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500 mhz unity plus spectrometer

Manufactured by Agilent Technologies

The 500 MHz Unity-Plus spectrometer is a laboratory instrument designed for high-resolution nuclear magnetic resonance (NMR) spectroscopy. It features a 500 MHz superconducting magnet and advanced electronics to enable the precise analysis of chemical and biological samples.

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4 protocols using 500 mhz unity plus spectrometer

1

NMR Spectroscopy and Kinetic Assays

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The proton NMR spectra were recorded in D2O using tetramethylsilane (TMS) as internal standard on Varian 500 MHz Unity-Plus spectrometer. Chemical shifts are reported in ppm in the following format: chemical shifts, multiplicity (s = singlet, d = doublet, t = triplet, q = quartet), type of hydrogen. In the course of column chromatographic separation the presence of products was checked by TLC using silica gel plates and acetonitrile:water (4:1; v/v) developing solvent (visualization by 0.1% ethanol solution of ninhydrin).
The kinetic assays were performed using Shimadzu-UV-1800 spectrophotometer in plastic UV-cuvette micro (BRAND, Germany).
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2

Purification and Characterization of Organic Compounds

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Ethyl acetate (ACS grade), hexanes (ACS grade), dichloromethane (ACS grade) were purchased from Fisher Scientific and used without further purification. ACS grade 1,2-dichloroethane were purchased from Acros Organics and used directly. Commercially available reagents were used without further purification. Reactions were monitored by thin layer chromatography (TLC) using Silicycle precoated silica gel plates. Flash column chromatography was performed over Silicycle silica gel (230–400 mesh). 1H NMR and 13C NMR spectra were recorded on a Varian 400 MHz spectrometer, a Varian 500 MHz Unity plus spectrometer, and a Varian 600 MHz Unity plus spectrometer, using residue solvent peaks as internal standards (CDCl3, 1H: 7.26 ppm; 13C: 77.00 ppm). Infrared spectra were recorded with a Perkin Elmer FT-IR spectrum 2000 spectrometer and are reported in reciprocal centimeter (cm−1). Mass spectra were recorded with Waters (Micromass) LCT premier #1, using electrospray method and TOF detector.
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3

Comprehensive Characterization of PEG-Functionalized C60

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Nuclear magnetic resonance (1H NMR) spectra were registered in D2O on Varian Unity Plus 500 MHz spectrometer. The Fourier Transform Infrared (FTIR) spectroscopy analysis was carried out in order to confirm successful functionalization of C60 fullerene with PEG. The samples were prepared as KBr disks and the measurements were performed using the Shimadzu 8400S spectrometer. The thermal stability of investigated samples was assessed by thermogravimetric analysis (TGA) using Q50 TGA (TA Instruments). The analyzed samples were previously dried under vacuum at 60 °C and the measurement was carried out under flow of nitrogen with heating rate of 10 K/min. In turn, electrochemical properties were evaluated using cyclic voltammetry. Cyclic voltammogram for PEG-functionalized fullerene was recorded at room temperature on Autolab PGSTAT 204 potentiostat, with three electrode arrangement: GC electrode (3 mm diameter) as working electrode, Ag/AgCl as the reference electrode and platinum wire as the counter electrode. The 0.1 M Bu4NPF6 in o-DCB:acetonitrile (3:1, v/v) was used as the supporting electrolyte solution.
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4

Synthesis and Characterization of Pd(II) Complex

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All starting materials were purchased from commercial sources and used without further purification. The ligand 4-chloro-N-(pyridin-2-ylmethyl)aniline (CPYA) and the complex precursor Na2[PdCl4] were synthesized and characterized following reported procedures [29 (link), 30 ]. Infrared spectra were measured from 4000 to 600 cm–1 on a Varian 660 FTIR equipped with Pike Miracle diamond/ZnSe ATR. 1H NMR spectra were recorded in DMSO-d6 at room temperature, using a Varian Unity-Plus 500 MHz spectrometer. Chemical shifts (δ) are given in ppm. CHN microanalyses were performed at the Universidade de São Paulo, Brazil, using a Perkin-Elmer CHN 2400 micro analyzer and with a Fisons EA 1108 analyzer at the Universitat de Barcelona, Spain. ESI–MS data were collected with a Perkin-Elmer SQ-300 mass spectrometer by direct infusion using MeOH (MS grade) as solvent.
For the DNA-interaction studies, sodium cacodylate, NaCl, Tris–borate–EDTA (TBE), ethidium bromide (EB), Hoechst 33258, pBR322 plasmid DNA (0.5 µg µL−1), calf thymus DNA (ct-DNA) and SYBR™ Safe DNA Gel Stain (Invitrogen) were acquired from commercial sources and used without further purification. Ultrapure Milli-Q® water was used to prepare the solutions.
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