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Inova 300 mhz

Manufactured by Agilent Technologies

The Inova 300 MHz is a nuclear magnetic resonance (NMR) spectrometer manufactured by Agilent Technologies. It operates at a proton frequency of 300 MHz and is designed to perform high-resolution NMR analysis of chemical samples.

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2 protocols using inova 300 mhz

1

Synthesis and Characterization of Platinum and Nickel Carbonyl Complexes

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All
reactions and sample manipulations were carried out using standard
Schlenk techniques under nitrogen and in dried solvents. All of the
reagents were commercial products (Aldrich) of the highest purity
available and were used as received, except [NR4]2[Pt3n(CO)6n] (n = 2–4)1 (link) and
[NR4]2[Ni6CO)12] (R =
Et, Bu),44 (link) which have been prepared according
to the literature. Analyses of C, H, and N were obtained with a Thermo
Quest Flash EA 1112NC instrument. Analysis of Ni and Pt were performed
by microwave plasma-atomic emission spectrometry on a Agilent 4210
MP-AES instrument. IR spectra were recorded on a PerkinElmer Spectrum
One interferometer in CaF2 cells. ESI mass spectra were
recorded on a Waters Micromass ZQ4000 instrument using CH3CN as the solvent (source temperature 150 °C; capillary voltage
2.54 kV; infusion flow 20 μL/min; cone voltage 10 V). 195Pt and 13C{1H} NMR measurements were performed
on Varian Mercury Plus 400 MHz and Varian Inova 300 MHz spectrometers.
The carbon chemical shifts were referenced to a nondeuterated aliquot
of the solvent. The platinum chemical shifts were referenced to external
Na2PtCl6 (1.2 M in D2O). Structure
drawings have been created with SCHAKAL99.45 Caution! CO and Ni(CO)4 may be
generated during manipulation of these compounds. All of the operations
must be carried out under a well-ventilated fume hood.
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2

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).
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