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Avance dpx 500 spectrometer

Manufactured by Bruker

The Avance DPX-500 spectrometer is a Nuclear Magnetic Resonance (NMR) spectrometer designed and manufactured by Bruker. It operates at a frequency of 500 MHz and is capable of performing various NMR experiments for the analysis and characterization of chemical compounds.

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5 protocols using avance dpx 500 spectrometer

1

Synthesis and Characterization of (C^N^C)Au Complexes

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Unless otherwise stated, all manipulations were performed using standard Schlenk techniques under dry nitrogen or using Saffron Scientific or MBRAUN glove boxes. Nitrogen was purified by passing through columns of supported P2O5 with moisture indicator and activated 4 Å molecular sieves. Anhydrous solvents were freshly distilled from appropriate drying agents. (C^N^C)AuOH (30 ), (C^N^C)Au(OAcF) (30 ), [(C^N^C)Au]2O (27 ), (C^N^C)AuH (25 ), [(C^N^C)Au]2 (25 ), [(C^N^C)Au(η2-C2H4)][B(C6F5)3(OAcF)] (26 ), and B(C6F5)3 (34 ) were prepared using literature methods. [Ph3C][PF6] (Sigma) was used as purchased. Natural abundance CO (BOC) and 13CO (Euriso-Top) were used as purchased or dried before use passing through columns with activated 4 Å molecular sieves.
1H, 13C{1H}, and 19F spectra were recorded using a Bruker Avance DPX-300 or a Bruker Avance DPX-500 spectrometer. Deuterated solvents were dried over CaH2, degassed by three freeze-pump-thaw cycles, and stored on 4 Å molecular sieves before use. 1H NMR spectra (300.13 MHz) were referenced to the residual protons of the deuterated solvent used. 13C{1H} NMR spectra (75.47 MHz) were referenced internally to the D-coupled 13C resonances of the NMR solvent. IR spectra were recorded using a Perkin Elmer Spectrum 65 FT-IR spectrometer with a diamond attenuated total reflectance attachment or using liquid cells with KBr plates.
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2

Isolation and Spectroscopic Analysis

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The isolation of compound was performed in an open column chromatography (60 cm length and 3 cm diameter) using silica gel 60 (60–120 mesh size, Merck) as stationary phase, being eluted with solvents hexane, chloroform, ethyl acetate, and methanol in mixtures of increasing polarity. The compounds were visualized by UV detection and/or sprayed with a solution of vanillin/sulphuric acid/EtOH. The 1D and 2D NMR data were acquired with a Bruker Avance DPX-500 spectrometer. Chemical shifts, given on the δ scale, were referenced to the residual undeuterated portion of the deuterated solvent CDCl3.
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3

Spectroscopic Characterization of Organic Compounds

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1H-NMR, 19F-NMR, and 2D-NMR spectra were recorded on a Bruker Avance DPX 500 spectrometer (1H at 500.1 MHz, 19F at 470.5 MHz). Chemical shifts (δ) are expressed in ppm recorded using the residual solvent as the internal reference in all cases. Signal splitting patterns are described as singlet (s), doublet (d), triplet (t), quartet (q), multiplet (m), broad (br), or a combination thereof. LC-MS analyses were performed using an Agilent Technologies 1200 series HPLC connected to an Agilent Technologies 6130 quadrupole LC/MS connected to an Agilent diode array detector. High-resolution electrospray measurements were performed on a Bruker Daltonics MicrOTOF mass spectrometer.
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4

GGDS Characterization by 13C NMR

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GGDS was dissolved in 99.6 atom% D 2 O, at a concentration of 100 mg in 3 mL in a 10 mm o.d. tube. The 13 C NMR spectrum was acquired at 125 MHz on a Bruker Avance DPX-500
spectrometer at 80 °C with data averaged over 6 h. Chemical shifts were measured relative to an internal standard of Me 2 SO 39.5 ppm.
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5

GGDS Characterization by 13C NMR

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GGDS was dissolved in 99.6 atom% D 2 O, at a concentration of 100 mg in 3 mL in a 10 mm o.d. tube. The 13 C NMR spectrum was acquired at 125 MHz on a Bruker Avance DPX-500
spectrometer at 80 °C with data averaged over 6 h. Chemical shifts were measured relative to an internal standard of Me 2 SO 39.5 ppm.
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