Materials and reagents. 2,2’-Azobispyridine (apy) and Ru(tpy)Cl3 were synthesized according to the literature methods.8, 14 XxXx, NaClO4 (both Merck), NaClO, AgNO3, (both Acros), tpy (Aldrich) and RuCl3·3H2O (Xxxxxxx & Xxxxxxx) were used as supplied. All other chemicals and solvents were reagent grade commercial materials and used as received, without further purification. Physical measurements C, H and N determinations were performed on a Xxxxxx Xxxxx 2400 Series II analyzer. Mass spectra were obtained with x Xxxxxxxx MAT TSQ-700 mass spectrometer equipped with a custom-made electrospray interface (ESI). FTIR spectra were obtained on a Perkin Xxxxx Xxxxxxx 1000 FTIR spectrophotometer equipped with a Golden Gate ATR device, using the diffuse reflectance technique (res. 4 cm-1). NMR spectra were recorded on a Bruker DPX-300 spectrometer operating at a frequency of 300 MHz, on a Bruker AV-500, at a frequency of 500 MHz, and on a Bruker DMX-400, at a frequency of 400 MHz. Chemical shifts were calibrated against tetramethylsilane (TMS).
Materials and reagents. 2,2´-azobispyridine (apy), Ru(tpy)Cl3, [Ru(apy)(tpy)Cl](ClO4), [Ru(apy)(tpy)(H2O)](ClO4)2·2H2O, [Ru(apy)(tpy)(CH3CN)](ClO4)2, [Ru(azpy)(tpy)Cl]Cl·5H2O and [Ru(impy)(tpy)Cl](ClO4) were synthesised according to the literature methods.30-32, 34, 35 LiCl, NaClO4 (both Merck), NaClO, AgNO3 (both Acros), tpy (Aldrich), RuCl3·3H2O (Johnson & Matthey), 9-EtGua (Sigma) and H2N(CH2)6NH2 (Fluka) were used as supplied. Ultra pure water (18.2 ΩM; Aldrich) was used for the MS, CD and LD experiments. All other chemicals and solvents were reagent grade, commercial materials and used as received. Calf-thymus DNA (ct-DNA) was purchased from Sigma Aldrich and used without further purification. The solid DNA salt was dissolved in ultra pure water (18.2 ΩM; Aldrich) and left at 278 K for 24 hours to fully hydrate. The resulting stock DNA solution was kept frozen and it was thawed when needed. The concentration of the DNA stock solution was determined spectroscopically, using the known molar extinction coefficient of ct-DNA at 258 nm: ε258 = 6600 molar base−1 cm−1 dm3.36 A 100 mM stock solution of sodium cacodylate buffer (pH 6.8) was prepared, as well as a 1M sodium chloride stock solution, using in both cases ultra pure water (18.2 ΩM; Aldrich). Physical measurements C, H and N determinations were performed on a Perkin Elmer 2400 Series II analyzer. Mass spectra were obtained with a Finnigan Aqa mass spectrometer equipped with an electrospray ionization source (ESI). NMR spectra were recorded on a Bruker DPX-300 spectrometer operating at a frequency of 300 MHz, at a temperature of 310 K, unless otherwise stated. Chemical shifts were calibrated against tetramethylsilane (TMS). CD spectra were collected in 2 mm path-length quartz cuvettes using a Jasco J-810 spectropolarimeter. Flow LD spectra were collected using a flow Couette cell in the above-mentioned spectropolarimeter. All CD and LD spectra were recorded at room temperature. Synthesis and characterization of [{Ru(apy)(tpy)}2{µ-H2N(CH2)6NH2}](ClO4)4 [Ru(apy)(tpy)(H2O)](ClO4)2·2H2O (26 mg, 0.034 mmol) and H2N(CH2)6NH2 (2 mg, 0.016 mmol) were dissolved in 12 mL EtOH abs:MeOH 5:1. The solution was vigorously refluxed for 15 hours. The pH remained constant around 7. The product was collected by filtration, washed with little ethanol and diethyl ether and dried in vacuo over silica. Yield: 20 mg (76%). Anal. Calc. for C56H54N16O16Cl4Ru2: C, 43.4; H, 3.5; N, 14.4%. Found: C, 43.8; H, 3.8; N, 14.5%. m/z (ESI-MS) 634.1 ([{Ru(apy)...
