Synthesis of the [Ru(dcbpy)(2)(OQN)](+) complex is reported in which dcbpy and OQN(-) are the bidentate 4,4'-dicarboxy-2,2'-bipyridyl and 8-oxyquinolate ligands, respectively. Spectroscopic, electrochemical, and theoretical analyses are indicative of extensive Ru(OQN) molecular orbital overlap due to degenerate Ru d(π) and OQN p(π) mixing. [Ru(dcbpy)(2)(OQN)](+) displays spectroscopic properties remarkably similar to those of the N3 dye, making it a promising candidate for application in dye-sensitized solar cell devices. However, its solar power conversion efficiency requires further optimization.
Rate coefficients can fluctuate in statically and dynamically disordered kinetics. Here, we relate the rate coefficient for an irreversibly decaying population to the Fisher information. From this relationship we define kinetic versions of statistical-length squared and divergence that measure cumulative fluctuations in the rate coefficient. We show the difference between these kinetic quantities measures the amount of disorder, and is zero when the rate coefficient is temporally and spatially unique.
The electronic structure of [Ru(bpy) 2 (OQN)] + (where bpy = 2,2Ј-bipyridine and OQN = 8-oxyquinolate) has been revisited using a complimentary suite of theoretical (DFT/TD-DFT), electrochemical (cyclic voltammetry) and spectroscopic techniques (UV/Vis/NIR absorption, EPR spectroscopy). Through functionalization of the R-OQN ligand (R = 2-Me; 5,7-Me 2 ; 5-F; 5-Cl; 5,7-Cl 2 ; 5-NO 2 ) charge delocalization across the non-innocent ruthenium-oxyquinolate framework has been investigated and correlated with substituent Hammett parameters. Combined spectroscopic and computational studies indicate substantial mixing at the [a]
Synthesis and characterization of the dimeric [fac-Re(R-OQN)(CO) 3 ] 2 and monomeric fac-Re(R-OQN)-(CO) 3 (CH 3 CN) complexes are reported where R = unsubstituted, 2-methyl, 5,7-dimethyl, or 5-fluoro and OQN = 8oxyquinolate. Facile solvolysis of the dimeric systems is observed in coordinating media quantitatively yielding the monomer complexes in situ. Due to poor synthetic yields of the dimeric precursors, a direct synthetic strategy for isolation of the acetonitrile monomer complexes with an improved yield was developed. The fac-Re(CH 3 CN) 2 (CO) 3 Cl complex was easily generated in situ as a convenient intermediate to give the desired products in quantitative yield via reaction with the appropriately substituted 8-hydroxyquinoline and tetramethylammonium hydroxide base. Key to the success of this reaction is the precipitation of the product with triflic acid, whose conjugate triflate base is here noncoordinating. Furthermore, isolation of the solvated single crystal [fac-Re(FOQN)(CO) 3 ](μ-Cl)[fac-Re(FHOQN)(CO) 3 ]•CH 3 C 6 H 5 has allowed a unique opportunity to access a possible reaction intermediate, giving insight into the formation of the [fac-Re(R-OQN)(CO) 3 ] 2 dimeric systems. Spectroscopic features (UV−vis, FTIR, and 1 H NMR) of both monomeric and dimeric structures are discussed in terms of the π-electron-donating ability of the oxyquinolate ligand. Interpretation of these electronic effects and the associated steric properties is aided by single-crystal X-ray diffraction, electrochemical, and DFT/TD-DFT computational studies.
An international team spanning 19 sites across 18 biopharmaceutical and in vitro diagnostics companies in the United States, Europe, and China, along with one regulatory agency, was formed to compare the precision and robustness of imaged CIEF (ICIEF) for the charge heterogeneity analysis of the National Institute of Standards and Technology (NIST) mAb and a rhPD-L1-Fc fusion protein on the iCE3 and the Maurice instruments. This information has been requested to help companies better understand how these instruments compare and how to transition ICIEF methods from iCE3 to the Maurice instrument. The different laboratories performed ICIEF on the NIST mAb and rhPD-L1-Fc with both the iCE3 and Maurice using analytical methods specifically developed for each of the molecules. After processing the electropherograms, statistical evaluation of the data was performed to determine consistencies within and between laboratory and outlying information. The apparent isoelectric point (pI) data generated, based on two-point calibration, for the main isoform of the NIST mAb showed high precision between laboratories, with RSD values of less than 0.3% on both instruments. The SDs for the NIST mAb and the rhPD-L1-Fc charged variants percent peak area values for both instruments are less than 1.02% across different laboratories. These results validate the appropriate use of both the iCE3 and Maurice for ICIEF in the biopharmaceutical industry in support of process development and regulatory submissions of biotherapeutic molecules. Further, the data comparability between the iCE3 and Maurice illustrates that the Maurice platform is a next-generation replacement for the iCE3 that provides comparable data.
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