All the results of C , H , N determinations were within ±0.4% of theoretical values, carried out by Carlo Erba Elemental Analyzer model NA-1500 (Carlo Erba, Thermo Scientific, Waltham, MA, USA). 1H NMR spectra were determined in DMSO (A –C ) or CDCl3 (D and E ) on a Bruker 300 MHz NMR spectrometer (Bruker, Billerica, MA, USA), using TMS as an internal standard. FTIR spectra were run on Perkin-Elmer Spectrum Two, UATR FT-IR spectrometer (Perkin Elmer, Waltham, MA, USA). The samples were applied as solid.
300 mhz nmr spectrometer
Manufactured by Bruker
Sourced in Germany
The 300 MHz NMR spectrometer is a laboratory instrument that uses nuclear magnetic resonance (NMR) spectroscopy to analyze the chemical composition and structure of samples. It operates at a frequency of 300 MHz, which is a standard frequency for this type of NMR spectrometer.
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Lab products found in correlation
Ft ir excalibur series mode no fts 300 mx spectrometer, by Bio-Rad (2 mentions)
Axio observer microscope, by Zeiss (2 mentions)
Xevo g2 qtof, by Waters Corporation (2 mentions)
Lc ms system, by Waters Corporation (2 mentions)
Uv254, by Cytiva (1 mentions)
Pre coated tlc plates merck 60 f254, by Merck Group (1 mentions)
4700 proteomics analyzer, by Thermo Fisher Scientific (1 mentions)
183 chns analyzer, by Leco (1 mentions)
Avs 310, by Schott (1 mentions)
Axon genepix 4000b, by Molecular Devices (1 mentions)
Bz x700 fluorescent microscope, by Keyence (1 mentions)
Biospin fourier spectrometer, by Bruker (1 mentions)
Spectrum two spectrophotometer, by PerkinElmer (1 mentions)
Uv 1700 uv vis spectrophotometer, by Shimadzu (1 mentions)
Tetrabutylammonium bromide, by Merck Group (1 mentions)
2400 chn analyzer, by PerkinElmer (1 mentions)
6520 qtof, by Agilent Technologies (1 mentions)
240 elemental analyzer, by PerkinElmer (1 mentions)
Diode array spectrophotometer, by Agilent Technologies (1 mentions)
7000 spectrofluorimeter, by Hitachi (1 mentions)
32 protocols using 300 mhz nmr spectrometer
1
Elemental and Spectroscopic Analysis
2
Compound Synthesis Protocol and Characterization
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All solvents and chemicals for compound synthesis were purchased from Acros Organics, Sigma-Aldrich, Combi-Blocks, or AstaTech, Inc. and were used as received. All evaporations were carried out in vacuo with a rotary evaporator. Nuclear magnetic resonance spectra for proton (1H NMR) were recorded on a Bruker 300 MHz NMR spectrometer. The chemical shift values are expressed in ppm (parts per million) relative to tetramethylsilane as an internal standard: s, singlet; d, doublet; t, triplet; q, quartet; m, multiplet; br, broad singlet. The relative integrals of peak areas agreed with those expected for the assigned structures. Elemental analyses were performed by AtlanticMicrolab, Incorporation (Norcross, GA, USA). Element compositions are within 0.4% of the calculated values. Thin-layer chromatography (TLC) was performed on WHATMAN UV254 silica gel plates with a fluorescent indicator and the spots were visualized under 254 and/or 365 nm illumination. Flash chromatography was performed on a Teledyne ISCO CombiFlash chromatography system using pre-packed silica gel columns purchased from Teledyne ISCO.
3
Synthesis and NMR Characterization of Nanocrystalline Li6PS5I
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The preparation of Li6PS5I is described elsewhere;46 (link) for the present
study, we used the material
of the same synthesis batch that has been recently investigated by
X-ray diffraction, 31P MAS NMR, and also by impedance measurements
and NMR spectroscopy.46 (link) To prepare nanocrystalline
Li6PS5I, 0.5 g of the starting powder was added
to ZrO2 milling vials (45 mL) under an Ar atmosphere (H2O < 1 ppm, O2 < 1 ppm). The milling jars
were filled with 60 milling balls (5 mm in diameter). Nano-Li6PS5I was treated in a Premium line 7 planetary
mill (Fritsch) that was operated at a rotation speed of 400 rpm.47 (link) The milling time was set to 120 min. For NMR
measurements, the powder was sealed in Duran ampoules.
The acquisition
of 7Li (116 MHz Larmor frequency) and 31P (121
MHz) NMR spin–lattice relaxation rates (1/T1) was carried out using a Bruker 300-MHz NMR
spectrometer; the procedures are identical to those described already
elsewhere.46 (link) We used the well-known saturation
recovery sequence to monitor the recovery of longitudinal magnetization
after a comb of closely spaced 90° perturbation pulses. The curves
were parametrized with appropriate exponential functions to extract
the rate 1/T1 as a function of temperature,
see theSupporting Information .
study, we used the material
of the same synthesis batch that has been recently investigated by
X-ray diffraction, 31P MAS NMR, and also by impedance measurements
and NMR spectroscopy.46 (link) To prepare nanocrystalline
Li6PS5I, 0.5 g of the starting powder was added
to ZrO2 milling vials (45 mL) under an Ar atmosphere (H2O < 1 ppm, O2 < 1 ppm). The milling jars
were filled with 60 milling balls (5 mm in diameter). Nano-Li6PS5I was treated in a Premium line 7 planetary
mill (Fritsch) that was operated at a rotation speed of 400 rpm.47 (link) The milling time was set to 120 min. For NMR
measurements, the powder was sealed in Duran ampoules.
