Melting points were determined using an Electrothermal 9100 apparatus at Kleinfeld in Gehrden, Germany. The 1H NMR and 13C NMR spectra were obtained using a Bruker AC 300 P (1H NMR: 300 MHz, 13C NMR: 75 MHz; Bruker, Rheinstetten, Germany) in DMSO‑d6, with TMS as the internal reference. The chemical shifts are expressed in δ (ppm) values. The 13C multiplicities were determined using DEPT and off-resonance pulse sequences. X-ray data [27 ,28 ] were collected with a Bruker Nonius Kappa diffractometer at Bruker in Rheinstetten, Germany, and corrected using SADABS factors and empirical absorption. The FTIR spectra (KBr) were recorded on a Nicolet 205 spectrophotometer manufactured by Nicolet in Madison, WI, USA. The graphic representation of the structure utilized the program SCHAKAL 99 [29 ]. X-ray crystallography was conducted in the Microanalytical laboratory of the Fakultät für Chemie und Chemische Biologie at TU Dortmund, Germany. The spectral and elemental analyses were carried out in the Microanalytical Center at Cairo University in Cairo, Egypt.
Ac 300 p
Manufactured by Bruker
Sourced in Germany
The AC 300 P is a nuclear magnetic resonance (NMR) spectrometer manufactured by Bruker. It is designed to analyze the composition and structure of chemical samples through the application of magnetic fields and radio waves. The core function of the AC 300 P is to generate detailed, high-resolution spectra that can be used to identify and quantify the compounds present in a given sample.
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5 protocols using ac 300 p
1
Melting Point and Spectroscopic Analysis
2
Nuclear Magnetic Resonance Characterization
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For routine characterization of the synthesized IL samples or intermediate compounds, the specimens were dissolved in CDCl3. 1H (300 MHz) and 13C (75 MHz) spectra were recorded on a Bruker AC 300 P, and 19F (282 MHz) spectra on a Bruker AV III 600 spectrometer at room temperature. For the investigations related to the behavior of Na12Ge17 or the oxidation of that phase, IL samples were investigated without solvent, because any possible reaction with, e. g., CDCl3 was to be excluded. In an argon glovebox, the IL specimens were filled into NMR sample tubes, a sealed capillary containing DMSO(D6) was inserted, providing a small detectable signal for spectrum calibration, and the tube was sealed air‐tight afterwards. 1H (300 MHz) spectra were likewise recorded on the Bruker AC 300 P spectrometer, 23Na (159 MHz) spectra were recorded on the Bruker AV III 600 spectrometer. 1H and 13C NMR spectra were referenced internally by using the solvent residual signal of CDCl3 (1H: 7.26 ppm, 13C: 77 ppm) and (CD3)2SO (1H: 2.50 ppm, 13C: 39.5 ppm), respectively, while 19F and 23Na NMR spectra were referenced by external device standards.
3
Comprehensive Analytical Characterization of Chemical Compounds
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All solvents were analytical grade. TLC: Merck silica gel 60 F254. CC: silica gel 60, 70–230 mesh ASTM. IR spectra: Shimadzu-FTIR 8400S infrared spectrophotometer, in cm-1. 1H and 13C NMR: Bruker AC 300P operating at 300.13 and 75 MHz respectively; compound purity was evaluated by HPLC analysis: Shimadzu LC-10AD; RID detector; column, Macherey-Nagel 250/4 Nucleosil 100-5; flow, 0.8 mL/min; T, 35 °C; all solvents were HPLC grade; tR in min. Mp: Mettler-FP-61 apparatus (uncorrected). HR mass spectra were recorded with a Micromass Q-TOF micro mass spectrometer (Waters). FIA-MS experiments were performed on a linear ion trap mass spectrometer (LXQ Thermo Finningan) equipped with a heated electrospray ionization (HESI) source. Operating conditions of the HESI were as follows: source temperature: 50 °C; ion spray voltage = +4.0 kV; sheath gas = 5 (arbitrary scale); capillary temperature = 275 °C. Methanolic solutions of samples (1 × 10−5 M) were infused via a syringe pump at a flow rate of 3–5 μL/min. Unless otherwise specified, all organic solutions were dried over anhydrous Na2SO4 and evaporated to dryness under reduced pressure.
4
NMR Spectroscopy and Elemental Analysis
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1H and 13C NMR spectra were obtained on a Bruker AC 300 P (1H: 300.1 MHz, 13C: 75.5 MHz, 19F: 282.4 MHz) or a Bruker DRX 500 (1H: 500.1 MHz, 13C: 125.8 MHz, 19F: 470.3 MHz) spectrometer at 298 K. Elemental analyses were performed by the microanalytical laboratory of our institute using an EuroVektor Euro EA-300 Elemental Analyzer. Chemicals were supplied by Acros, Fluka and Aldrich and used as received; solvents were dried by standard procedures before use. Imidazolium salts 1 –4 [34 (link)], silver complexes 5 –8 [27 (link)], chloro(methyl)(cyclooctadiene)palladium(II) [54 (link)] and dimethyl-(N,N,N',N'-tetramethyl-1,2-ethylendiamine)palladium(II) [38 (link)] were prepared according to literature procedures.
5
NMR Spectroscopic Analysis of Isolated Compounds
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Most NMR spectra were obtained using a Bruker Advance III spectrometer operating at 500 MHz for protons. Only spectra of compounds 13-15 were obtained in a Bruker AC-300P operating at 300 MHz for protons. For 1 H and 13 C NMR spectra obtained with the equipment operating at 500 MHz for protons, acquisition parameters were described previously (Zamora, Aguilar, Granvogl, & Hidalgo, 2016) . All experiments were performed at 24 ºC and 2D experiments (COSY, HMQC, and HMBC) were carried out to determine the chemical structures of the isolated compounds.
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