The elemental composition of the synthesized CTCs were analyzed using a Perkin-Elmer 2400CHN Elemental Analyzer to determine their hydrogen, carbon, and nitrogen content (%). The NMR (1H and 13C), FTIR, and UV–visible spectra of the synthesized CTCs were registered with Bruker DRX-250 Digital FT-NMR, Shimadzu FTIR, and Perkin − Elmer Lambda 25 UV/Vis spectrophotometers, respectively, at room temperature. The electronic spectra were collected from the CTCs solubilized in methanol from 200 to 800 nm, while solid-state CTCs were used to collect FTIR spectra in the 400 to 4000 cm−1 range. At 400 MHz, the Bruker DRX-250 instrument generated the 1H and 13C NMR spectra of the solid-state CTCs in DMSO‑d6 solution, where the chemical shift values are presented in δ scale relative to the internal reference tetramethylsilane (TMS).
Drx 250
Manufactured by Bruker
Sourced in Germany
The DRX-250 is a nuclear magnetic resonance (NMR) spectrometer designed for routine analysis and characterization of chemical compounds. It operates at a proton resonance frequency of 250 MHz and is capable of acquiring high-resolution NMR spectra.
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5 protocols using drx 250
1
Characterization of Synthesized Charge Transfer Complexes
2
Nuclear Magnetic Resonance and Mass Spectrometry Analysis
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1H- and 13C-NMR spectra were recorded on a Bruker DRX-250, a Inova-400 and a DD-500 spectrometers. Sample concentrations were about 10% (w/v) in CDCl3 or DMSO-d6 and the J values are given in Hz. The mass spectral analyses were performed on an Aligent Technologies 6540 UHD Accurate-Mass Q-TOF LC/MS. The clog P values were calculated using ChemDraw Professional, Version 15.1.0.144.
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1H- and 13C-NMR spectra were recorded on a Bruker DRX-250, a Inova-400 and a DD-500 spectrometers. Sample concentrations were about 10% (w/v) in CDCl3 or DMSO-d6 and the J values are given in Hz. The mass spectral analyses were performed on an Aligent Technologies 6540 UHD Accurate-Mass Q-TOF LC/MS. The clog P values were calculated using ChemDraw Professional, Version 15.1.0.144.
3
Spectroscopic Characterization of Organic Compounds
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Melting points (m.p.) were determined on a Boetius hot-stage microscope. 1H and 13C NMR spectra were obtained with a Bruker DRX250, Bruker DRX400, and DRX 500 spectrometer (Bruker BioSpin GmbH, Rheinstetten, Germany) in CDCl3 or acetone-d6 as solvent. Chemical shifts were reported in parts per million (ppm, δ) relative to the solvent peak (7.26 ppm for 1H; 77.16 ppm for 13C). Coupling constants (J) were measured in Hertz (Hz). Elemental analyses (C, H, N) were carried out by a Vario III microanalyzer. The results obtained were within 0.4% of theoretical values. Thin-layer chromatography (TLC) was carried out on silica gel plates (Kieselgel 60 F254). Flash column chromatography was performed with Merck 60 silica gel (0.040–0.063 mm).
4
Characterization of Deep Eutectic Solvents
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All reagents were purchased from the chemical companies Merck or Sigma Aldrich and used as received. Thin layer chromatography (TLC) was performed on silica gel 60 F-254 [Merck, Germany]. NMR was recorded on a Bruker DRX-250 using DMSO-d6 as solvent. FT-IR (KBr) spectra were recorded using an Alpha Perkin Elmer spectrophotometer. Melting points were determined using a Stuart melting point meter. Thermo-Gravimetric-Differential Thermal Analysis (TGA–DTA) was performed using the SDT Q600 V20.9 Build 20 device. The density of the DES catalyst was determined using AND-HR200.
5
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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