The compounds EuCl3·6H2O (99.9%, Aldrich) and 4,4,5,5,6,6,6-heptafluoro-1-(2-thienyl)-1,3-hexanedione (hth) (Apollo Scientific), and the co-ligands dpso (97%, Aldrich), dpsoCH3 (97%, Aldrich), dpsoCl (97%, Aldrich), and tppo (>98%, Fluka) were used without further purification. The NMR spectra of the complexes, in CDCl3 (99.8%, Cambridge Isotope Labs) at 25 °C, were recorded on a Varian Mercury 400 MHz and on an Agilent DD2 500 MHz equipped with the OneNMR probe NMR spectrometers. The infrared spectra were recorded using a VERTEX 70v Bruker FT-IR spectrometer, examining powder samples in anhydrous KBr via diffuse reflection spectroscopy. Elemental analyses were carried out using a Thermo Scientific™ FLASH 2000 CHNS/O Analyzer at the Department of Chemical, Pharmaceutical and Agricultural Sciences, University of Ferrara.
Mercury 400 mhz
Manufactured by Agilent Technologies
The Mercury 400 MHz is a nuclear magnetic resonance (NMR) spectrometer designed for analytical applications. It provides a magnetic field strength of 400 MHz, enabling high-resolution analysis of chemical samples. The core function of the Mercury 400 MHz is to perform NMR spectroscopy, a widely used technique for structural elucidation and identification of organic compounds.
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Lab products found in correlation
Gemini 200 mhz, by Agilent Technologies (2 mentions)
Flash 2000 chns o analyzer, by Thermo Fisher Scientific (1 mentions)
Eucl3 6h2o, by Merck Group (1 mentions)
Cdcl3, by Cambridge Isotopes (1 mentions)
Dd2 500 mhz, by Agilent Technologies (1 mentions)
Alliance 2795, by Waters Corporation (1 mentions)
Safire plate reader, by Tecan (1 mentions)
2996 pda detector, by Waters Corporation (1 mentions)
Thermo nicolet nexus 6700, by Thermo Fisher Scientific (1 mentions)
Inova 600 mhz, by Agilent Technologies (1 mentions)
Zq 4000 mass spectrometer, by Waters Corporation (1 mentions)
Inova 300 mhz, by Agilent Technologies (1 mentions)
Vario micro cube elemental analyzer, by Elementar (1 mentions)
Tqd mass spectrometer, by Waters Corporation (1 mentions)
400 mhz spectrometer, by Agilent Technologies (1 mentions)
Mercury 300 mhz, by Agilent Technologies (1 mentions)
Hp 5ms column, by Agilent Technologies (1 mentions)
341 polarimeter, by PerkinElmer (1 mentions)
6890 series gc system, by Agilent Technologies (1 mentions)
Ultrashield 400 mhz, by Agilent Technologies (1 mentions)
12 protocols using mercury 400 mhz
1
Synthesis and Characterization of Eu(III) Complexes
2
Comprehensive Characterization of Polymer Properties
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1H NMR spectra were recorded
using an Agilent Mercury 400 MHz instrument. HPLC measurements were
carried out on an Alliance 2795 instrument equipped with a 2996 PDA
detector (Waters, Milford, MA, USA). Polymer morphology and size were
determined using a Zeiss EVO LS 10 (E) SEM (Carl Zeiss AG, Oberkochen,
Germany). Infrared spectra were recorded using a Thermo Nicolet Nexus
6700 instrument (Thermo Scientific, Waltham, MA, USA). UV absorbance
and fluorescence measurements were performed on a Safire plate reader
(Tecan Group Ltd., Männedorf, Switzerland) using a polystyrene
96-well microplate. Elemental analysis was performed at Nicolaus Copernicus
University in Toruń on a Vario MACRO 0000 (Elementar Analysensysteme
GmbH, Germany). Elemental analysis was performed at the Department
of Organic Chemistry, Johannes Gutenberg Universitat Mainz using a
Heraeus CHN-rapid analyzer (Hanau, Germany).
