Designed Synthesis of Mononuclear Tris(heteroleptic) Ruthenium Complexes Containing Bidentate Polypyridyl Ligands

Anderson, Peter; Deacon, Glen B.; Haarmann, Klaus H.; Keene, F. Richard; Meyer, Thomas J.; Reitsma, David A.; Skelton, Brian W.; Strouse, Geoffery F.; Thomas, Nicholas C.; Treadway, Joseph A.; White, Allan H.

doi:10.1021/ic00128a028

Cited by 258 publications

(214 citation statements)

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“…The title compound was prepared by the following procedure: [Ru(bpy)(CO)2Cl2] (0.1 g) 3 was added to H2O (10 cm 3 ), and an ethanolic solution (10 cm 3 ) of dppy (0.09 g) was added to the suspension. The mixture was refluxed with stirring for 2 h. The addition of a saturated aqueous solution of KPF6 to the solution resulted in a colorless precipitate.…”

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confidence: 99%

Crystal Structure of (2,2'-Bipyridine-N,N')(diphenyl-2-phosphinopyridine-P)-chloro(dicarbonyl)ruthenium(II) Hexafluorophosphate

Ooyama

Sato

2003

Anal. Sci. X

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The chemistry of polynuclear metal complexes including various bridging ligands has been widely developed for many years. 1 In particular, the diphenyl-2-phosphinopyridine (dppy) ligand has been used to construct hetero-binuclear metal complexes due to its possessing both the soft (P) and hard (N) donor atoms. 2In this work, an X-ray structural analysis of [Ru(bpy)(dppy)(CO)2Cl] + (bpy = 2,2′-bipyridine), which is a precursor for constructing new hetero-binuclear metal complex systems based on polypyridyl ruthenium complexes, was carried out.The title compound was prepared by the following procedure: [Ru(bpy)(CO)2Cl2] (0.1 g) 3 was added to H2O (10 cm 3 ), and an ethanolic solution (10 cm 3 ) of dppy (0.09 g) was added to the suspension. The mixture was refluxed with stirring for 2 h. The addition of a saturated aqueous solution of KPF6 to the solution resulted in a colorless precipitate. The recrystallized compound from ethanol-acetone was identified as a dppy coordination complex, [Ru(bpy)(dppy)(CO)2Cl]PF6. 4 A colorless crystal of the title compound, having approximate dimensions of 0.33 × 0.28 × 0.05 mm, was mounted on a glass fiber. Data collections were performed at 173 K with graphitemonochromated Mo Kα radiation (λ = 0.71070 Å) on a Rigaku/MSC Mercury CCD diffractometer. The data were corrected for Lorentz and polarization effects. The structure was solved by the Patterson method using DIRDIF94 PATTY.All of the non-hydrogen atoms were refined anisotoropically by full-matrix least-squares methods. All hydrogen atoms were located by a geometrical calculation, and were not refined. All calculations were performed using the teXsan crystallographic software package. The crystal and experimental data are given in Table 1. The atomic positional and thermal parameters are given in Table 2.The molecular structure of the cation is shown in Fig. 2 and selected bond distances and angles are listed in Table 3. Although both the P-mono and P,N-bidentate coordination manners have been known for mononuclear systems, 5 the dppy ligand coordinates to the ruthenium center through only the phosphorus atom, as shown in Fig. 2. The coordination sphere of the ruthenium atom consists of one dppy ligand, two mutually cis carbonyl ligands, a chelating bipyridine ligand, and one chloride ligand. The Ru-P bond is not significantly x39 ANALYTICAL SCIENCES 2003, VOL. 19 X-ray Structure Analysis Online Crystal Structure of (2,2′-Bipyridine-N,N′)(diphenyl-2-phosphinopyridine-P)-chloro(dicarbonyl)ruthenium(II) HexafluorophosphateDai OOYAMA † and Masahito SATO Faculty of Education, Fukushima University, Kanayagawa, Fukushima 960-1296, Japan The crystal structure of (2,2′-bipyridine-N,N′)(diphenyl-2-phosphinopyridine-P)-chloro(dicarbonyl)ruthenium(II) hexafluorophosphate ([Ru(bpy)(dppy)(CO)2Cl]PF6; bpy = 2,2′-bipyridine, dppy = diphenyl-2-phosphinopyridine) has been determined by X-ray diffraction. This compound crystallizes in a monoclinic system, space group P21/n, with the following unit cell parameters: a = 10.237 (1)

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confidence: 99%

Crystal Structure of (2,2'-Bipyridine-N,N')(diphenyl-2-phosphinopyridine-P)-chloro(dicarbonyl)ruthenium(II) Hexafluorophosphate

Ooyama

Sato

2003

Anal. Sci. X

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“…The complement strand was 5Ј[ 32Ϫ P]-labeled using polynucleotide kinase and PAGE-purified. [Ru(phen)(dppz)(bpyЈ)]Cl 2 was synthesized using general procedures (31,32). E. coli SoxR was expressed and purified as outlined (33).…”

Section: Methodsmentioning

confidence: 99%

“…The abortive transcription assay was modified from one published previously (5). DNA (30 fmol in 15 mM NaPi, 50 mM NaCl, pH 7.4) was incubated in 30 L 300 nM SoxR (75 mM KCl, 10 mM Tris, 2 mM MgCl 2, pH 8.0), from E. coli or Pseudomonas aeruginosa (32,12). Reduced samples were prepared as described previously using dithionite in an anaerobic chamber.…”

Section: Methodsmentioning

confidence: 99%

DNA-mediated redox signaling for transcriptional activation of SoxR

Lee

Demple

Barton

2009

Proc. Natl. Acad. Sci. U.S.A.

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In enteric bacteria, the cellular response to oxidative stress is activated by oxidation of the iron-sulfur clusters in SoxR, which then induces transcription of soxS, turning on a battery of defense genes. Here we demonstrate both in vitro and in cells that activation of SoxR can occur in a DNA-mediated reaction with guanine radicals, an early genomic signal of oxidative stress, serving as the oxidant. SoxR in its reduced form is found to inhibit guanine damage by repairing guanine radicals. Moreover, cells treated with a DNA-binding photooxidant, which generates guanine radicals, promotes the expression of soxS. In vitro, this photooxidant, tethered to DNA 80 bp from the soxS promoter, induces transcription by activating SoxR upon irradiation. Thus, transcription can be activated from a distance through DNA-mediated charge transport. This chemistry offers a general strategy for DNA-mediated signaling of oxidative stress.DNA charge transport ͉ guanine radicals ͉ oxidative stress

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“…The reaction of the polymer [Ru(CO) 2 Cl 2 ] n , readily available from RuCl 3 ·nH 2 O in refluxing formic acid [26], with the corresponding sodium carboxylate and a two-electron ligand such as pyridine (py) in refluxing methanol produces directly the corresponding pyridine complexes Ru 2 (CO) 4 (OOCR) 2 (py) 2 according to Eq. (6), the yields, however, being not higher than those obtained from Ru 3 (CO) 12 .…”

Section: Synthetic Methodsmentioning

confidence: 99%