NMR spectra were recorded on a Varian 500 2-channel NMR spectrometer with an Agilent OneNMR probe (1H-19F/31P-15N 5 mm PFG OneNMR probe) and a Varian 400 2-channel NMR spectrometer with an Agilent OneNMR probe (1H-19F/31P-15N 5 mm PFG OneNMR probe). Chemical shifts (δ) are expressed in parts per million (ppm). All the experiments were performed at 25°C. All samples were diluted to 1mL in an 80% CD3CN, 20% D2O solvent system. For all samples 2.80mg of bortezomib (7.3×10-3mmols) and adequate quantity of phenol was added by mass and spun for 15 minutes at room temperature. All spectra were processed with MestReNova v9.0 software.
Onenmr probe
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The OneNMR probe is a nuclear magnetic resonance (NMR) probe designed for Agilent Technologies' NMR spectrometers. It is a key component for performing high-resolution NMR analysis of samples. The probe's core function is to generate and detect the radio frequency (RF) signals necessary for NMR experiments, while maintaining the appropriate magnetic field conditions for the sample.
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600 mhz spectrometer, by Agilent Technologies (5 mentions)
Mrf 400, by Agilent Technologies (2 mentions)
400 mhz spectrometer, by Agilent Technologies (2 mentions)
500 mhz nmr spectrometer, by Agilent Technologies (2 mentions)
Hiseq 4000, by Illumina (2 mentions)
Hiseq 2500, by Illumina (2 mentions)
Typhoon fla 9500, by GE Healthcare (2 mentions)
400 mhz dd2 spectrometer, by Agilent Technologies (2 mentions)
6550a q tof, by Agilent Technologies (2 mentions)
Dmso d6, by Cambridge Isotopes (2 mentions)
Amicon ultra 0.5 ml centrifugal filter, by Merck Group (2 mentions)
Vnmrs 400, by Agilent Technologies (1 mentions)
500 mhz spectrophotometer, by Agilent Technologies (1 mentions)
Avance 500 mhz spectrometer, by Bruker (1 mentions)
Inova 500 mhz spectrometer, by Agilent Technologies (1 mentions)
Uv 2075 detector, by Jasco (1 mentions)
Jms 700 mstation, by JEOL (1 mentions)
Mercury 400 mhz spectrometer, by Agilent Technologies (1 mentions)
Dip 360 polarimeter, by Jasco (1 mentions)
Du800 spectrophotometer, by Beckman Coulter (1 mentions)
30 protocols using onenmr probe
1
NMR Spectroscopic Analysis of Bortezomib
2
Semi-Hydrogenation of Internal Alkynes
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Experimental procedures and details, NMR spectra, and computational and crystallographic details can be found in the Supporting Information. In addition, NMR and computational data files can be obtained from the 4TU database under DOI: 10.4121/20015018.
Deposition Number(s)2160732 (for 2 ) and CCDC 2160733 (for 5 ) contain the supplementary crystallographic data for this paper. These data are provided free of charge by the joint Cambridge Crystallographic Data Centre and Fachinformationszentrum Karlsruhe Access Structures service .
Procedure for the semi‐hydrogenation of internal alkynes : 0.60 mL of a stock solution of complex 3 (2.5 μmol/0.60 mL) in C6D6 was added to the alkyne substrate (50 μmol, 20 equiv). The solutions were then transferred to J. Young valved NMR tubes and mesitylene (internal standard, 3.0 μL) was added. The mixtures were degassed by three freeze‐pump‐thaw cycles and filled with H2 (1 atm). The mixtures were placed in an oil bath at 25 °C (or 40 °C for some experiments) and the quantitative NMR spectra were collected after 24 h or 48 h (using an acquisition time of 5 sec and a relaxation time between scans set at 20 sec). Spectroscopic yields were determined with mesitylene as the internal standard. NMR data was recorded on an Agilent MRF 400 equipped with a OneNMR probe and Optima Tune system or a Varian VNMR−S‐400 equipped with a PFG probe at 298 K.