using an Agilent Mercury 400 MHz instrument. HPLC measurements were
carried out on an Alliance 2795 instrument equipped with a 2996 PDA
detector (Waters, Milford, MA, USA). Polymer morphology and size were
determined using a Zeiss EVO LS 10 (E) SEM (Carl Zeiss AG, Oberkochen,
Germany). Infrared spectra were recorded using a Thermo Nicolet Nexus
6700 instrument (Thermo Scientific, Waltham, MA, USA). UV absorbance
and fluorescence measurements were performed on a Safire plate reader
(Tecan Group Ltd., Männedorf, Switzerland) using a polystyrene
96-well microplate. Elemental analysis was performed at Nicolaus Copernicus
University in Toruń on a Vario MACRO 0000 (Elementar Analysensysteme
GmbH, Germany). Elemental analysis was performed at the Department
of Organic Chemistry, Johannes Gutenberg Universitat Mainz using a
Heraeus CHN-rapid analyzer (Hanau, Germany).
3
Synthesis of Cyclometalated Iridium(III) Precursor
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Analytical grade solvents and commercially available reagents were used as received unless otherwise stated. Chromatographic purifications were performed using 70-230 mesh silica gel. 1 H and 13 C NMR spectra were recorded on Varian Inova 300 MHz, Varian Mercury 400 MHz, Agilent 500 MHz or Inova 600 MHz spectrometers. Chemical shifts (δ) are reported in ppm relative to residual solvent signals for 1 H and 13 C NMR ( 1 H NMR: 7.26 ppm for CDCl 3 , 5.33 ppm for CD 2 Cl 2 ; 13 C NMR: 77.0 ppm for CDCl 3 , 53.84 ppm for CD 2 Cl 2 ). 13 C NMR spectra were acquired with the 1 H broadband decoupled mode. Coupling constants are given in Hz. The abbreviations used to indicate the multiplicity of signals are s, singlet; d, doublet; t, triplet; q, quartet; dd, double doublet; and m, multiplet. The high-resolution mass spectra (HRMS) were obtained with an ESI-QTOF (Agilent Technologies, model G6520A) instrument, and the m/z values are referred to as the monoisotopic mass. ESI-MS analyses were performed by direct injection of acetonitrile solutions of the compounds using a WATERS ZQ 4000 mass spectrometer.
The cyclometalated μ-dichloro-bridged iridium(III) precursor [Ir( ppy) 2 (µ-Cl)] 2 (Ir-dimer) was prepared following a reported procedure 33, 34 by refluxing the IrCl 3 •xH 2 O salt and the cyclo-metalating ligand Hppy = 2-phenylpyridine in a 2-ethoxyethanol/water mixture (3 : 1).
The cyclometalated μ-dichloro-bridged iridium(III) precursor [Ir( ppy) 2 (µ-Cl)] 2 (Ir-dimer) was prepared following a reported procedure 33, 34 by refluxing the IrCl 3 •xH 2 O salt and the cyclo-metalating ligand Hppy = 2-phenylpyridine in a 2-ethoxyethanol/water mixture (3 : 1).
4
Characterization of Organic Compounds
5
Quantitative NMR Analysis of Extracts
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The extracts were dried in vials to produce samples weighing about 6.0 ± 0.1 mg. Then, a solution of 300 μL of CD3OD with maleic acid at a concentration of 16.70 ± 0.01 mg/mL as internal standard was added. The final solutions (20.0 ± 0.3 mg/mL) were transferred to Shigemi 5 mm tubes for NMR measurement.
The samples were measured on a Varian Mercury 400 MHz at 23 °C, using a 45° pulse (pulse width = 4.65 μs), a relaxation delay of 1.0 s, an acquisition time of 4.5 s, and an accumulation of 32 scans. The free induction decay (FID) size was 32 k data points, with a spectral width of 5995.2 Hz. Chemical shifts are given in ppm to one decimal point, and the spectra were centered using the deuterated solvent.
