All 1H NMR oxidation titrations were carried out by adding a well-stirred suspension of thianthrenium hexafluoroantimonate to a solution of the porphyrin nanoring in CD2Cl2 at –60 °C to –20 °C under a counterflow of argon (see Supplementary Material for details). These oxidation experiments were conducted in NMR tubes fitted with J. Young greaseless PTFE stopcocks using CD2Cl2 stored over molecular sieves, using standard Schlenk line techniques to exclude moisture. Exposure to water is immediately deleterious to porphyrin polycations, but they are stable to oxygen (O2). The neutral nanorings are only sparingly soluble in CD2Cl2 at low temperatures (< –40 °C), but solubility improves dramatically upon oxidation. The NMR measurements were performed on a Bruker AVII 500 (5 mm BBFO probe). 1H NMR chemical shifts were calibrated to residual proton signals of the solvent (CHDCl2 5.32 ppm). 13C NMR chemical shifts were referenced to the solvent peak (CD2Cl2 54.00 ppm). 19F NMR spectra were referenced to hexafluorobenzene (–164.8 ppm). At the end of each titration, decamethylferrocene (FeCp2*) was added to reduce the porphyrin nanoring back to its neutral form; the whole oxidation process is highly reversible.
Avii 500
Manufactured by Bruker
The AVII 500 is a high-performance nuclear magnetic resonance (NMR) spectrometer designed for analytical and research applications. It features a 500 MHz superconducting magnet and provides advanced capabilities for the investigation of chemical and biological samples.
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Lab products found in correlation
Av 400, by Bruker (2 mentions)
Aviii hd 400, by Bruker (1 mentions)
Aviii hd 500, by Bruker (1 mentions)
Si 60, by Merck Group (1 mentions)
Neo400, by Bruker (1 mentions)
Lcms 2020, by Shimadzu (1 mentions)
T60u spectrometer, by PG Instruments (1 mentions)
Mercury vx 300, by Agilent Technologies (1 mentions)
Aviii hd 600, by Bruker (1 mentions)
507 pp tubes, by Wilmad (1 mentions)
Mercury vx 300, by Bruker (1 mentions)
Asx300, by Bruker (1 mentions)
Drx 250, by Bruker (1 mentions)
9 protocols using avii 500
1
Oxidation Titration of Porphyrin Nanorings
2
Oxidation Titration of Porphyrin Nanorings
3
Synthesis of Organic Compounds
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All reactions were performed open to air and without precautions to exclude air/moisture unless specified otherwise. Reagents and solvents were purchased from commercial sources and used without further purification unless specified otherwise. NMR spectra were recorded on Bruker AVIII HD 400, NEO 400, AVIII HD 500 and AVII 500 spectrometers. Chemical shifts (δ) are quoted in parts per million (ppm). 1H and 13C NMR spectra are referenced to residual protons in chloroform-d (δH = 7.26, δC = 77.16) and acetone-d6 (δH = 2.05, δC = 28.95). Peak multiplicities are defined as s (singlet), d (doublet), t (triplet), q (quartet), m (multiplet) and br (broad). Coupling constants (J) are reported to the nearest 0.1 Hz. High-resolution mass spectra (HRMS) were recorded on a Thermo Scientific exactive mass spectrometer (Waters Equity autosampler and pump) for electrospray ionisation (ESI). Flash chromatography refers to normal phase column chromatography on silica gel (Merck Si 60, 0.040–0.063 mm) under a positive pressure of nitrogen.
4
Organic Synthesis Characterization Methods
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All reagents and solvents were used as purchased from commercial sources. Chromatography was performed using silica gel (200–300 mesh). All reactions were monitored by thin layer chromatography (TLC), using silica gel plates with fluorescence F254 and ultraviolet light visualization. Proton nuclear magnetic resonance (NMR) spectra were obtained on a Bruker AVII 500 with the use of CDCl3, CD3OD, (CD3)2CO or DMSO-d6 as solvents. Carbon-13 NMR spectra were obtained on a Bruker spectrometer (125 MHz) by the use of DMSO-d6 as a solvent. Chemical shifts are referenced to the residual solvent peak and reported in ppm (d-scale) and all coupling constant (J) values are given in Hz. The following multiplicity abbreviations are used: (s) singlet, (d) doublet, (t) triplet, (q) quartet, (m) multiplet and (br) broad. Electron spray ionization-mass spectrum (ESI-MS) data were recorded on a Shimadzu LC-MS 2020.
5
Purification and Characterization of Compounds
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All commercially available starting materials were used without further purification. Nuclear magnetic resonance (NMR) spectra were recorded on a Bruker AV (II) 500 at 500 MHz. High resolution mass spectra (HRMS) were recorded on a Bruker microOTOFII with electrospray ionization (ESI).
