• Bulletin of the Korean Chemical Society
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• v.20 no.1
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• pp.65-68
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• 1999

Novel mononuclear group 13 metal complexes with the formula (R2M){NC5H4C(CH3)NNC(S)NH(C6H5)} (M=Al, R=iC4H9 (1); M=Ga, R=iC4H9 (2); M=Al, R=CH2SiMe3 (3); M=Ga, R=CH2SiMe3 (4)) result when 2-acetyl pyridine 4-phenyl-thiosemicarbazone ligand is mixed with trialkyl aluminum or trialkylgallium. These compounds 1-4 are characterized by microanalysis, NMR (1H, 13C) spectroscopy, mass spectra, and singlecrystal X-ray diffraction. X-ray single-crystal diffraction analysis reveals that 1 is mononuclear metal compound with coordination number of 5 and N, N, S-coordination mode.

• Journal of the Korean Magnetic Resonance Society
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• v.25 no.2
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• pp.12-16
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• 2021

Daphnia magna is used as target organism for environmental metabolomics. The metabolome of D. magna was studied with NMR spectroscopy. Most studies used the extract of D. magna, but the reproducibility cannot be obtained using extracted sample. In this study, lyophilized D. magna samples were analyzed with two different ¹H NMR techniques, HR-MAS on intact tissues and solution NMR on extracted tissues. Samples were measured three times using 600 MHz NMR spectrometer. Metabolite extraction required more than twice as many D. magna, but the metabolite intensity was lower in solution NMR. In the spectra of HR-MAS NMR, the lipid signal was observed, but they did not interfere with metabolite profiling. We also confirmed the effect of swelling time on signal intensities of metabolites in HR-MAS NMR, and the results suggest that appropriate swelling should be used in lyophilized D. magna to improve the accuracy of metabolite profiles.

• Journal of Ginseng Research
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• v.40 no.3
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• pp.245-250
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• 2016

Background: Ginsenosides are the major effective ingredients responsible for the pharmacological effects of ginseng. Malonyl ginsenosides are natural ginsenosides that contain a malonyl group attached to a glucose unit of the corresponding neutral ginsenosides. Methods: Medium-pressure liquid chromatography and semipreparative high-performance liquid chromatography were used to isolate purified compounds and their structures determined by extensive one-dimensional- and two-dimensional nuclear magnetic resonance (NMR) experiments. Results: A new saponin, namely malonyl-ginsenoside Re, was isolated from the fresh flower buds of Panax ginseng, along with malonyl-ginsenosides Rb1, Rb2, Rc, Rd. Some assignments for previously published $^1H$- and $^{13}C$-NMR spectra were found to be inaccurate. Conclusion: This study reports the complete NMR assignment of malonyl-ginsenoside Re, $Rb_1$, $Rb_2$, Rc, and Rd for the first time.

• Journal of the Korean Magnetic Resonance Society
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• v.14 no.2
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• pp.88-104
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• 2010

Human melanocortin-4 receptor (hMC4R) has a critical role in part of energy homeostasis, and their heterozygous mutations related in genetic cause of severe human obesity. In order to study the structure and function of these membrane proteins, it is important to prepare the samples. However, the preparation of transmembrane peptide is seriously difficult and time-consuming. Overexpression and purification of membrane proteins was reported to be difficult due to their innate insoluble and toxic properties. Among the many difficulties, the most important is the difficulty in obtaining sufficient quantities of purified protein. Recently, we succeed to produce large amounts of the second transmembrane domain from the wild-type hMC4R (wt-TM2) and D90N mutant hMC4R (m-TM2) and proposed the structural difference of them in membrane-like environments. In this paper, we demonstrate the optimization procedures to express and purify wt-TM2 or m-TM2 peptides, and solution NMR studies in different detergents to get high-resolution spectra were also described.

• Bulletin of the Korean Chemical Society
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• v.35 no.5
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• pp.1317-1322
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• 2014

Membrane disruption by an antimicrobial peptide (AMP) was investigated by measuring the $^2H$ solid-state nuclear magnetic resonance spectra of 1-palmitoyl-$d_{31}$-2-oleoyl-sn-glycero-3-phosphatidylcholine (POPC_$d_{31}$) in mixtures of POPC_$d_{31}$/cholesterol and either magainin 2 or aurein 3.3 deposited on thin cover-glass plates. The line shapes of the experimental $^2H$ solid-state nuclear magnetic resonance (SSNMR) spectra were best simulated by assuming the coexistence of a mosaic spread of bilayers containing pore structures and a fasttumbling isotropic phase or a hexagonal phase. Within a few days of incubation in a hydration chamber, an isotropic phase and a pore structure were induced by magainin 2, while in case of aurein 3.3 only an isotopic phase was induced in the presence of a bilayer phase. After an incubation period of over 100 days, alignment of the bilayers increased and the amount of the pore structure decreased in case of magainin 2. In contrast with magainin 2, aurein 3.3 induced a hexagonal phase at the peptide-to-lipid ratio of 1/20 and, interestingly, cholesterol was not found in the hexagonal phase induced by aurein 3.3. The experimental results indicate that magainin 2 is more effective in disrupting lipid bilayers containing cholesterol than aurein 3.3.

