All manipulations were carried out using standard Schlenk line or dry‐box techniques under an atmosphere of argon or dinitrogen. Solvents were degassed by sparging with argon and dried by passing through a column of the appropriate drying agent. NMR spectra were measured in [D6]benzene (which was dried over potassium), with the solvent then being distilled under reduced pressure and stored under argon in Teflon valve ampoules. NMR samples were prepared under argon in 5 mm Wilmad 507‐PP tubes fitted with J. Young Teflon valves. 1H, 31P{1H}, 13C{1H}, 11B{1H}, 19F{1H} NMR spectra were measured on a Bruker Avance III HD nanobay 400 MHz or Bruker Avance 500 MHz spectrometer at ambient temperature and referenced internally to residual protio‐solvent (1H) or solvent (13C) resonances and are reported relative to tetramethylsilane (δ=0 ppm). Assignments were confirmed using two‐dimensional 1H‐1H and 13C‐1H NMR correlation experiments. Chemical shifts are quoted in δ (ppm) and coupling constants in Hz. Elemental analyses were carried out by Elemental Microanalysis Ltd, Okehampton, Devon, UK. Compound 1 ,[15] B(C6F5)3[23] and KCH2Ph[24] were prepared by literature methods. All other reagents were used as received. The synthetic and characterizing data for H(PON) (2 ) and (PON)GaI2 are included in the Supporting Information.
Avance 3 hd nanobay 400 mhz
Manufactured by Bruker
The Avance III HD NanoBay 400 MHz is a compact and high-performance nuclear magnetic resonance (NMR) spectrometer. It is designed to provide reliable and accurate measurements of chemical compounds and materials. The core function of this product is to facilitate the analysis and identification of samples through the detection and interpretation of their NMR signals.
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Lab products found in correlation
507 pp tubes, by Wilmad (2 mentions)
Avance 500 mhz spectrometer, by Bruker (2 mentions)
Silica gel 60 f254, by Merck Group (1 mentions)
Avance dpx 400 mhz, by Bruker (1 mentions)
Qexactive plus orbitrap instrument, by Thermo Fisher Scientific (1 mentions)
Nicolet is5 ftir spectrometer, by Thermo Fisher Scientific (1 mentions)
Silica gel, by Thermo Fisher Scientific (1 mentions)
Drx 600 nmr spectrometer, by Bruker (1 mentions)
Chiralpak ig, by Daicel (1 mentions)
Potassium perchlorate, by Thermo Fisher Scientific (1 mentions)
Cesium perchlorate, by Merck Group (1 mentions)
Avance 3 500 mhz, by Bruker (1 mentions)
Avc 500 spectrometer, by Bruker (1 mentions)
6 protocols using avance 3 hd nanobay 400 mhz
1
Synthesis and Characterization of H(PON) and (PON)GaI2
2
Synthesis and Characterization of Organic Compounds
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All reagents were purchased from Sigma-Aldrich and used without further purification. Dichloromethane (DCM) and tetrahydrofuran (THF) were distilled from calcium hydride. All reactions were conducted in flame-dried glassware and under nitrogen atmosphere unless stated otherwise. All reactions were magnetically stirred and monitored by thin-layer chromatography (TLC) using Merck silica gel 60 F254 pre-coated plates (0.25 mm). Flash column chromatography was performed using silica gel (0.032–0.063 mm particle size) from Fisher Scientific. All 1H-, 13C- and 2D-NMR experiments were performed on either a Bruker Avance DPX 400 MHz, Bruker Avance III HD NanoBay 400 MHz or DRX600 NMR spectrometer equipped with a TXI (5 mm) cryoprobe. Chemical shifts were reported in ppm using residual CDCl3 (δH; 7.26 ppm, δC; 77.36 ppm), or (CD3)2CO (δH; 2.05 ppm, δC; 29.84 ppm), or CD3OD (δH; 3.31 ppm, δC; 49.00 ppm) as an internal reference. Polarimetry data was collected on a JASCO polarimeter (model no. P-1010). LC–MS was conducted using an Agilent 6130 single-quadrupole LC–MS system. High-resolution mass-spectrometry (HRMS) was conducted using a Thermo-Fisher QExactive-Plus Orbitrap instrument. Infrared spectroscopy was conducted using a Thermo-Fisher Nicolet iS5 FT–IR spectrometer.
3
Air-Sensitive Organometallic Compound Characterization
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All manipulations were carried out using standard Schlenk line or dry-box techniques under an atmosphere of argon or dinitrogen. Solvents were degassed by sparging with argon and dried by passing through a column of the appropriate drying agent. NMR spectra were measured in benzene-d6 (which was dried over potassium), with the solvent then being distilled under reduced pressure and stored under argon in Teflon valve ampoules. NMR samples were prepared under argon in 5 mm Wilmad 507-PP tubes fitted with J. Young Teflon valves. 1H, 13C{1H}, 11B{1H}, 19F{1H} NMR spectra were recorded on Bruker Avance III HD nanobay 400 MHz or Bruker Avance 500 MHz spectrometer at ambient temperature and referenced internally to residual protio-solvent (1H) or solvent (13C) resonances and are reported relative to tetramethylsilane (δ = 0 ppm). 19F resonances are referenced externally to CFCl3. Assignments were confirmed using two-dimensional 1H–1H and 13C–1H NMR correlation experiments. Chemical shifts are quoted in δ (ppm) and coupling constants in Hz. Elemental analyses were carried out by London Metropolitan University. (HCDippN)2BBr was prepared by the literature method (see Supplementary Information S1). All other reagents were used as received.
