• Title/Summary/Keyword: ^{13}C chemical shift

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$^{13}C$ Solid State NMR Study on the Dynamics of the Poly(vinyl butylal) with Various Water Contents

  • Hyun Namgoong;Kim, Jong-Soo;Han, Oc-Hee
    • Journal of the Korean Magnetic Resonance Society
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    • v.6 no.1
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    • pp.1-11
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    • 2002
  • Physical properties of PVB [Poly(vinyl butyral)] polymer are strongly correlated with water contents in the polymer. Thus dynamics of PVB containing 10~50(w/w) % of water were studied by $^{13}$ C CP/MAS/DD over the temperature range 293K -348K. From the Peak area, line width, chemical shift, and relaxation times ( $T_{1}$ $T_{1p}$) measured at 9.4 T, it was deduced that water facilitates molecular dynamics of the PVB molecules overall including conformational exchange of the racemic and meso butyaldehyde rings in the PVB. However, the influence of water was not linear to the amount of water in the PVB samples. It is suggested that water up to 30 w/w % of the sample is closely bound to the PVB polymer and water relatively free from the PVB polymer starts to appear when water is added more than 30 w/w %.%.

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A Study on the Sulfur-Resistant Catalysts for Water Gas Shift Reaction IV. Modification of $CoMo/γ-Al_2O_3$ Catalyst with K

  • Park, Jin Nam;Kim, Jae Hyeon;Lee, Ho In
    • Bulletin of the Korean Chemical Society
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    • v.21 no.12
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    • pp.1239-1244
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    • 2000
  • A study of K addition to the catalyst of CoMo/ ${\gamma}-Al_2O_3$ was studied. The catalyst with 10 at% of K to Mo atoms in 3C10M, the catalyst added 3 wt% CoO to 10 wt% $MoO_3/{\gamma}-Al_2O_3$, showed the highest activity for water gas shift reaction. The addition of K retarded the reducibility of cobalt-molybdenum catalysts. It gave, however, good dispersion and large BET surface area to the catalysts which were attributed to the disappearance of polymolybdate clustyer such as $Mo_7O_{24}^{6-}$ and the formation of small Mo$O_4^{2-}$ cluster. It was confirmed by the analyses of pore size distribution, activation energy, Raman spectroscopy, and electron diffraction. The activation energies and the frequency factors of the catalysts 3C10M and 5KC10M (the catalyst added 5 at% K for Mo to the catalyst 3C10M) were 43.1 and 47.8 kJ/mole, and 4,297 and 13,505 $sec^{-1}$, respectively. These values were also well correlated with our suggestion. These phenomena were attributed to the direct interaction between K and CoMo oxides irrelevant to the support.

Backbone 1H, 15N, and 13C Resonance Assignment and Secondary Structure Prediction of HP1298 from Helicobacter pylori

  • Kim, Won-Je;Lim, Jong-Soo;Son, Woo-Sung;Ahn, Hee-Chul;Lee, Bong-Jin
    • Journal of the Korean Magnetic Resonance Society
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    • v.12 no.2
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    • pp.65-73
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    • 2008
  • HP1298 (Swiss-Prot ID ; P65108) is an 72-residue protein from Helicobacter pylori strain 26695. The function of HP1298 was identified as Translation initiation factor IF-l based on sequence homology, and HP1298 is included in IF-l family. Here, we report the sequence-specific backbone resonance assignments of HP1298. About 97% of all the $^{1}HN$, $^{15}N$, $^{13}C{\alpha}$, $^{13}C{\beta}$, and $^{13}CO$ resonances could be assigned unambiguously. We could predict the secondary structure of HP1298, by analyzing the deviation of the $^{13}C{\alpha}$ and $^{13}C{\beta}$ shemical shifts from their respective random coil values. Secondary structure prediction shows that HP1298 consists of six $\beta$-strands. This study is a prerequisite for determining the solution structure of HP1298 and investigating the structure-function relationship of HP1298. Assigned chemical shift can be used for the study on interaction between HP1298 and other Helicobacter pylori proteins.

Effects of Li$^+$ and Ag$^+$ Ions on the Rotational Barrier in Acetamide and propionamide System

  • Kwon, Dae-Keun;Choi, Young-Sang;Yoon, Chang-Ju
    • Bulletin of the Korean Chemical Society
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    • v.7 no.1
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    • pp.1-5
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    • 1986
  • The influences of $LiNO_3\;and\;AgNO_3$ on the N-C(O) rotational barrier of N,N-dimethylacetamide and N,N-dimethylpropionamide have been investigated. The rotational activation free energy $({\Delta}G^{\neq})\;for\;Li^{+}$-amide complexes is found to increase with increasing salt concentration. On the other hand, that for $Ag^+$-amide complexes increases in the presence of $Ag^+$ ion up to 0.25 M ion concentration and then decreases as the concentration of $Ag^+$ ion is further increased. Such an unusual behavior of $Ag^+$-amide complexes has been interpreted in terms of ion-pairing and diluent effect on the amides. However, $^{13}C$ nmr chemical shift data for the amides have shown that both of these ions interact primarily with the carbonyl group in amides.

