• Title/Summary/Keyword: F NMR

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31P NMR Spectroscopy Revealed Adenylate kinase-like Activity and Phosphotransferase-like Activity from F1-ATPase of Escherichia coli

  • Kim, Hyun-Won
    • Bulletin of the Korean Chemical Society
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    • v.32 no.1
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    • pp.183-185
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    • 2011
  • Adenylate kinase-like activity and phosphotransferase-like activity from $F_1$-ATPase of Escherichia coli was revealed by $^{31}P$ NMR spectroscopy. Incubation of F1-ATPase with ADP in the presence of $Mg^{2+}$ shows the appearance of $^{31}P$ resonances from AMP and Pi, suggesting generation of AMP and ATP by adenylate kinase-like activity and the subsequent hydrolysis to Pi. Incubation of $F_1$-ATPase with ADP in the presence of methanol shows additional peak from methyl phosphate, suggesting phosphotransferase-like activity of $F_1$-ATPase. Both adenylate kinase-like activity and phosphotransferase-like activity has not been reported from $F_1$-ATPase of Escherichia coli. $^{31}P$ NMR could be a valuable tool for the investigation of phosphorous related enzyme.

19F NMR investigation on the ratio of amorphous to crystal for the binder PVdF in Li ion battery

  • Im, Jong-san;Park, Junghwan;Kim, Kyoung Soo;Jung, Hyunok
    • Journal of the Korean Magnetic Resonance Society
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    • v.23 no.1
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    • pp.1-5
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    • 2019
  • $^{19}F$ NMR experiments were carried out to observe the change of the characteristics of the PVdF binder which is an auxiliary material of the lithium ion battery. PVdF has various crystalline or amorphous phases by thermal treatment. A mixture of cathode and auxiliary materials including PVdF was coated on aluminum foil as an electron collector and then subjected to thermal treatment at various temperatures. The overlapped $^{19}F$ NMR signals obtained from the various phases were separately convoluted into the respective phases, and it was found that there was a relative ratio change of these phases. In addition, the crystal and amorphous phase of PVdF was changed during the vacuum drying, which is the last step of the actual electrode manufacturing. It was observed that the relative amount of amorphous phase, which may affect the flexibility of the electrode or the wettability of the electrolyte, abruptly changes after a certain temperature.

13C-NMR Spectroscopy of Urea-Formaldehyde Resin Adhesives with Different Formaldehyde/Urea Mole Ratios

  • Park, Byung-Dae;Lee, Sang M.;Park, Jong-Young
    • Journal of the Korean Wood Science and Technology
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    • v.36 no.2
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    • pp.63-72
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    • 2008
  • As a part of abating formaldehyde emission of urea-formaldehyde (UF) resin adhesive, this study was conducted to investigate chemical structures of UF resin adhesives with different formaldehyde/urea (F/U) mole ratios, using carbon-13 nuclear magnetic resonance ($^{13}C$-NMR) spectroscopy. UF resin adhesives were synthesized at four different F/U mole ratios such as 1.6, 1.4, 1.2, and 1.0 for the analysis. The analysis $^{13}C$-NMR spectroscopy showed that UF resin adhesives with higher F/U mole ratios (i.e., 1.6 and 1.4) had two distinctive peaks, indicating the presence of dimethylene ether linkages and methylene glycols, a dissolved form of free formaldehyde. But, these peaks were not detected at the UF resins with lower F/U mole ratios (i.e., 1.2 and 1.0). These chemical structures present at the UF resins with higher F/U mole ratios indicated that UF resin adhesive with higher F/U mole ratio had a greater contribution to the formaldehyde emission than that of lower F/U mole ratio. Uronic species were detected for all UF resins regardless of F/U mole ratios.

Effective Synthesis of $\alpha$--Bromo-$\omega$ -fluoroalkane with Analysis of Gas-chromatography (가스크로마토그라피 분석을 통한 $\alpha$-브로모-$\omega$ -플루오로알칸의 효율적 합성)

  • Yu, Kook Hyun
    • Journal of the Korean Chemical Society
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    • v.39 no.5
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    • pp.414-420
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    • 1995
  • $\alpha$-Bromo-$\omega$-fluoroalkanes are synthesized in 19∼55% yields from the reactions of dibromoalkanes with AgF and TBABr in acetonitrile at $82^{\circ}C$ for 20 minutes. The reaction is monitored with gas-chromatography. 1^H$ NMR and $19^F$ NMR-Spectrometer are used for identification of $\alpha$-Bromo-$\omega$-fluoroalkanes, difluoroalkane, fluoroalken and bromoalkene.