The acquisition
of 7Li (116 MHz Larmor frequency) and 31P (121
MHz) NMR spin–lattice relaxation rates (1/T1) was carried out using a Bruker 300-MHz NMR
spectrometer; the procedures are identical to those described already
elsewhere.46 (link) We used the well-known saturation
recovery sequence to monitor the recovery of longitudinal magnetization
after a comb of closely spaced 90° perturbation pulses. The curves
were parametrized with appropriate exponential functions to extract
the rate 1/T1 as a function of temperature,
see the
4
Photochemical Synthesis Using Kessil LEDs
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The acquired 1H and 13C NMR spectra were recorded in CDCl3 using a Bruker 300 MHz NMR spectrometer with TMS as an internal standard (see ESI† ). Mass spectra were recorded using a Xevo G2S Q-TOF spectrometer (see ESI† ). The light source for photochemical reactions was a Kessil 456 nm-wavelength blue light-emitting diode (LED) (see ESI Fig. S1† ) (model number: KSPR160L-456-EU). LEDs producing light of different wavelengths including 370 nm, 390 nm, 467 nm and 527 nm were purchased from Kessil and were also used. Reaction tubes made of borosilicate glass were used as reaction vessels. The distance between the light source and the reaction vessel was 8 cm. TLC was performed using Merck pre-coated TLC plates (Merck 60 F254) and the results were visualized using UV light. Column chromatographic separation was carried out with silica gel (100–200 mesh). Reagents and solvents were purified as per standard procedures and used.
5
NMR and MALDI-TOF Analysis of Organic Compounds
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For each step, 1H NMR spectra were recorded with a Bruker 300 MHz NMR spectrometer at 25 °C with CDCl3 as solvent. MALDI-TOF mass spectra were acquired on a 4700 Proteomics Analyzer (Applied Biosystems). Dithranol (DT; 1,8-dihydroxy-9,10-dihydroanthracen-9-one) was used as the matrix for the ionization. Laser (YAG, 355 nm) power was adapted to obtain a significant signal-to-noise ratio and a good resolution of the mass peaks.
6
Comprehensive Analytical Techniques for Compound Characterization
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A Gallenkamp melting point apparatus (MP-D) was used to determine the melting point through an open capillary method. FTIR analysis was performed using a Bruker FT-IR Bio-Rad-Excalibur Series Mode No. FTS 300 MX spectrometer. The 1H NMR and 13C NMR spectra were recorded on a Bruker 300 MHz NMR spectrometer in deuterated DMSO and CDCl3 solutions with tetramethylsilane (TMS) as an internal reference. HPLC-MS analysis was achieved by an LC Agilent system 1200 series instrument and the elemental analyses were conducted using an LECO-183 CHNS analyzer. A UV-visible spectrophotometer (Shimadzu-1800; TCC-240, Japan), with temperature controller to maintain a required temperature of the sample (in quartz cuvette) and an automated Schott Gerate digital viscometer (Model; AVS 310) were used for DNA binding experiments.
7
NMR, Brightfield, and Fluorescence Imaging
8
Magnetic Field Characterization of NMR Spectrometers
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The axial magnetic field of the Bruker 300 MHz NMR spectrometer was measured with a resolution of 2 mm on the central axis of the magnet and at a radial distance of 40 mm from this axis with a Hall sensor of a Lakeshore 475 DSP gaussmeter. Given that potential magnetic field distributions are constrained by Maxwell’s equations, such measurements enable the estimation of both the radial and the axial component of the magnetic fields throughout the warm bore (detailed in Section A of the Supplementary Materials ). The field characteristics for the entire warm bore of the 300 MHz magnet, along with the field characterizations on the axis of the 200 MHz, 400 MHz, and 700 MHz magnets, are presented in Sections B1 and B2 of the Supplementary Materials .
9
NMR Characterization of Royleanone Derivatives
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The structures of the final product were characterized by 1D and 2D-NMR. The 1H NMR spectra of 12BzRoy-Sq, Roy-OA, and Roy-Sq were recorded on a Bruker 300 MHz NMR spectrometer and 13C, HSQC, and HMBC at 100 MHz at room temperature on a Bruker® Biospin Fourier spectrometer at the Faculty of Pharmacy of the University of Lisbon. The chemical shifts (δ, ppm) were reported relative to the residual solvent peak, CDCl3 (δ, ppm), (Aldrich 99.80%, <0.01% H2O), 7.26 [1H] and 77.16 ppm [13C]).
10
Comprehensive Characterization of Novel Compound
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Elemental analyses (carbon, hydrogen and nitrogen) were performed using a PerkinElmer 240C elemental analyzer. IR spectrum in KBr (4500–500 cm−1) was recorded with a PerkinElmer Spectrum Two spectrophotometer. Electronic spectrum in CH3CN was recorded on a Shimadzu UV-1700 UV-vis spectrophotometer. The magnetic susceptibility measurement was performed with an EG and PAR vibrating sample magnetometer, model 155 at room temperature (300 K) in a 5000 G magnetic field, and diamagnetic corrections were performed using Pascal's constants. 1H NMR spectrum in DMSO-d6 solvent was recorded in a JEOL 400 MHz NMR instrument (Fig. S4, ESI† ).13C NMR spectrum of the complex in DMSO-d6 solvent was recorded in a BRUKER 300 MHz NMR Spectrometer (Fig. S5, ESI† ).
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