6
Characterization of Chemical Reagents and Solvents
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All solvents and reagents were purchased from commercial suppliers and used as received, unless otherwise stated. Dry solvents were obtained by purging with N2 and then passing through an MBraun MPSP-800 column. H2O was deionised and microfiltered by using a Milli-Q Millipore machine. Et3N was distilled and stored over KOH. TBA salts were stored in a vacuum desiccator containing P2O5 prior to use. 1H, 13C, 19F and 31P NMR spectra were recorded on a Varian Mercury-VX 300, a Varian Unity Plus 500, a Bruker AVD500 or a Bruker AVII500 with cryoprobe at 293 K. Chemical shifts are quoted in parts per million relative to the residual solvent peak. Mass spectra were obtained by using a Micromass LCT (ESMS) instrument or a MALDI Micro MX instrument. Electronic absorption spectra were recorded on a PG instruments T60U spectrometer.
7
Characterization of Organic Compounds by TLC, NMR, and MS
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Thin layer chromatography (TLC) was performed on aluminium sheets coated with 60 F254 silica. All solvents are used anhydrous unless stated otherwise. NMR spectra were recorded on Bruker AV400 (400 MHz), Bruker AVII 500 (500 MHz) or AVIIIHD 600 (600 MHz) instruments in the deuterated solvent stated. All chemical shifts (δ) are quoted in ppm and coupling constants (J), which are not averaged, in Hz. Residual signals from the solvents were used as an internal reference using the stated deuterated solvent. Infrared spectra were recorded on a Perkin-Elmer 1750 IR Fourier Transform spectrophotometer using thin films on a diamond ATR surface (thin film). Only the characteristic peaks are quoted. Melting points were determined using a Stanford Research Systems EZ-Melt. Low resolution mass spectra (m/z) were recorded on an Agilent 6120 spectrometer and high resolution mass spectra (HRMS m/z) on a Bruker microTOF mass analyzer using electrospray ionization (ESI). Compounds were synthesised from commercially available starting materials, and fully characterised by Infrared (IR) Spectroscopy, Mass Spectrometry (ESI-MS, HRMS-ESI) and Nuclear Magnetic Resonance (1H and 13C NMR). Spectra supporting the synthesis of these compounds are provided in the S1 File .
8
Synthesis and Characterization of Organometallic Complexes
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All manipulations were carried out using standard Schlenk line or dry-box techniques under an atmosphere of argon. Solvents were degassed by sparging with argon and dried by passing through a column of the appropriate drying agent using a commercially available Braun SPS. NMR spectra were measured in C6D6 or CDCl3 which were dried over potassium or molecular sieves, respectively, and stored under argon in a Teflon valve ampoule. NMR samples were prepared under argon in 5 mm Wilmad 507-PP tubes fitted with J. Young Teflon valves. NMR spectra were measured on Varian Mercury-VX-300 or Bruker AVII-500 spectrometers; 1 H and 13 C NMR spectra were referenced internally to residual protio-solvent ( 1 H) or solvent ( 13 C) resonances and are reported relative to tetramethylsilane (δ = 0 ppm). 7 Li, 27 Al and 119 Sn NMR spectra were referenced with respect to LiCl/D2O, Al(H2O)6 3+ and SnMe4, respectively. Chemical shifts are quoted in δ (ppm) and coupling constants in Hz. Elemental analyses were carried out at London Metropolitan University. The syntheses of MesNC(Cl)NEt2, MesNC(Me)NEt2, MesNC(CH2Ph)NEt2, DippNC(Cl)NMe2, DippNC(Me)-NMe2, 2 and 3 are described in the supporting information.
9
Synthesis of Germanium-Iron Organometallic Complex
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All reactions were performed under a nitrogen atmosphere by using Schlenk techniques. Toluene and thf were dried with sodium and pentane was dried with CaH 2 . All organic solvents were freshly distilled under nitrogen prior to use. Bruker DRX-250, ASX-300, AV-400 and AVII-500 spectrometers were used to obtain 1 H, 13 C, and 29 Si NMR spectra. 1 H, 13 C, and 29 Si chemical shifts δ are given in ppm and are referenced to Me 4 Si. NMR spectra were recorded at room temperature. KGe 9 (Hyp) 3 8 and BrFeCp(CO) 2 46 were synthesized via literature procedures.
Synthesis of [Ge 9 (Hyp) 3 FeCp(CO) 2 ] 1
In a round bottom flask with a magnetic stirrer BrFeCp(CO)
Synthesis of [Ge 9 (Hyp) 3 FeCp(CO) 2 ] 1
In a round bottom flask with a magnetic stirrer BrFeCp(CO)
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