All reagents and solvents were purchased from commercial sources and used without further purification. Manipulations were performed under a normal laboratory atmosphere unless otherwise noted. Nuclear magnetic resonance (NMR) spectra were recorded at ambient temperature using Bruker AVANCE III 400/500 or Agilent DD2 600 spectrometers, with working frequencies of 400/500/600 and 100/125/150 MHz for 1H and 13C, respectively. Chemical shifts are reported in ppm relative to the residual internal non-deuterated solvent signals (CDCl3: δH= 7.26 ppm, δC= 77.16 ppm, D2O: δH= 4.79 ppm, DMSO-d6: δH= 2.50 ppm, δC= 39.52 ppm). High-resolution mass spectra (HRMS) were measured using a SHIMADZU liquid chromatograph mass spectrometry ion trap time of flight (LCMS-IT-TOF) instrument. X-Ray crystallographic data were collected on a Bruker APEX-II CCD diffractometer.
Dd2 600
Manufactured by Agilent Technologies
Sourced in United States
The DD2 600 is a digital delay generator that provides precise timing and synchronization control for various laboratory and research applications. With a time resolution of up to 5 picoseconds and a wide range of delay settings, the DD2 600 can be used to accurately trigger and synchronize complex experimental setups.
Automatically generated - may contain errors
Lab products found in correlation
Dd2 500, by Agilent Technologies (2 mentions)
Empower 3, by Waters Corporation (2 mentions)
Tlc silica gel 60, by Merck Group (2 mentions)
20 cm aluminum sheets, by Merck Group (2 mentions)
2695 separation module system, by Waters Corporation (2 mentions)
Apex 2 ccd diffractometer, by Bruker (1 mentions)
Avance 3 400, by Bruker (1 mentions)
D8 venture, by Bruker (1 mentions)
Chirascan v100, by Applied Photophysics (1 mentions)
Autoflex 3, by Bruker (1 mentions)
1525 binary pump, by Phenomenex (1 mentions)
Xevo qtof, by Waters Corporation (1 mentions)
Luna 5μ c18 2 250, by Phenomenex (1 mentions)
400 mr dd2, by Agilent Technologies (1 mentions)
Origin 2020, by OriginLab (1 mentions)
Mestrenova, by Mestrelab Research (1 mentions)
Avance 600, by Bruker (1 mentions)
Q exactive, by Thermo Fisher Scientific (1 mentions)
Avance neo, by Agilent Technologies (1 mentions)
Nicolet in10, by Thermo Fisher Scientific (1 mentions)
16 protocols using dd2 600
1
Synthesis and Characterization of Organic Compounds
2
Multidimensional NMR Spectroscopy Protocol
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All measurements were performed on Agilent DD2 600 and 800 MHz spectrometers equipped with standard triple resonance room temperature probes. In all experiments: four scans were acquired for each FID, relaxation delay of 1.3 s was used, mixing time was set to 250 ms and temperature to 288 K. Δ of 500 and 250 μs was used for α-synuclein and Tau3x protein measurements, respectively. Detailed spectral widths and maximal evolution times are given in the Supporting Information Table S1. The pulse sequence codes for Varian/Agilent spectrometers are available from the authors on demand.
For 5D spectra 3D HNCO was used as an input for Sparse Multidimensional Fourier Transform procedure (Kazimierczuk et al. 2009 (link)). All spectra were processed using ToASTD (Kazimierczuk et al. 2006 (link)), additionally cleaner3d (Stanek and Koźmiński 2010 (link)), cleaner4d (Stanek et al. 2012 (link)), and reduced (Kazimierczuk et al. 2009 (link)) programmes were used for processing 3D, 4D and 5D spectra, respectively. All used processing software is available athttp://nmr.cent3.uw.edu.pl/software . All spectra were inspected using the Sparky program (Goddard and Kneller 2000 ), Nmrglue Python package was used for visualization purposes (Helmus and Jaroniec 2013 (link)). The whole spectra analysis and resonance assignment were performed manually.
For 5D spectra 3D HNCO was used as an input for Sparse Multidimensional Fourier Transform procedure (Kazimierczuk et al. 2009 (link)). All spectra were processed using ToASTD (Kazimierczuk et al. 2006 (link)), additionally cleaner3d (Stanek and Koźmiński 2010 (link)), cleaner4d (Stanek et al. 2012 (link)), and reduced (Kazimierczuk et al. 2009 (link)) programmes were used for processing 3D, 4D and 5D spectra, respectively. All used processing software is available at
3
NMR Characterization of Organic Compounds
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All NMR spectra were recorded on Agilent DD2-600 at 600 MHz, for 1H NMR, 1H-1H COSY, HMQC, and HMBC, and 150 MHz for 13C NMR and 13C DEPT, using CDCl3 and CD3OD as solvents. Chemical shifts were reported in ppm relative to TMS. FAB-MS and HRFAB-MS were performed using a JEOL MS-700 mass spectrometer.