4
Separation and Characterization of Chiral Compounds
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Starting materials were purchased from Sigma-Aldrich unless otherwise noted. Compounds [Bu4N][1], [Na][1], and 2 were prepared as reported in the literature. Lithium perchlorate (Fluka), sodium perchlorate monohydrate (Fluka), potassium perchlorate (Acros Organics), rubidium perchlorate (abcr), cesium perchlorate (Sigma-Aldrich), magnesium perchlorate (Fluka), calcium perchlorate tetrahydrate (Acros Organics), strontium perchlorate trihydrate (Thermo Scientific), and barium perchlorate (Acros Organics) were purchased from commercial sources and used without further purification. Enantiomers of rac-2 were separated by HPLC using a Daicel Chiral Technologies CHIRALPAK® IG (inner diameter × length; particle size: 10 mm × 250 mm; 5 μm) semi-preparative column as chiral stationary phase and CH2Cl2–MeCN 70 : 30 (0.1% Et2NH) as eluent (2.0 mL min−1 flow rate, 25 °C). 23 mg of rac-2 dissolved in CH2Cl2 (1.5 mL), inj.: 500 μL. Ratios of solvents for the eluents are given in volumes (mL mL−1). NMR spectra were measured using a Bruker Avance III HD Nanobay 400 MHz spectrometer equipped with a 5 mm CPP BBO probe, or using a Bruker Avance III 500 MHz spectrometer equipped with a 5 mm CPP DCH 13C–1H/D helium-cooled cryogenic probe. NMR solvent: MeCN-d3 (Apollo Scientific). All signals were internally referenced to the solvent residue (MeCN-d3: 1.940 ppm for 1H NMR).
5
Characterization of Dark-Red Oil Synthesis
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To characterize the dark-red oil produced at the end of synthesis, Nuclear Magnetic Resonance (NMR) measurements were performed on a Bruker Avance III HD NanoBay 400 MHz NMR spectrometer. Chemical shifts (δ) were reported in parts per million referenced to the residual solvent peak. Multiplicities of observed peaks are denoted by s (singlet), d (doublet), t (triplet), q (quartet), quin (quintet), m (multiplet), and br (broad). Coupling constants of signals are reported as J values with the unit of Hertz. See NMR characterization data below. 1 H NMR [CDCl 3 , 400 MHz, 298 K], δ: 11.36 (br s, 1 H), 8.85 (dd, 1 H, 3 J HH = 4.2 Hz, 4 J HH = 1.7 Hz), 8.81 (dd, 1 H, 3 J HH = 7.1 Hz, 4 J HH = 1.9 Hz), 8.15 (dd, 1 H, 3 J HH = 8.3 Hz, 4 J HH = 1.7 Hz), 7.54 (dd, 1 H, 3 J HH = 8.3, 7.1 Hz), 7.51 (dd, 1 H, 3 J HH = 8.3 Hz, 4 J HH = 1.9 Hz), 7.45 (dd, 1 H, 3 J HH = 8.3, 4.2 Hz), 3.73 (t, 2 H, 3 J HH = 5.1 Hz), 3.68-3.61 (m, 4 H), 3.57 (s, 2 H), 3.52 (t, 2 H, 3 J HH = 5.2), 2.94 (t, 2H, 3 J HH = 5.1), 2.87 (t, 2 H, 3 J HH = 5.2 Hz). 13 C NMR [CDCl 3 , 100 MHz, 298 K], δ: 170. 84, 148.62, 139.17, 136.36, 134.49, 128.23, 127.48, 121.83, 121.65, 116.74, 73.80, 70.83, 70.55, 70.41, 53.77, 49.53, 41 .82.
6
Schlenk Synthesis of Organometallic Complexes
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All manipulations were carried out using standard Schlenk line and glove box techniques under an atmosphere of argon and dinitrogen, respectively. With the exceptions of tetrahydrofuran and diethyl ether, solvents were dried using a commercially available Braun SPS. Tetrahydrofuran and diethyl ether were distilled from sodium/benzophenone. Imidazole was sublimed in vacuo at 120°C; benzimidazole and 4,5-diphenylimidazole were dried in vacuo at 100°C. Methyl trifluoromethanesulfonate, sodium bis(trimethylsilyl)amide, potassium bis(trimethylsilyl)amide and selenium powder were used as received. {(HCDippN)2}BBr, [10] (THT)AuCl, [29] [Rh(cod)Cl]2, [30] and [Rh(CO)2Cl]2 [31] were synthesized according to literature procedures. 1 H, 13 C{ 1 H}, 11 B, 19 F and 77 Se NMR spectra were measured on a Bruker Avance III HD nanobay 400 MHz or a Bruker AVC500 spectrometer and referenced internally to residual protio-solvent ( 1 H) or solvent ( 13 C) resonances, and are reported relative to tetramethylsilane (δ = 0 ppm). 11 B and 19 F NMR spectra were referenced to external Et2O•BF3 and 77 Se NMR spectra to SePh2 in CDCl3. Assignments were confirmed using two dimensional 1 H-1 H, 13 C-1 H and ROESY NMR correlation experiments. Chemical shifts are quoted in δ (ppm) and coupling constants in Hz. Elemental analyses were carried out by London Metropolitan University.
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