Deposition Number(s)
3
NMR Characterization of Fluorinated R67 DHFR
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Lyophilized R67 DHFR (100–750 μM tetramer) was dissolved in 10 mM perdeuterated Tris‐DCl (Tris‐d11) buffer, pH 8.0 in D2O. 19F NMR measurements were acquired on a Varian 500 MHz spectrophotometer equipped with a OneNMR probe operating at 470 MHz. 19F spectra were obtained with 512 scans, a spectral width of 230 ppm, relaxation delay of 1 second, and 87° pulse angle. The 19F chemical shifts were referenced to 10 mM trifluoroacetic acid. All NMR data were processed using MestReNova (Mestrelab) applying a 20 Hz line‐broadening. Fluorine incorporation levels were measured by integrating the area of a known concentration of labeled apo R67 DHFR and comparing to an internal 10 mM trifluoroacetic acid standard.
Incomplete labeling of 5F and 6F R67 DHFR was explored using the pH‐induced tetramer‐to‐dimer dissociation of R67 DHFR.16 The NMR spectra for 5F or 6F R67 DHFR were obtained at pH 8. Next, the fluorine‐labeled R67 DHFR was mixed with a molar equivalent of unlabeled R67 DHFR, equilibrated for 5 min. Subsequently, the pH of the mixture of labeled and unlabeled R67 DHFR was lowered to pH 5 to form dimeric R67 DHFR. Finally, the pH of the solution was adjusted back to pH 8 to reform the tetramer, which should be a mixture of fully labeled, fully unlabeled, and partially labeled R67 DHFR tetramers. NMR spectra were recorded at each step.
Incomplete labeling of 5F and 6F R67 DHFR was explored using the pH‐induced tetramer‐to‐dimer dissociation of R67 DHFR.
4
NMR Spectra Analysis of Synthesized Compounds
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NMR spectra of the synthesized MorBr, MorOAc and MorCl (in D2O) were obtained with Bruker Avance 500 MHz spectrometers with 16 scans for 1H NMR (500 MHz) and up to 1024 scans for 13C NMR (125 MHz) at 25 °C.
NMR spectra of the synthesized NDMMI and MorOH (in DMSO-d6 or D2O) were obtained on a Varian (400 MHz) spectrometer equipped with One NMR probe at 25 °C.
NMR spectra of the synthesized NDMMI and MorOH (in DMSO-d6 or D2O) were obtained on a Varian (400 MHz) spectrometer equipped with One NMR probe at 25 °C.
5
Optical and Spectroscopic Characterization
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Optical rotation measurements were carried out at the Na D line (589.3 nm) with a 5 cm cell at 20 ºC on a UniPol L1000 polarimeter (Schmidt + Haensch, Berlin, Germany). UV and ECD data were obtained on a Chirascan V100 spectrophotometer (Applied Photophysics, Leatherhead, U.K.). NMR experiments were performed on a Varian Inova 500 MHz spectrometer with a 5 mm OneNMR probe (Varian, Palo Alto, CA, U.S.) and on a Agilent Premium Compact 600 MHz spectrometer with a 5 mm Cryoprobe (Agilent, California, U.S). Chemical shifts were referenced in ppm to the residual solvent signals (CD3OD, at δH 3.31 and δC 49.00 ppm; DMSO-d6, at δH 2.50 and δC 39.52 ppm). High-resolution mass spectra data were obtained with an Agilent 6540 q-Tof mass spectrometer UHPLC-DAD-HRMS (Agilent 6540, Santa Clara, CA, U.S). Purifications were performed using HPLC-UV equipped with a Jasco PU-2087 pump and UV-2075 detector (Tokyo, Japan).