The samples were measured on a Varian Mercury 400 MHz at 23 °C, using a 45° pulse (pulse width = 4.65 μs), a relaxation delay of 1.0 s, an acquisition time of 4.5 s, and an accumulation of 32 scans. The free induction decay (FID) size was 32 k data points, with a spectral width of 5995.2 Hz. Chemical shifts are given in ppm to one decimal point, and the spectra were centered using the deuterated solvent.
6
Synthesis and Purification of Bioactive Compounds
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Chemical reagents and solvents were obtained from commercial sources and were used without further purification. When necessary, solvents were dried and/or purified by standard methods. All reactions were monitored by thin-layer chromatography with preparative silica gel F254 plates purchased from Merck, Inc. Flash chromatography was performed using either a glass column packed with silica gel (200–300 mesh) or pre-packed silica gel cartridges by a combi-flash machine from Teledyne Isco. The purity of all target compounds assayed was identified by thin-layer chromatography (silica gel F254) and NMR spectra. In particular, the purity of the most active compounds, 2a, 2d and 3b, was further determined by HPLC (ESI† ). 1H-NMR spectra were recorded on Varian Mercury 300 MHz or 400 MHz spectrometer. 13C-NMR spectra were recorded on Varian Mercury 400 MHz or 500 MHz spectrometer. Chemical shifts are reported in parts per million (δ) relative to internal tetramethylsilane (TMS) standard. Coupling constants are given in hertz. All melting points were determined on Yanaco melting point apparatus. Mass spectra were taken in HR-ESI mode on Exactive Plus™ LC/MSD Orbitrap from Thermo Fisher Scientific. Reactions under microwave irradiation were performed in a Biotage Initiator microwave reactor in sealed vessels.
7
NMR and GC-MS Analysis of Reaction Products
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NMR spectra of products as well as the proportions of each product in the reaction mixture were recorded on Varian Gemini 200 MHz and Varian Mercury 400 MHz (1H-NMR), and 50 and 100 MHz (13C-NMR) spectrometers, using CDCl3 as a solvent and tretramethylsilane (TMS) as an internal standard. The proportions of each product in the reaction mixture were determine by Gas Chromatography-Mass Spectrometry on an Agilent GC system 6890 series coupled to an Agilent mass selective detector 5973N with an HP-5MS column length of 30 m, internal size of 0.25 mm, film thickness of 0.25 μm, split ration of 5:1, 40 °C min−1, 5 °C min−1 to 250 °C min−1, 10 °C min−1 to 280 °C min−1. Retention times (min): 4 = 25.3, 3 = 28, and 5 = 43. Enantiomeric excesses were measured by an HPLC Dionex Ultimate 3000 model and UV Shodex detector RI-101 model at 210 nm, using a Chiracel® OD-H column (5 × 250 mm), hexane/i-PrOH 98/2 (v/v) as eluent at a flow rate of 0.8 mL min−1 at 25 °C for 4 . Retention times: (R)-4 : 11 min, (S)-4 : 13 min. A CHIRALPAK® AS-H column (5 × 250 mm) was used for 5 , with hexane/i-PrOH 80/20 (v/v) as eluent at a flow rate of 1 mL min−1 at 25 °C. Retention times: (S)-5 : 20 min, (R)-5 : 29 min. Optical rotations were measured by means of a Perkin-Elmer 341 polarimeter.
8
Comprehensive Characterization of Reaction Products
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NMR spectra of products as well as the proportions of each product in the reaction mixture were recorded on Varian Gemini at 200 MHz and Varian Mercury 400 MHz (1H-NMR), and 50 and 100 MHz (13C-NMR) spectrometers, using CDCl3 as a solvent and tretramethylsilane (TMS) as an internal standard. A mass spectrometric analysis was performed using an Agilent 6530 quadrupole time-of-flight (QTOF) LCMS with an electrospray ionization (ESI) source (Agilent Technologies, Santa Clara, CA, USA). A mass spectrometry analysis was conducted in positive ion mode, set for a detection of mass-to-charge ratio (m/z) of 100–1000. The X-ray structures were obtained using an APEX-Bruker apparatus.
