Screening of Conditions that Facilitate Crystallization of Oligopeptidase B from Serratia Proteamaculans by Differential Scanning Fluorimetry

Crystallography Reports - Oligopeptidases B (OpdBs) are two-domain serine peptidases with trypsin-like substrate specificity belonging to the prolyl oligopeptidase family. These enzymes are...     

Base-free aerobic oxidation of 5-hydroxymethylfurfural to 2,5-furandicarboxylic acid over Pt/C catalysts synthesized by pulse alternating current technique

The Pt/C catalysts with various Pt content (5-30 wt%) synthesized via electrochemical pulse alternating current technique have been evaluated for the base-free aerobic oxidation of 5-hydroxymethylfurfural to 2,5-furandicarboxylic acid. The higher Pt content in the catalyst (30 wt%) provides the product yield up to 65% upon performing the process in concentrated (～0.1 M) aqueous solutions of the substrate.     

Preparation, crystallographic characterization and theoretical study of two isomers of C70(CF3)12

Two isomers of C70(CF3)12 have been isolated from a mixture obtained by trifluoromethylation of C70 with CF3I; their molecular structures determined by X-ray crystallography are in good agreement with the results of theoretical DFT calculations for the most stable C70(CF3)12 isomers.     

CrxRe1−xO2 oxides with different rutile-like structures: changes in the electronic configuration and resulting physical properties

Mixed chromium-rhenium oxides, Cr_xRe_1−xO₂ with 0.31?x?0.66, have been synthesized for the first time by high-pressure high-temperature synthesis and in evacuated quartz tubes. The crystal structures of the compounds have been determined by single crystal and powder X-ray diffraction. Depending on synthesis conditions (pressure and temperature) these phases crystallize either in a tetragonal structure (P4₂/mnm) with statistical distribution of metal ions on one site (rutile-type), with cation ordering along c-axis (trirutile-type), or in a monoclinic rutile-like structure (C2/m) with ordering of Cr- and Re-cations and metallic Re-Re bonds. The “a” parameter of the tetragonal unit cell increases with increasing Re content whereas the “c” parameter decreases, indicating a strengthening of the Re-Re bond. The thermal stability of tetragonal Cr_xRe_1−xO₂ in Ar-atmosphere depends on the Re-content, decomposition is observed at 1241 K for x=0.34, but already at 966 K for x=0.5. The thermal expansion of Cr_xRe_1−xO₂ is anisotropic with a larger expansion coefficient in the “c” direction. Tetragonal Cr_xRe_1−xO₂ with 0.31?x<0.54 order antiferromagnetically at low temperatures with T_N depending on the Cr-content x.     

Use of the mathematical apparatus of two-component spectrophotometry for the simultaneous catalymetric determination of two anions

Previously studied reactions of aluminum(III) with Xylenol Orange and of cobalt(III) with nitroso-R salt in weakly acidic solutions were proposed for the simultaneous catalymetric determination of carbonate and borate ions and carbonate and phosphate ions, respectively. It was demonstrated that the mathematical apparatus of two-component spectrophotometry is suitable for processing the results of analysis.Translated from Zhurnal Analiticheskoi Khimii, Vol. 60, No. 1, 2005, pp. 7–10.Original Russian Text Copyright © 2005 by Mikhailova, Belikov, Blank.     

Phase formation in the ZrO(NO3)2-NaF(HF)-H3PO4-H2O system at 20°C

Phase formation in the ZrO(NO₃)₂-NaF(HF)-H₃PO₄-H₂O system was studied at 20°C and 2.0–14.5 wt % ZrO₂ in the initial solution along sections with molar ratios PO ₄ ^3? /Zr = 0.5 and 1.5 and also in the presence of hydrogen fluoride at Na/Zr = 1 and PO ₄ ^3? /Zr = 0.5, 1.0, and 1.5. Crystalline zirconium hydrophosphate Zr(HPO₄)₂ · H₂O, fluorozirconates Na₅Zr₂F₁₃ and Na₇Zr₆F₃₁ · 12H₂O, fluorophosphatozirconates NaH₂Zr₃F₃(PO₄)₄ · 3H₂O and NaZr₂F₆(PO₄) · 4H₂O, and amorphous NaZrO_0.5F(PO₄) · 4H₂O (provisional composition) were separated at room temperature. NaH₂Zr₃F₃(PO₄)₄ · 3H₂O and NaZr₂F₆(PO₄) · 4H₂O were prepared for the first time and were studied by crystal-optical, elemental, and thermal analyses, X-ray powder diffraction, IR spectroscopy, scanning electron microscopy (SEM), and X-ray microanalysis. Na₇Hf₆F₃₁ · 12H₂O was found to exist in a mixture with the hydrophosphate.     

