1H NMR experiments were performed in Bruker AVANCE 500 Spectrometer (Bruker UltraShield 500 plus, Bruker, Billerica, MA, USA) using 5 mm BBO probe at 298 K. Field strength was 11.7 Tesla. The operating frequencies were 500.13 MHz and for 1H NMR. 1H-NMR spectra of lyophilized CHX, QMix, brown precipitates and PCA were recorded in perdeuterated dimethyl sulfoxide (d6-DMSO) separately in accordance with tetramethylsilane as an external standard in a 1H-NMR Spectroscopy Unit [18 (link)].
Ultrashield 500 plus
Manufactured by Bruker
Sourced in United States
The Ultrashield 500 Plus is a high-performance NMR spectrometer designed for advanced analytical applications. It features a superconducting magnet that provides a stable and uniform magnetic field, enabling precise and accurate data acquisition. The core function of the Ultrashield 500 Plus is to facilitate the analysis of chemical structures and molecular properties through Nuclear Magnetic Resonance spectroscopy.
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4 protocols using ultrashield 500 plus
1
1H NMR Characterization of Organic Compounds
2
Analytical Methods for Natural Products
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Optical rotations were measured with a JASCO P-1020 digital polarimeter. IR spectra were recorded on a PerkinElmer 100 IR spectrometer with KBr. NMR spectra were obtained on a Bruker Ultrashield 500 Plus instrument, using tetramethylsilane as internal standard. Waters AQUITY UPLC/Q-TOF mass spectrometer was used to record HRESIMS spectra. Semi-preparative HPLC was performed using a RAININ pump equipped with a Gilson 133 refractive index detector. A semi-preparative column (COSMOSIL-Pack 5C18-MS-II, 10ID × 250 mm, 5 μm) was used for HPLC. Microplate reader (Kehua Technologies, Inc., Shanghai, China) was used for bioassay.
3
1H NMR Analysis of Ligands
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The 1H NMR studies for the ligands were carried out on a Bruker Ultrashield 500 Plus instrument (Billerica, MA, USA). DSS was used as an internal NMR standard and WATERGATE water suppression pulse scheme was used. Spectra were recorded in 10% (v/v) D2O/H2O or in 30% (v/v) DMSO-d6/H2O solvent mixtures in a concentration of 1 mM, respectively, at ionic strength of 0.10 M (KCl).
4
Characterization of Ruthenium Complexes
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All solvents were of analytical grade and used without further purification. the computer program Hyperquad2013 [30] . [Ru(η 6 -toluene)Cl 2 ] 2 was prepared according to a well known procedure [31] . A stock solution of [Ru(η 6 -toluene)(Z) 3 ] 2+ and the concentration of the K + , Na + and Cl -ions corresponds approximately to that of the human blood serum (c(K + ) = 3.5-5.1 mM, c(Na + ) = 135-145 mM, c(Cl -) = 96-106 mM [32] ).
HSA solution was freshly prepared before the experiments and its concentration was estimated from its UV absorption: 280 nm (HSA) = 36850 M -1 cm -1 [33] . Stock solution of N-MeIm was prepared on a weight-in-volume basis in PBS' solution. For the characterization of the prepared complexes 1 H and 13 C NMR spectroscopy, elemental analysis and electrospray ionization mass spectrometry (ESI-MS, Fig. S1) were used in addition to X-ray crystallography (vide infra). NMR spectra were recorded on a Bruker Avance III 500 spectrometer or a Bruker Ultrashield 500 Plus instrument, and DMSO-d 6 was used as solvent. ESI-MS measurements were performed using a Micromass Q-TOF Premier (Waters MS Technologies) mass spectrometer equipped with electrospray ion source.
HSA solution was freshly prepared before the experiments and its concentration was estimated from its UV absorption: 280 nm (HSA) = 36850 M -1 cm -1 [33] . Stock solution of N-MeIm was prepared on a weight-in-volume basis in PBS' solution. For the characterization of the prepared complexes 1 H and 13 C NMR spectroscopy, elemental analysis and electrospray ionization mass spectrometry (ESI-MS, Fig. S1) were used in addition to X-ray crystallography (vide infra). NMR spectra were recorded on a Bruker Avance III 500 spectrometer or a Bruker Ultrashield 500 Plus instrument, and DMSO-d 6 was used as solvent. ESI-MS measurements were performed using a Micromass Q-TOF Premier (Waters MS Technologies) mass spectrometer equipped with electrospray ion source.
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