9
NMR Characterization of HRas-Ligand Binding
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For the experiments with the free ligand, cmp4 was dissolved in a [D11]-Tris buffer at pH = 7.3, 5 mM MgCl2. COSY and HSQC experiments were performed by using the standard sequences. For the binding experiments, wild type or G13D mutated HRas was dissolved in 500 μL of the same [D11]-Tris buffer, containing an amount of GDP equimolar to the protein, and transferred into a 5 mm NMR tube; 50 μL of the ligand solution dissolved in the same buffer were added slowly. Final protein concentration was 50 µM, final ligand concentration was 1 mM.
STD experiments were performed without saturation of the residual HDO signal and with spin-lock to avoid the presence of protein resonances in the spectra. A train of Gaussian-shaped pulses of 50 ms each was employed, with a total saturation time of the protein envelope of 2 s. An off-resonance frequency of δ = 40 ppm and on-resonance frequency δ = −1.5 ppm (protein aliphatic signals region) were applied. Spectra were acquired with a Varian Mercury 400 MHz instrument and processed using the program Mestre-Nova 9.
STD experiments were performed without saturation of the residual HDO signal and with spin-lock to avoid the presence of protein resonances in the spectra. A train of Gaussian-shaped pulses of 50 ms each was employed, with a total saturation time of the protein envelope of 2 s. An off-resonance frequency of δ = 40 ppm and on-resonance frequency δ = −1.5 ppm (protein aliphatic signals region) were applied. Spectra were acquired with a Varian Mercury 400 MHz instrument and processed using the program Mestre-Nova 9.
10
NMR and LC/MS Compound Characterization
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NMR measurements
for characterization of the compounds were performed
using either a Bruker UltraShield 400 MHz or a Varian Mercury 400
MHz spectrometer using 400 MHz for 1H and 100 MHz for 13C measurements. Proton and carbon chemical shifts were documented
in parts per million (ppm) downfield from trimethylsilane (TMS), using
the resonance frequency of the deuterated solvent as the internal
standard. Abbreviations reported for the multiplets are s: singlet;
t: triplet; and m: multiplet. Liquid chromatography/mass spectrometry
(LC/MS) measurements were performed on a system using Shimadzu LC-10AD
VP liquid chromatography pumps equipped with an Alltima C18 3 μm
(50 mm × 2.1 mm) reversed-phase column, a diode array detector
(Thermo Finnigan Surveyor PDA Plus detector), and an Ion-Trap (Thermo
Scientific LCQ Fleet). This system used a water–acetonitrile
mobile phase enriched with 0.1% v/v formic acid.
for characterization of the compounds were performed
using either a Bruker UltraShield 400 MHz or a Varian Mercury 400
MHz spectrometer using 400 MHz for 1H and 100 MHz for 13C measurements. Proton and carbon chemical shifts were documented
in parts per million (ppm) downfield from trimethylsilane (TMS), using
the resonance frequency of the deuterated solvent as the internal
standard. Abbreviations reported for the multiplets are s: singlet;
t: triplet; and m: multiplet. Liquid chromatography/mass spectrometry
(LC/MS) measurements were performed on a system using Shimadzu LC-10AD
VP liquid chromatography pumps equipped with an Alltima C18 3 μm
(50 mm × 2.1 mm) reversed-phase column, a diode array detector
(Thermo Finnigan Surveyor PDA Plus detector), and an Ion-Trap (Thermo
Scientific LCQ Fleet). This system used a water–acetonitrile
mobile phase enriched with 0.1% v/v formic acid.
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