Materials and reagents. 2-pyridinealdazine (paa), 4-amino-3,5-bis(pyridine-2-yl)-1,2,4-triazole (abpt), Ru(tpy)Cl3 and cis-Ru(bpy)2Cl2 were synthesized following procedures described in literature.33-36 2-cyanopyridine, 2-pyridinaldehyde, hydrazine monohydrate, NH4PF6 and tpy (Xxxxxxx), LiCl (Merck), NaBF4 and bpy (Acros) and RuCl3·3H2O (Xxxxxxx & Xxxxxxx) were used as supplied. All other chemicals and solvents were reagent grade commercial materials and used as received, without further purification. Physical measurements C, H and N determinations were performed on a Xxxxxx Xxxxx 2400 Series II analyzer. Mass spectra were obtained with a Xxxxxxxx MAT TSQ-700 mass spectrometer equipped with a custom-made electrospray interface (ESI). NMR spectra were recorded on a Bruker DPX-300 spectrometer operating at a frequency of 300 MHz. Chemical shifts were calibrated against tetramethylsilane (TMS). Synthesis and characterization of [{Ru(tpy)Cl}2(µ-paa)](BF4)2 (1h) LiCl (500 mg, 11.80 mmol) was dissolved in 80 ml of ethanol-water (3:1). Triethylamine (0.160 ml, 1.135 mmol) was added, followed by Ru(tpy)Cl3 (500 mg, 1.135 mmol) and paa (360 mg, 1.715 mmol). The mixture was vigorously refluxed for 90 minutes, and the hot solution was filtered to remove any insoluble material. The brown solution was evaporated to dryness. 15 ml methanol were used to dissolve the residue, to which 35 ml of a methanolic saturated solution of NaBF4 were added. The flask was left for 3 days at 4 °C. A brown precipitate had then appeared, which was filtered, washed with little ice-cold ethanol and ether and dried in vacuo over silica Yield: 39 mg (3%). Anal. Calc. for C42H32N10B2F8Cl2Ru2: C, 44.9; H, 2.9; N, 12.5. Found: C, 42.2; H, 2.9; N, 11.7. m/z (ESIMS) 580.1 ([Ru(paa)(tpy)Cl]+); 475.0 ([{Ru(tpy)Cl}2(μ-paa)]2+). 1H NMR (DMSO-d6): δ (ppm): 9.71 (2H, d, 5.49 Hz, 6P); 8.44 (8H, m, 3T, 3T´); 8.22 (2H, t, 6.93 Hz, 4P); 8.12 (4H, t, 7.12 Hz, 4T); 8.00 (4H, m, 5P, 4T´); 7.92 (2H, d, 8.06 Hz, 3P); 7.46 (4H, t, 6.24 Hz, 5T); 7.11 (4H, d, 4.83 Hz, 6T); 6.97 (2H, s, CH=). Synthesis and characterization of [Xx(abpt)(bpy)2](PF6)2 (1i) The synthesis of [Ru(abpt)(bpy)2](PF6)2 was carried out as described in the literature,32 with slight modifications. cis-Ru(bpy)2Cl2 (75 mg, 0.18 mmol) and abpt (82 mg, 0.34 mmol) were dissolved in 15 ml of ethanol and refluxed for two hours. The mixture was evaporated under reduced pressure, and the obtained residue was dissolved in 2.5 ml methanol. 5 ml of a saturated solution of NH4PF6 ...
Materials and reagents. All chemicals were analytical reagent grade and obtained from Sigma-Xxxxxxx and used as purchased unless otherwise specified. Copper(I) bromide was obtained with g99.995% purity (trace metals basis) from Sigma-Xxxxxxx and stored under vacuum before use. Solvents were obtained from Xxxxxx Scientific. Methacryloxyethyltrimethylammonium chloride (METAC) was obtained as a 75% aqueous solution containing 600 ppm monomethyl ether hydroquinone as inhibitor; the monomer was purified to remove the inhibitor by passing the solution through a basic alumina column (Xxxxxxxxx grade I).
Materials and reagents. Chemicals used for treatments: β-NF, PB, TCPOBOP, 3MC, KA, PCN, dexamethasone (water soluble) were all acquired from Sigma-Xxxxxxx (St. Xxxxx, MO) as well as Xxxxxxxx' E medium, Xxxxx-Xxxxxx buffer, collagenase and other general chemicals. Antibodies to CYP2B1 and CYP3A2 were provided by Xx. Xxxxx Xxxxxxx (University of California, San Diego, CA), and anti-CYP1A antibody was purchased from Daichi Pure Chemicals (Tokyo, Japan). The anti-GAPDH monoclonal antibody was acquired from Millipore (Billereca, MA) and the anti-CAR polyclonal antibody was purchased from Santa Xxxx Biotechnology (Santa Cruz, CA).
Materials and reagents. 2.1.1 Plasticware 6, 12, 24, 48, 96 -well tissue culture plate (Costar corning). 96-well U-bottom tissue culture plate (Costar corning). 25cm2 / 75cm2 tissue culture flasks (Costar corning). 10cm culture dishes (Costar corning).