Phase formation along sections of the HfO(NO3)2-H3PO4-RbF-H2O system

The phase formation in the system HfO(NO₃)₂-H₃PO₄-RbF-H₂O was studied along the sections at the molar ratios PO ₄ ^3? /Hf = 0.5, 1.0, 1.5, 2.0, and 3.0 and RbF: Hf = 1?5. The initial solutions contained 2–10 wt % HfO₂. The synthesis was performed at room temperature. The following substances were obtained for the first time: crystalline fluorophosphatehafnate RbHfF₂PO₄ · 0.5H₂O, crystalline triple salt HfF₄ · Rb(PO₄)_0.33 · RbNO₃, crystalline solvate Rb₃Hf₃(PO₄)₅ · 3HF, and amorphous fluorophosphate Hf₃O₂F₂(PO₄)₂ · 8H₂O (formula is conditional). The compounds were studied by crystal-optical, elemental, X-ray diffraction, thermogravimetric, IR spectroscopic, and electron microscopic analyses.     

A Mechanism‐Based Approach to Screening Metagenomic Libraries for Discovery of Unconventional Glycosidases

Functional metagenomics has opened new opportunities for enzyme discovery. To exploit the full potential of this new tool, the design of selective screens is essential, especially when searching for rare enzymes. To identify novel glycosidases that employ cleavage strategies other than the conventional Koshland mechanisms, a suitable screen was needed. Focusing on the unsaturated glucuronidases (UGLs), it was found that use of simple aryl glycoside substrates did not allow sufficient discrimination against β‐glucuronidases, which are widespread in bacteria. While conventional glycosidases cannot generally hydrolyze thioglycosides efficiently, UGLs follow a distinct mechanism that allows them to do so. Thus, fluorogenic thioglycoside substrates featuring thiol‐based self‐immolative linkers were synthesized and assessed as selective substrates. The generality of the approach was validated with another family of unconventional glycosidases, the GH4 enzymes. Finally, the utility of these substrates was tested by screening a small metagenomic library.     

Enantioselective Access to 1H‐Isoindoles with Quaternary Stereogenic Centers by Palladium(0)‐Catalyzed C−H Functionalization

A catalytic enantioselective method for the synthesis of chiral 1H‐isoindoles bearing quaternary stereogenic centers is reported. Powered by readily accessible phosphordiamidite ligands, the presented palladium(0)‐catalyzed C?H functionalization uses trifluoroacetimidoyl chlorides as electrophilic components. It delivers previously inaccessible perfluoroalkylated 1H‐isoindoles in high yields and enantioselectivities. The subsequent diastereoselective addition of nucleophiles provides access to densely substituted and sterically hindered isoindolines.     

Thermal Pretreatment of Harvest Residues and Their Use in Anaerobic Co-digestion with Dairy Cow Manure

Several batch experiments were conducted on the anaerobic co-digestion of dairy cow manure (DCM) with three harvest residues (HR) (soybean straw, sunflower stalks, and corn stover). The influence of thermal pretreatment of HR on biogas production was investigated, where the HR were thermally pretreated at two different temperatures: T = 121 °C and T = 175 °C, during t = 30 and t = 90 min, respectively. All anaerobic co-digestion batch experiments were performed simultaneously under thermophilic regime, at T = 55 °C. Biogas and methane yields were significantly improved in experiments performed with corn stover thermally pretreated at 175 °C for 30 min (491.37 cm³/g VS and 306.96 cm³/g VS, respectively), if compared to experiments performed with untreated corn stover. The highest VS and COD removal rates were also observed in the same group of experiments and were 34.5 and 50.1%, respectively. The highest biogas and methane yields with soybean straw (418.93 cm³/g VS and 261.44 cm³/g VS, respectively) were obtained when soybean straw pretreated at 121 °C during 90 min. The highest biogas and methane yields with sunflower stalk (393.28 cm³/g VS and 245.02 cm³/g VS, respectively) were obtained when sunflower stalk was pretreated at 121 °C during 90 min.