4
Variable Temperature NMR Analysis of a(CFC)2
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For the Job plots 3 mM stock solutions of each component in deuterated buffer were mixed in different ratios with an interval of 10% or 20%. Spectra were recorded on a DD2 500 (Agilent) or a DD2 600 (Agilent) spectrometer. Small amounts of DMSO (83 nM) were used as reference (δ = 2.62 ppm). Variable temperature 1H NMR of a(CFC) 2 was recorded in pure D2O.
Deuterated buffer was prepared by the following procedure. Regular non-deuterated NaHPO4·2H2O (156 mg, 1 mmol) was dissolved in D2O (1 mL) and afterwards dried in vacuo. This step was repeated for a total number of three times. The salt was dissolved again in D2O (10 mL) and the pD was adjusted with NaOD (40 wt % in D2O) using a pH-calibrated glass electrode and the following relation [26 (link)].
Deuterated buffer was prepared by the following procedure. Regular non-deuterated NaHPO4·2H2O (156 mg, 1 mmol) was dissolved in D2O (1 mL) and afterwards dried in vacuo. This step was repeated for a total number of three times. The salt was dissolved again in D2O (10 mL) and the pD was adjusted with NaOD (40 wt % in D2O) using a pH-calibrated glass electrode and the following relation [26 (link)].
5
NMR and HPLC Characterization of Compounds
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The methodology used in this study was based on that used by Ble-González et al. [83 (link)] but with some modifications. NMR spectra were recorded on an Agilent DD2-600 at 600 MHz for 1H and 150 MHz for 13C NMR, using CD3OD as the solvent. Chemical shifts are reported in ppm relative to TMS. Thin-layer chromatography (TLC) was performed using TLC Silica gel 60, F254, and 20 × 20 cm aluminum sheets (Merck KGaA, Darmstadt, Germany). High-performance liquid chromatography (HPLC, Waters, Milford, MA, USA) analyses were performed on a Waters 2695 Separation module system, equipped with a photodiode array detector (Waters Co. 2996) and Empower 3 software (Waters Corporation, Milford, MA, USA).
6
Isotopic Labeling Experiment for Ammonia Source
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15N2 was used as the feeding gas for the isotopic labeling experiment to confirm the source of ammonia. 15N2 (≥98.5% chemical purity) was purchased from Newradar Special Gas Co., Ltd. Before the NRR test, 15N2 was fed into the electrolytic cell with a flow rate of 10 sccm for 30 min. Pd/ACC was tested at 0.1 V vs. RHE for 4 h in the airtight device. This procedure was repeated for 2 times. The obtained acid electrolyte solution was concentrated, added with D2O, and then identified by 600 M 1H NMR (Agilent, DD2-600).
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15N2 was used as the feeding gas for the isotopic labeling experiment to confirm the source of ammonia. 15N2 (≥98.5% chemical purity) was purchased from Newradar Special Gas Co., Ltd. Before the NRR test, 15N2 was fed into the electrolytic cell with a flow rate of 10 sccm for 30 min. Pd/ACC was tested at 0.1 V vs. RHE for 4 h in the airtight device. This procedure was repeated for 2 times. The obtained acid electrolyte solution was concentrated, added with D2O, and then identified by 600 M 1H NMR (Agilent, DD2-600).
7
NMR and HPLC Analysis of Compounds
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NMR spectra were recorded on an Agilent DD2-600 at 600 MHz for 1H and 150 MHz for 13C NMR, using CD3OD as the solvent. Chemical shifts are reported in ppm relative to TMS. Thin-layer chromatography (TLC) was performed using TLC Silica gel 60, F254, and 20 × 20 cm aluminum sheets (Merck KGaA, Darmstadt, Germany). High-performance liquid chromatography (HPLC, Milford, MA, USA) analyses were performed on a Waters 2695 Separation module system, equipped with a photodiode array detector (Waters Co. 2996) and Empower 3 software (Waters Corporation, Milford, MA, USA).
8
Spectroscopic Characterization of Chemical Compounds
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Nuclear magnetic resonance (NMR) spectra were recorded at ambient temperature using Bruker AVANCE III 400, Bruker AVANCE III 500, or Agilent DD2 600 spectrometers, with working frequencies of 400/500/600 and 100/125/150 MHz for 1H and 13C, respectively. Chemical shifts are reported in ppm relative to the residual internal non deuterated solvent signals (CDCl3: δ = 7.26 ppm, DMSO-d6: δ = 2.50 ppm). High-resolution mass spectra (HRMS) were measured by using a SHIMADZU liquid chromatograph mass spectrometry ion trap time of flight (LCMS-IT-TOF) instrument and Bruker Daltonics Autoflex III (MALDI-TOF). X-ray crystallographic data were collected on a Bruker D8 Venture diffractometer. CD spectra were recorded on a Circular Dichroism Spectrometer (Chirascan V100, Applied Photophysics Ltd).
9
Spectroscopic Analysis and Characterization
10
NMR Spectroscopy of Organic Compounds
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NMR spectra were recorded on an Agilent DD2-600 at 600 MHz for 1H and 150 MHz for 13C NMR, using CDCl3 (compounds 1 and 2 ), CD3COCD3 (compound 3 ) as the solvent. Bidimensional experiments (COSY, HSQC, and HMBC). Chemical shifts are reported in ppm relative to TMS.
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