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4f spin dynamics in TbNi$_2$B$_2$C by $^{11}$B NMR

  • Lee, K.H.;Seo, S.W.;Kim, D.H.;Khang, K.H.;Seo, H.S.;Hwang, C.S.;Hong, K.S.;Cho, B.K.;Lee, W.C.;Lee, Moo-Hee
    • 한국초전도학회:학술대회논문집
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    • v.10
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    • pp.61-64
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    • 2000
  • $^{11}$B NMR measurements have been performed to investigate local electronic structure and 4f spin dynamics for TbNi$_2$B$_2$C single crystal. $^{11}$B NMR spectra show three resonance peaks due to the quadrupolar interaction. Shift and linewidth are huge and strongly temperature-dependent. In addition, both are proportional to magnetic susceptibility, indicating that the hyperfine field at the boron site originates from the 4f spins of Tb. $^{11}$B NMR shift and relaxation rates show high anisotropy for field parallel and perpendicular to the c-axis. Anisotropy of the shift and the relaxation rates suggests that the hyperfine field perpendicular to the c-axis is larger.

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Regiospecific Protein Perturbation on F NMR Shifts and Photoisomerization of Fluororhodopsins. An Interpretation Based on Recent Crystal Structures of Rhodopsin

  • Colmenares, Letica U.;Liu, Robert S.H.
    • Journal of Photoscience
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    • v.10 no.1
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    • pp.81-87
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    • 2003
  • Based on structural information provided by recently reported crystal structures of rhodopsin, we present rationales for the regiospecific protein perturbation on the previously reported $\^$19/F chemical shifts of the vinyl and trifluoromethylrhodopsins and their photoproducts. The crystal structures also suggest that H-bonding is a likely cause for the earlier reported regiospecific photoisomerization of the 10-fluororhodopsins. Photoisomerization was revealed by chemical shift of the photoproducts. Additionally, possible use of 3-bond F,F coupling constants for following photoisomerization of retinal-binding proteins is discussed.

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Solution-State Structure of Native Coenzyme F430 by NMR Methods

  • 원호식;Karl D. Olson;박지석;Ralph S. Wolfe;Dennis R. Hare;Michael F. Summers
    • Bulletin of the Korean Chemical Society
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    • v.16 no.7
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    • pp.649-653
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    • 1995
  • Solution-state structure of native F430 was determined by using NMR methods and NMR-based distance geometry (DG) computations. Structures were generated with loose NOE-derived interproton distance restraints (2.0-2.5 Å, 2.0-3.5 Å and 2.0-4.5 Å for strong, medium, and weak NOE cross-peak intensities, respectively). 2D NOESY back-calculations of structures were subsequently carried out for establishing the consistence between experimental data and DG-model structures. The back-calculated 2D NOESY spectra of resulting DG structures were well consistent with experimental 2D NOESY spectra. Superposition of 20 independent structures with macrocyclic ring atoms and all atoms of F430 afforded pairwise root mean square deviations (RMSD) of 0.025-0.125 Å and 0.64-1.3 Å, respectively. The macrocyclic rings of structures are well converged to a unique conformation with saddle-shaped deformation whereas most of side chains are not converged. The average dihedral angle (N1-N2-N3-N4, 27.78±1.50°) of 20 DG-structures exhibits that the macrocyclic ring conformation is puckered as much as 12,13-diepimeric F430 (28.75±4.07°).

Complete assignments of $^{1}H$ and $^{13}C NMR$ spectra of Chivosazole F

  • Park, Jung-Rae;Jongheonn Shin;Kim, Jin-Cheol;Ahn, Jong-Woong
    • Journal of the Korean Magnetic Resonance Society
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    • v.5 no.2
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    • pp.91-98
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    • 2001
  • The $^1$H and $^{13}$ C NMR spectra of chivosazole F from Sorangium cellulosum were completely assigned by a combination of ID and 2D NMR techniques. The configurations of double bonds were confirmed from the ROESY spectra. The stereochemistry at asymmetric carboncenters was partially assigned on the basis of the results of NOE analysis.

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19F NMR Investigation of F1-ATPase of Escherichia coli Using Fluorinated Ligands

  • Jung, Seun-Ho;Kim, Hyun-Won
    • BMB Reports
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    • v.31 no.1
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    • pp.44-47
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    • 1998
  • Asymmetry amongst nucleotide binding sites of Escherichia coli $F_1$-ATPase was examined using $^{19}F$ NMR signal from fluorinated analogs of adenine nucleotides bound to nucleotide binding sites. ADP-$CF_2-{PO_3}^{2-}$ showed no inhibitory effect to $F_1$-ATPase. But ADP-CHF-${PO_3}^{2-}$ (racemic mixture) showed competitive inhibition of $F_1$-ATPase with $K_i$ of $60\;{\mu}m$. ADP-CHF-${PO_3}^{2-}$ shows only negligible binding to $EF_1$ in the absence of $Mg^2+$. With the addition of $Mg^2+$ to the medium, the $^{19}F$ resonance of free ADP-CHF-${PO_3}^{2-}$ disappeared and the new broad resonances appeared. Appearance of more than two new asymmetric resonances following the binding of ADP-CHF-${PO_3}^{2-}$ to $EF_1$ may indicate that at least one of the isomers showed split resonances. This may suggest that the region between ${\alpha}$-and ${\beta}$-phosphate of ADP-CHF-${PO_3}^{2-}$ which is bound to catalytic sites is experiencing a different environment at different sites.

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