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8 protocols using dmf d7

1

NMR Characterization of Pyrazole Complexes

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An appropriate amount of the complexes 1a,b and 2a,b was dissolved in 200 µL of DMF-d7 and 300 µL of D2O was added (1 mM final concentration). 1H NMR spectra (Varian spectrometer (Varian Inc.; Palo Alto, CA, USA), 400 MHz, 298 K) of these solutions were recorded at various time points (0–48 h), and the solutions were stored at r.t. in the dark between the individual experiments. The spectra were referenced to the residual signal of water (4.79 ppm). Note: DMF-d7 ensured the solubility of the complexes, as their solubility in water is not sufficient for 1H NMR. Deuterated solvents DMF-d7 and D2O were supplied by Merck/Sigma-Aldrich (Prague, Czech Republic). Free pyrazoles were studied by 1H NMR under the same experimental conditions (for comparative purposes).
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2

Evaluation of Ru(II)-7-azaindole Complexes

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The chemicals (RuCl3xH2O, 7-azaindole (aza), 3-iodo-7-azaindole (3Iaza), 3-chloro-7-azaindole (3Claza), 5-bromo-7-azaindole (5Braza), 5-fluoro-7-azaindole (5Faza), 2-methyl-4-chloro-7-azaindole (2Me4Claza), 3-chloro-5-bromo-7-azaindole (3Cl5Braza), 3-iodo-5-bromo-7-azaindole (3I5Braza), α-terpinene, cisplatin (CDDP), reduced glutathione (GSH), ethidium bromide (EtBr), tris(hydroxymethyl)aminomethane (TRIS)), solvents (methanol, diethyl ether, n-hexane, CDCl3, DMF-d7, MeOD-d4, D2O) and calf thymus DNA (ctDNA) were purchased from Sigma-Aldrich (Prague, Czech Republic), Acros Organics (Pardubice, Czech Republic) and Precious Metals Online (University of Wollongong, Australia). [Ru(μ-Cl)(η6-p-cym)Cl]2 was prepared according to the reported synthetic procedure [23 ].
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3

Synthesis and Characterization of Novel 7-Azaindole Gold(I) Complexes

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H[AuCl4]∙3H2O, triphenylphosphane (PPh3), 7-azaindole (Haza), 3-chloro-7-azaindole (H3Claza), 3-bromo-7-azaindole (H3Braza), 3-iodo-7-azaindole (H3Iaza), 5-bromo-7-azaindole (H5Braza), 3-chloro-5-bromo-7-azaindole (H3Cl5Braza), 3-iodo-5-bromo-7-azaindole (H3I5Braza), 2-methyl-4-chloro-7-azaindole (H2Me4Claza), NaOH, cisplatin, reduced glutathione (GSH), cysteine, BSA, Roswell Park Memorial Institute medium, fetal calf serum, glutamine, penicillin and streptomycin, and solvents (acetone, methanol, diethyl ether, chloroform, DMF, DMSO) and solvents for NMR experiments (DMF-d7, D2O) were supplied by Sigma-Aldrich Co. (Prague, Czech Republic) and Fisher-Scientific Co. (Pardubice, Czech Republic).
The starting chlorido-triphenylphosphanegold(I) complex, [AuCl(PPh3)], was prepared as described previously [51 (link)], and its composition was checked by elemental analysis and FTIR spectroscopy.
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4

Proton NMR Characterization of Triblock Terpolymers

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The triblock terpolymers were analyzed by proton nuclear magnetic resonance spectroscopy (1H-NMR). 1H-NMR measurements were performed on a Bruker Ascend 500 NMR spectrometer (500 MHz) (Bruker BioSpin GmbH, Rheinstetten, Germany) using CDCl3 (Sigma-Aldrich, Schnelldorf, Germany) and DMF-d7 (Sigma-Aldrich, Schnelldorf, Germany) as solvent at room temperature.
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5

Synthesis of Silicone-based Nanocomposite

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Silicone polyol (DMS-C15) was purchased from Gelest, USA. IPDI, DMF, glycerol 1,2-carbonate, and furfurylamine were purchased from Tokyo Chemical Industry, Japan. DMF-d7, dibutyltin dilaurate, and BMI were purchased from Sigma-Aldrich, USA. All chemicals were used as received without purification. An AgNW solution dispersed in IPA was purchased from Dittotechnology Ltd., Korea. The average diameter and length of the nanowires were 35 nm and 20 μm, respectively.
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6

Synthesis of K5Bi4 via Arc-Welding

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All reactions were carried out under a dry, argon atmosphere using a standard Schlenk line or glove box techniques. Solvents were purified as appropriate: en (Aldrich, 99.8%) was refluxed over CaH2 for 24 hours, distilled and stored on 4 Å molecular sieves; DMF (Aldrich, 99.8%) and DMF-d7 (Sigma-Aldrich, 99.5%) were stored over 3 Å molecular sieves for five days, distilled under vacuum (~50 mbar) and stored on 4 Å molecular sieves; acetonitrile (VWR Chemicals, >99%) was stored over 3 Å molecular sieves for five days, distilled and stored on 3 Å molecular sieves; and n-hexane (Sigma-Aldrich, >95%) and toluene (Acros Organics) were refluxed over Na for 24 hours, distilled and stored on 4 Å molecular sieves. The crypt-222 (Kryptofix 222, Sigma-Aldrich) was dried under vacuum. The A was prepared by the published procedure on a larger scale (0.50 mmol)44 (link). All other reagents were used as received: K (Acros Organics, 98%), Bi powder (ChemPur, 99.5%), [(cod)IrCl]2 (ChemPur) and [CpRu(MeCN)3][PF6] (Sigma-Aldrich). K5Bi4 was synthesized by combining K and Bi in stoichiometric amounts in a niobium ampoule. The ampoule was sealed by arc-welding, sealed in a quartz tube under vacuum, placed in an oven and kept at 700 °C for 7 days.
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7

Synthesis and Photophysical Analysis

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BiCl3, BiBr3, BiI3, and hydrazine hydrate were obtained from Sigma-Aldrich.
DMF-d7 was purchased from Sigma-Aldrich.
All other reagents were purchased from Fluorochem and Apollo Scientific
and used without further purification. HPLC-grade dimethylformamide
(DMF), acetonitrile (ACN), and tetrahydrofuran (THF) were purchased
from Sigma-Aldrich for photophysical analysis.
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8

Synthesis and Characterization of 7-Azaindole Derivatives

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The chemicals K2[PtCl4] was purchased from Precious Metals Online, while KI, 7-azaindole, 3-chloro-7-azaindole, 3-bromo-7-azaindole, 3-iodo-7-azaindole, 4-chloro-7-azaindole, 4-bromo-7-azaindole, 5-bromo-7-azaindole, 4-chloro-2-methyl-7-azaindole, cisplatin, oxaliplatin, reduced glutathione, guanosine 5′-monophosphate disodium salt hydrate, ethidium bromide, tris(hydroxymethyl)aminomethane, calf thymus DNA, Roswell Park Memorial Institute medium, fetal calf serum, glutamine, penicillin and streptomycin, and solvents (methanol, diethyl ether, n-octanol, DMF-d7, D2O) were supplied by Sigma-Aldrich Co. and Fisher-Scientific Co.
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