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21 protocols using 240c analyzer

1

Characterization of Luminescent Compounds

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All reagents were purchased from commercial suppliers and used as received. High-resolution ESI (HR-ESI) mass spectrometry spectra were acquired on a Thermo Scientific Q Exactive Mass Spectrometer. Elemental analysis was performed on a PerkinElmer 240C analyzer. The samples were dried under vacuum at 50 °C for 24 h to remove solvated molecules prior to elemental analysis. The 1H and 13C NMR spectra were obtained on a Bruker DRX-400 spectrometer. Coupling constants are given in hertz. UV-vis spectra were measured on a UV-3600 spectrophotometer. Photoluminescence (PL) spectra were measured with the Hitachi F-4600 PL spectrophotometerex = 420 nm). Circular dichroism (CD) spectra in CH2Cl2 solution were recorded on a Jasco J-810 spectropolarimeter at a scan rate of 100 nm min−1 and a resolution of 1 nm at room temperature. CPL spectra were recorded using a circularly polarizer on a Jasco CPL-300 spectrophotometer at a scan rate of 100 nm min−1 and a resolution of 1 nm at room temperature.
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2

Synthesis of Buprenorphine Derivatives

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Reagents and solvents
were purchased
from Sigma-Aldrich or Alfa Aesar and used as received. Buprenorphine
(1a) was supplied by the National Institute on Drug Abuse,
Bethesda, Maryland. 1H and 13C NMR spectra were
obtained with a Bruker 400 MHz instrument (1H at 400 MHz, 13C at 100 MHz); δ is given in ppm, J, in Hz, with TMS as an internal standard. ESIMS: microTOF (BRUKER),
EIMS: Fisons Autosampler. Microanalysis: PerkinElmer 240C analyzer.
Column chromatography was performed using RediSep prepacked columns
with a Teledyne Isco CombiFlash instrument. Most ligands were tested
as their hydrochloride salts, prepared by adding 5 equiv of HCl (1
N solution in diethyl ether) to a solution of compound in anhydrous
methanol. Alternatively, the oxalate salt was formed by adding 1 equiv
of oxalic acid in EtOH to the ligand in EtOH. All reactions were carried
out under an inert atmosphere of nitrogen unless otherwise indicated.
All compounds were >95% pure, as determined by microanalysis. A
representative
synthesis is reported here.
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3

Characterization of Novel Compounds

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All the chemical reagents are analytical grade or prepared by our lab. Melting points were measured using an X-4 apparatus and were uncorrected. 1H NMR spectra were recorded on a Bruker Avance 500 MHz spectrometer using DMSO-d6 as solvent. 13C NMR and 19F NMR spectra were recorded on a Bruker Avance 600 MHz spectrometer using DMSO-d6 as solvent. Mass spectra were determined on a Thermo Finnigan LCQ Advantage LC/mass detector instrument. Elemental analysis data of title compounds were collected by a Perkin-Elmer 240C analyzer. CEM Discover Focused Synthesizer was used to carry out the microwave reaction (600 W, 2450 MHz).
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4

Spectroscopic Analysis of Compounds

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All of the chemicals purchased were analytical reagent grade and were utilized exactly as received. On a Bruker AM 400 spectrometer using DMSO (d6) as a solvent, 1H NMR (400 MHz) spectra were recorded. The mass spectra were recorded using a PerkinElmer PE Sciex API/65 LC-MS apparatus. A PerkinElmer type 240C analyzer was used to examine the elements (C, H, and N). A Koffler device was used to determine the melting point.
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5

Analytical Characterization of Novel Compounds

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Most of the chemicals and reagents used in the investigation came from Merck Chemicals in Bangalore, India. Compound melting points measured with the Hicon melting point device (New Delhi, India) were found to be inaccurate and to have exposed capillary tubes. Thin-layer chromatography (TLC) plates fixed with silica gel G were employed to assess how pure the newly produced chemicals were. As a detection toolkit, UV light and iodine fumes were employed. A Fourier-transform infrared spectroscopy (FT-IR) spectrophotometer from Shimadzu was utilized to get the FT-IR spectra. DRX400 series of Nuclear Magnetic Resonance (NMR) spectrometer (Bruker, US) was used to acquire the IH spectra (at 400 MHz) and 13C spectra (at 100 MHz). Tetrmethylsilane (TMS) was used as a comparative internal standard, and chemical changes (δ) are expressed in parts per million (ppm), while J values (coupling constants) are expressed in hertz (Hz). The mass of the developed chemical was measured using a mass spectrometer (Applied Biosystems; API-3000), and the result is given in daltons. C, H, and N elemental analysis of synthetic derivatives was performed using a Perkin-Elmer (240C analyzer) (PerkinElmer, US).
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6

Purification and Characterization of Organic Compounds

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Reagents and solvents were purchased from Sigma-Aldrich or Alfa Aesar and used as received. 1H and 13C NMR spectra were obtained with a Brucker-400-MHz instrument (1H at 400 MHz, 13C at 100 MHz); δ in ppm, J in Hz with TMS as an internal standard. ESIMS: microTOF (BRUKER). Microanalysis: Perkin-Elmer 240C analyzer. Column Chromatography was performed using pre-packed column in combi flash instrument. Ligands were tested as their hydrochloride salts, prepared by adding 5 equivalent of HCl (1 N solution in diethyl ether) in a solution of compound in anhydrous methanol. All reactions were carried out under an inert atmosphere of nitrogen unless otherwise indicated. All compounds were >95% pure.
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7