Comparison of Metal Cleaning Effect on Pt Particles Supported on Carbon and Pt Black Observed by NMR, CV, and TEM

  • Han, Kee-Sung;Han, Oc-Hee
    • Journal of the Korean Magnetic Resonance Society
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    • v.6 no.1
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    • pp.38-44
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    • 2002
  • 60% Pt on Vulcan XC-72 with similar Pt sizes to fuel cell grade Pt black was investigated by $\^$13/C nuclear magnetic resonance spectroscopy (NMR), cyclic voltammery (CV), transmission electron microscopy (TEM). Experiments were carried out on electrochemically cleaned samples as well as as-received. The TEM and CV results showed that the average particle sizes were changed by cleaning. However, the chemical shift ($\delta$$\_$G/) of $\^$13/C of $\^$13/CO absorbed on Pt surfaces did not show any appreciable variation with particle size change as did in Pt black. These results indicate that a combination of different analytic techniques is essential to understand the properties of the metal particle catalysts and that the presence of carbon black support strongly influences the NMR data, probably through metal-support interaction.

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Ginsenoside $Rg_5$, A Genuine Dammarane Glycoside from Korean Red Ginseng

  • Kim, Shin-Il;Park, Jeong-Hill;Ryu, Jae-Ha;Park, Jong-Dae;Lee, You-Hui;Park, Jae-Hyun;Kim, Tae-Hee;Kim, Jong-Moon;Baek, Nam-In
    • Archives of Pharmacal Research
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    • v.19 no.6
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    • pp.551-553
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    • 1996
  • A genuine dammarane glycoside, named ginsenoside $Rg_{5}$, has been isolated by repeated column chromatography and preparative HPLC from the MeOH extract of Korean red ginseng (Panax ginseng C.A. Meyer). The chemical structure of ginsenoside$ Rg_{5}$ was determined as $3-O-[{\beta}-D-glucopyranosyl (1{\rightarrow}2)-{\beta}-D-glucopyranosyl]$ dammar-20(22), $24-diene-3{\beta},12{\beta}-diol$ by spectral and chemical methods. The stereostructure of a double bond at C-20(22) of ginsenoside $Rg_{5}$ was characterized as (E) from the chemical shift of C-21 in the $^{13}C-NMR $and a NOESY experiment in the $^{1}H-NMR$.

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Correlation of Chemical Shifts with Substituent Parameters in N-Benzyl Derivatives of Pyrrole,3a,7a-Dihydroindole,and Indole Esters

  • Jeon, Kyu-Ok;Yu, Sook-Yu;Lee, Chang-Kiu
    • Bulletin of the Korean Chemical Society
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    • v.23 no.9
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    • pp.1241-1255
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    • 2002
  • Series of m- and p-substituted benzyl derivatives of pyrrole, tetramethyl 1-benzyl-3a,7a-dihydroindole-2,3,3a,4-tetracarboxylate, and trimethyl 1-benzylindole-2,3,4-tricarboxylate were prepared and their 13C NMR spectra were obtained in 0.1 M solutions of chloroform-d. Both single substituent parameter and dual substituent parameter analyses were carried out to correlate the substituent chemical shifts. The ${\beta}$ carbon of the indole series showed the most profound substituent effect dependence as well as the best correlation. The results are explained by the hyperconjugation of the benzyl methylene group.

HMQC vs HSQC for Small Molecules

  • Kim, Eunhee;Cheong, Hae-Kap
    • Journal of the Korean Magnetic Resonance Society
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    • v.21 no.4
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    • pp.131-134
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    • 2017
  • Proton detected Heteronuclear Multiple Quantum Coherence (HMQC) and Heteronuclear Single Quantum Coherence (HSQC) essentially provide the same information - correlation of the chemical shift of the proton to J-coupled hetero nuclei such as $^{13}C$ or $^{15}N$ nuclei. This paper is a practical note for the students who ask which one is better and which methods they use routinely. Artifact suppression using phase cycling and gradient pulses are discussed.

Chmical Shift Variation of Bovine Angiogenin Upon Binding with Phosphate ions

  • Baek, Sun-Hee;Kang, Dong-Il;Lee, Jee-Young;Shin, Hang-Cheol;Kim, Yang-Mee
    • Journal of the Korean Magnetic Resonance Society
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    • v.10 no.2
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    • pp.155-162
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    • 2006
  • Angiogenin is unique among angiogenic molecules in that it is a member of the pancreatic ribonuclease superfamily and, in fact, is a ribonucleolytic enzyme. Its enzymatic activity is extremely weak compared to that of the digestive RNases but is critical for its capacity to induce neovascularization. In this study, we completed the backbone resonance assignment of bovine angiogenin using triple resonance NMR experiments of $^{15}N\;and/or\;^{13}C$ isotope labeled protein and investigated the chemical shift variation upon binding with inhibitor phosphate ion and determine the phosphate binding site.

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H-1, C-13, and N-15 resonance assignments of ENOD40B, a plant peptide hormone

  • Young Kee Chae
    • Journal of the Korean Magnetic Resonance Society
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    • v.27 no.2
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    • pp.5-9
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    • 2023
  • t ENOD40B, a plant peptide hormone, was doubly labeled with C-13 and N-15 by recombinant production in Escherichia coli. The peptide was prepared by affinity chromatography followed by protease cleavage and reverse-phase chromatography. To elucidate the mode of action against its receptor, sucrose synthase, we proceeded to assign the backbone and side-chain resonances using a set of double and triple resonance experiments. This result will be used to determine the three-dimensional structure of the peptide at its bound state as well as to observe the chemical shift changes upon binding.