6
Spectroscopic Characterization of Organic Compounds
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Infrared absorbance spectra were collected with a Fourier transform infrared (FTIR) spectrometer (NICOLET 6700). Positive FAB-MS spectra were recorded on a JEOL MStation JMS700 mass spectrometer using m-nitrobenzyl alcohol as the matrix. 1H, gCOSY, and HSQC NMR experiments were performed with a Varian Mercury 400 MHz spectrometer. 13C experiments were performed with a Varian 400 MHz spectrometer equipped with a Varian OneNMR probe. Chemical shifts were referenced to the residual solvent peaks in CD3OD. Optical rotation was measured with a Jasco DIP 360 polarimeter fitted with a microcell (10 mm path length).
7
Analytical Characterization of Compounds
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Optical rotations were measured using a Jasco P-2000 polarimeter (Jasco Inc., Easton, MD, USA). UV spectra were measured using a Beckman Coulter DU-800 spectrophotometer (Beckman Coulter Inc., Brea, CA, USA). NMR spectra were collected using a Bruker 800 MHz NMR instrument (Bruker, Rheinstetten, Germany) equipped with a cryoprobe with CDCl3 and DMSO-d6 as the internal standard (δC 77.0, δH 7.26; δC 39.5, δH 2.50). A Varian 500 MHz NMR spectrometer equipped with a 5 mm, room temperature OneNMR probe was utilized for certain experiments (Varian Inc., Palo Alto, CA, USA). HRESIMS analysis was performed using a AB SCIEX TripleTOF 4600 mass spectrometer (SCIEX, Framingham, MA, USA) with Analyst TF software. Semi-preparative HPLC was carried out using a Dionex Ultimate 3000 HPLC system equipped with a micro vacuum degasser, an autosampler and a diode–array detector (Thermo Scientific, Waltham, MA, USA).
8
Spectroscopic Characterization of Organic Compounds
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NMR mono- and bi-dimensional spectra were recorded at 25 °C in a spectrometer Agilent DD2, 600 MHz with the OneNMR probe. The sample was dissolved in CDCl3 and the chemical shifts of 1H and 13C were reported using TMS as reference. Infrared spectra were obtained in a Spectrum Two FT-IR Spectrometer (Perkin Elmer) with ATR, and the samples were analyzed by forming a film with chloroform. The GC-MS analysis was record in an Agilent Technologies, and the spectral data were digitalized using the Mass Spectrum Digitizer program from the National Institute of Standards and Technology (NIST). The UV spectrum was obtained in a Perkin Elmer Lambda 35 spectrophotometer (MeOH), scanning was performed from 200 to 400 nm.
9
NMR Spectroscopy of Recombinant Allophycocyanin
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Recombinant allophycocyanin alpha subunit wild type and K6A mutant protein were prepared in phosphate saline buffer, pH 7.4, 50 mM NaH13CO3 with 20–50% D2O. 13C-NMR experiments spectra were acquired with a Varian 600 MHz spectrometer equipped with an Agilent OneNMR Probe to deliver a maximum pulsed-field gradient strength of 62 G cm−1. A 1H spectrum was acquired to examine for small molecule impurities. Thirteen 1H experiments were recorded in 12 h, collecting 131072 complex points. The repetition time was 6.7 s, of which 1.7 s comprised the acquisition time. The excitation pulse angle was set to 45 degrees. The strong interfering H2O signal was eliminated using the Robust-5 pulse sequence31 (link). Thirty-two 13C scans were collected, comprising 65 536 complex data points and a spectral width of 10 kHz. The repetition time was 6.3 s, of which 3.3 s comprised the acquisition time. The W5 inter-pulse delay was set to 240 µs. Rectangular 1 ms pulsed-field gradients were used in all cases with a strength of G1 = 28.3 G cm−1 (first pair) and G2 = 4.9 G cm−1 (second pair). The gradient stabilisation delay was 0.5 ms. The first pair of lock pre-focusing field gradients were separated from the first radio-frequency pulse by a 1.5 ms delay.
10
NMR and Mass Spectrometry Analysis of O-PnAS
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