Characterization of Coordination Complexes

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Elemental analyses were performed on a PerkinElmer 240C analyzer. The UV–Vis spectra were applied on a Puxi Tu-1901 spectrophotometer. The luminescence curves were recorded on a Hitachi F-7000 Fluorescence spectrometer. IR curves were collected on an ABB Bomen MB 102 series FT−IR spectrometer. The ESR spectra were measured on CIQTEK EPR200-Plus with a continues-wave X band frequency of 9.84 GHz for H2ADC ligand, and a Bruker E500 spectrometer with continues-wave X band frequencies of 9.84 GHz at room temperature and 9.41 GHz at low temperatures for 1 and 2. Magnetic measurements of the polycrystalline samples were carried out on a Quantum Design SQUID PPMS magnetometer. PXRD curves were performed on a Rigaku diffractometer with a Cu-target tube and a graphite monochromator. Simulation of the PXRD curves were performed by the single-crystal data and diffraction-crystal module of the Mercury (Hg) program available free of charge via the Internet at http://www.iucr.org. Furthermore, a Rietveld refinement of PXRD between the experimental pattern and the single crystal data were also performed. For the light irradiation experiments, a Perfect Light PLS-SXE 300 Xe-lamp (320–780 nm, 250 W, at least 180 min) was equipped to prepare the colored samples of 1 and 2 for elemental analyses, IR, crystal XRD, UV–Vis, PXRD, ESR and magnetic studies.
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8

Comprehensive Spectroscopic Characterization of Compounds

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Elemental analyses for C, H, N, and S were performed on Perkin-Elmer 240C analyzer. FT-IR data were recorded on Vector27 Bruker Spectrophotometer with KBr pellets in the 4000–400 cm−1 region. TGA data were obtained on an STA 449C thermal analysis system with a heating rate of 10 °C min−1 under N2 atmosphere. The PXRD were collected with a scan speed of 0.1 s deg−1 on a Bruker Advance D8 (40 kV, 40 mA) diffractometer with Cu radiation (λ = 1.54056 Å) at room temperature. Calculated PXRD patterns were generated using Mercury 3.0. Magnetic susceptibility measurements were performed using a Quantum Design SQUID VSM magnetometer on microcrystalline samples for all compounds. EPR spectra were obtained by using a Bruker EMX-10/12 variable-temperature apparatus at 110 K. Gas sorption measurements were conducted using a Micrometritics ASAP 2020 system. See Supplementary Methods for details.
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9

NMR Characterization of Imidazole-2-ylidene Silver(I) Complexes

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Reagents and solvents. All chemicals were commercially available (TCI chemicals) and were used as received unless stated otherwise. The solvents were dried and distilled before use. NMR Analysis: the NMR spectra were recorded on Bruker Advance 300, 400, and 600 MHz spectrometers at 25 °C. The 1H and 13C NMR chemical shifts are referenced to SiMe4 (δ=0 ppm) using the residual proton impurities of the deuterated solvents as internal standards. 1H NMR spectra are referenced using the residual solvent peak δ 7.27 for CDCl3, δ 5.32 for CD2Cl2, and δ 2.50 for DMSO‐d6. 13C NMR spectra are referenced using the residual solvent peak at δ 77.23 for CDCl3, δ 54.00 for CD2Cl2, and δ 39.51 for DMSO‐d6. Chemical shifts (δ) are expressed as parts per million. Multiplicities are abbreviated as follows: singlet (s), doublet (d), triplet (t), quartet (q), multiplet (m), and broad (br). Elemental analysis was recorded on a with a PERKIN‐Elmer 240‐C analyzer.
The complexes [N‐methyl,N’‐[(2‐sodiumalcholate‐2‐phenyl)ethyl])‐imidazole‐2‐ylidine]silver(I)] iodide (1) and [N‐methyl,N’‐(2‐metoxy‐2‐phenyl) ethyl‐imidazole‐2‐ylidene silver(I)] iodide (3) were obtained following the procedure reported in rif..[20]
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10

Characterization of Metal-Organic Frameworks

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All solvents and reagents for synthesis were of reagent grade quality, bought from commercial sources and used as received. PXRD patterns were collected on a D2 PHASER A26-X1 XRD diffractometer. The IR spectra (4000–400 cm−1) were obtained from KBr pellets with an FTIR Nexus spectrophotometer. Elemental analyses were performed on a PerkinElmer 240 C analyzer. Thermogravimetric analysis (TGA) curves were measured under air atmosphere at a heating rate of 10 °C min−1 on a PerkinElmer TG-7 thermal analyzer. The fluorescence spectra were recorded on a HITACHI F-7000 Spectrometer.12 (link) ECL signals were monitored and recorded by an MPI-B ECL analyzer (Xi'an Remax Electronic Science and Technology Co. Ltd, Xi'an, China, with the voltage of the photomultiplier tube set at 600 V and the potential scan from −0.8 to 0.8 V at a scanning rate of 0.1 V s−1. UV-vis adsorption spectra were collected on a Cary 300 spectrophotometer. CO2 and CH4 adsorption measurements (up to 1 bar) were carried out on an Autosorb-3.0 (Quantachrome) volumetric analyzer.13 (link)
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