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Avance 400

Manufactured by JEOL

The AVANCE 400 is a nuclear magnetic resonance (NMR) spectrometer designed for laboratory applications. It provides high-resolution analysis of chemical samples. The AVANCE 400 operates at a frequency of 400 MHz and is capable of performing various NMR experiments for structure elucidation and analysis of organic and inorganic compounds.

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4 protocols using avance 400

1

Comprehensive Spectroscopic Characterization

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1H, 13C and 19F NMR spectra were recorded at 400 MHz (100 MHz) or 500 MHz (125 MHz) using either Bruker AVANCE-400 or JEOL JNM-ECZR-500 NMR spectrometers, respectively. Chemical shifts are reported in ppm and referenced to residual NMR solvent peaks (1H NMR: δ 3.62 ppm for THF, δ 7.26 ppm for CDCl3; 13C NMR: δ 77.2 ppm for CDCl3). High-resolution mass spectra were determined with a Bruker Daltonics APEXIV 4.7 Tesla FT–ICR–MS using ESI or DART ionization. The MALDI-MS spectra were acquired in linear and reflection modes in the Koch Institute at MIT using a Bruker Microflex MALDI-MS spectrometer. UV–Vis absorption spectra were measured using an Agilent Cary 4000 Series UV–Vis spectrophotometer. Gel permeation chromatography (GPC) measurements were performed in tetrahydrofuran using an Agilent 1260 Infinity system and calibrated with a polystyrene standard. ATR–FTIR spectra were acquired using a Thermo Scientific Nicolet 6700 FT–IR with either a Ge or ZnSE crystal for ATR and subjected to the ‘atmospheric suppression’ correction in OMNIC™ Spectra software. Raman spectra were collected with excitation at 633 nm laser using a Horiba LabRAM HR800 Raman spectrometer.
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2

Microwave-Assisted Organic Synthesis Protocols

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Microwave assisted reactions were performed using a CEM Discover BenchMate. Reaction completions were monitored on E. Merck silica gel F254 TLC plates. Purification of the synthesized compounds was performed by flash column chromatography using Merck Silica Gel 60 (230–400 mesh). The synthesized compounds were characterized by an 1H NMR on Bruker AVANCE 400 (1H: 400 MHz) and JEOL ECA 500 (1H: 500 MHz) spectrometers and their chemical shift δ values were measured in ppm with TMS as a standard reference. Mass spectra were obtained using a Waters ACQUITY UPLC, Micromass Quattro microTM API.
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3

Biophysical Characterization of Molecular Interactions

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The experiments were performed following the methods reported in the literature.11 Fluorescence spectra were recorded on a Hitachi High-Tech F7000 spectrometer equipped with a thermostatic cell holder and a stirrer, UV-vis spectra were recorded on a JASCO V-670 spectrophotometer equipped with a JASCO ETC-717 temperature controller, and NMR spectra were recorded on a Bruker AVANCE 400 (400 MHz for 1H) or JEOL ECA-600 (600 MHz for 1H) spectrometer. ITC analysis was performed using a GE Healthcare MicroCal iTC200 microcalorimeter.
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4

Synthesis and Characterization of Novel Organometallic Compounds

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General consideration: All manipulations, unless otherwise stated, were carried out by using standard Schlenk and glovebox techniques under an atmosphere of high purity argon. The chemicals were purchased from commercial sources: Sigma-Aldrich, and Alfa Aesar and were used as received. Toluene and hexane were dried using a MBraun Solvent Purification System.
Benzene-d6, THF and THF-d8 were dried and distilled over molten potassium. CD2Cl2 was dried and distilled over calcium hydride. All NMR spectra were recorded on Bruker Avance 400 or Jeol ECA 400 MHz spectrometers. The NMR spectra were recorded in d-solvents and the chemical shifts are relative to SiMe4 for 1 H, 13 C and 29 Si; BF3 . Et2O for 11 B. Compound 1 and [LSiCl] (L = PhC(NtBu)2) were synthesized according to literature procedures.
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