques under a nitrogen atmosphere. All chemicals were purchased from commercial sources and are of analytical grade. THF and DCM were dried using PURE-SOLV solvent purification system, (Innovative Technology, Amesbury, MA, USA, now known as inert, inertcorp.com). [Ag(CH3CN)4]PF6 [53 (link)] and NH4[S2P(4-C6H4OMe)(OR)] derivatives [54 (link),55 (link)] were prepared following literature procedures. NMR spectra were recorded on a Bruker AV-400 instrument (Billerica, MA, USA) operating at 400MHz. The 1H and 31P-NMR spectra were recorded at 162 MHz. For the 1H-NMR, the residual solvent proton was used as a reference (δ, ppm, CDCl3, 7.26). For 31P-NMR, H3PO4 (85%) was used as an external reference. The melting point was determined on an Electrothermal 9100 melting point apparatus (Stone, UK) and was uncorrected. The electronic absorption spectra were recorded on a Shimadzu UV-3600 UV-VIS-NIR spectrophotometer (Kyoto, Japan) using quartz cuvettes with a path length of 1 cm in the 200–400 nm for UV and 400–900 nm visible regions. The emission spectra were recorded on Perkin Elmer LS 55 fluorescence spectrometer (Waltham, MA, USA). Electrospray ionization mass spectrum (ESI-MS) for cluster 1 was recorded on Waters Micromass LCT Premier TOF-MS (Milford, MA, USA).
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9

Spectroscopic Analysis of Metal Ion Complexes

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The reagents used in the experiment process were commercially available and used directly. The metal ions salts employed are NaCl, KCl, CaCl2·2H2O, MgCl2·6H2O, CdCl2, HgCl2, FeCl3·6H2O, CrCl3·6H2O, Zn(NO3)2·6H2O, AgNO3, CoCl2·6H2O, MnCl2·4H2O, CuCl2·2H2O, NiCl2·6H2O, and PbCl2. The anions salts employed are NaClO, Na2SO4, NaNO3, Na2CO3, NaCl, NaAc, NaClO4, NaBr, KI, NaSCN, and Na2HPO4, respectively.
UV-vis absorption spectra and fluorescence emission spectra were recorded on Hitachi U-2910 spectrophotometer and Hitachi 4600 spectrofluorimeter at 25 °C with 1 cm quartz cell, respectively. Mass spectra were collected on a Thermo TSQ Quantum Access Agillent 1100 system. Nuclear magnetic resonance spectra were performed with a Bruker AV 400 instrument (400 MHz), and chemical shifts were given in ppm by using tetramethylsilane (TMS) as internal standards.
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10

Solubility of [HOOCmim]+ in Water

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The solubility of [HOOCmim]+ in water (Fig. S2) during extraction were analysed by 1H NMR recorded on a Bruker AV-400 instrument.
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