• Macromolecular Research
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• v.12 no.1
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• pp.100-106
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• 2004

We have prepared the polymethylene-bridged, dinuciear, half-sandwich constrained geometry catalysts (CGC)［Zr(η$\^$5/:η$^1$-C$\_$9/H$\_$5/SiMe$_2$NCMe$_3$)］$_2$［(CH$_2$)$\_$n/］［n=6(9), n=12(10)］by treating 2 equivalents of ZrCl$_4$with the corresponding tetralithium salts of the ligands in toluene. $^1$H and $\^$13/C NMR spectra of the synthesized complexes provide firm evidence for the anticipated dinuciear structure. In $^1$H NMR spectra, two singlets representing the methyl group protons bonded at the Si atom of the CGC are present at 0.88 and 0.64 ppm, which are considerably downfield positions relative to the shifts of 0.02 and 0.05 ppm of the corresponding ligands. To investigate the catalytic behavior of the prepared dinuciear catalysts, we conducted copolymerizations of ethylene and styrene in the presence of MMAO. The prime observation is that the two dinuclear CGCs 9 and 10 are not efficient for copo-lymerization, which definitely distinguishes them from the corresponding titanium-based dinuclear CGC. These species are active catalysts, however, for ethylene homopolymerization; the activity of catalyst 10, which contains a 12-methylene bridge, is larger than that of 9 (6-methylene bridge), which indicates that the presence of the longer bridge between the two active sites contributes more effectively to facilitate the polymerization activity of the dinuciear CGC. The activities increase as the polymerization temperature increases from 40 to 70$^{\circ}C$. On the other hand, the molecular weights of the polyethylenes are reduced when the polymerization temperature is increased. We observe that dinuciear metallocenes having different-length bridges give different polymerization results, which reconfirms the significant role that the nature of the bridging ligand has in controlling the polymerization properties of dinuclear catalysts.

• Journal of the Korean Magnetic Resonance Society
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• v.16 no.2
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• pp.162-171
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• 2012

SAV2228 has an OB (Oligomer-Binding)-motif which is frequently used for nucleic acid recognition. To characterize the activity of translation initiation factor-1 (IF-1) from Staphylococcus aureus, SAV2228 was expressed and purified in Escherichia coli. We acquired 3D NMR spectra showing well dispersed and homogeneous signals which allow us to assign 94.4% of all $^1HN$, $^{15}N$, $^{13}C{\alpha}$, $^{13}C{\beta}$ and $^{13}CO$ resonances. We could predict a secondary structure of SAV2228 using TALOS and CSI from NMR data. SAV2228 was consisted of one ${\alpha}$-helix and five ${\beta}$-sheets. The predicted secondary structure, ${\beta}-{\beta}-{\beta}-{\alpha}-{\beta}-{\beta}$, was similar to other bacterial IF-1, but it was not completely same to the eukaryotic one. Assigned NMR peaks and secondary structre prediction can be used for the study on interaction with nucleic acid in the future.

• Bulletin of the Korean Chemical Society
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• v.18 no.3
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• pp.311-316
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• 1997

The synthesis and characterization of the mononuclear group 13 heterocyclic carboxaldehyde methyldithiocarbazate complexes Me2M[NC5H4CRNNC(S)SCH3] (M=Al, R=H(1); M=Ga, R=H(2); M=Al, R=CH3(3); M-Ga, R=CH3(4); M=In, R=CH3(5)) are described. Compounds 1-5 were prepared by the reaction of MMe3 (M=Al, Ga, In) with 2-formy or 2-acetylpyridine-S-methyldithiocarbazate in toluene. These compounds 1-5 have been characterized by microanalysis, NMR (1H, 13C) spectroscopy, mass spectra, and single-crystal X-ray diffraction. X-ray single-crystal diffraction analyses reveal that 4-5 are mononuclear metal compounds with coordination number of 5 and N,N,S coordination mode.

• Journal of the Korean Chemical Society
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• v.32 no.6
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• pp.536-542
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• 1988

A nickel(Ⅱ) complex, Ni(IAA-NBz) (IAA-NBz') with ligand, N-benzylisonitrosoacetyl acetone imine (H-IAA-NBz) has been synthesized. This complex is very stable at room temperature and has cis-form and trans-form isomers. The ratio of nickel (Ⅱ) ion and ligand combined is 1 : 2. The elemental analysis, ir, nmr. electronic spectra and mass spectra have been studied. It is suggested from these studies that the isonitroso group of one ligand, H-IAA-NBz coordinates to nickel(Ⅱ)ion through the nitrogen atom to form five-membered ring, while that of the other ligand, H-IAA-NBz coordinates to nickel (Ⅱ) ion through the oxygen atom to form six-membered ring in square-planar complex.

• Bulletin of the Korean Chemical Society
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• v.23 no.11
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• pp.1629-1634
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• 2002

Reaction of tetrahomodioxa p-phenylcalix[4]arene with alkyl halide and NaH in DMF leads to the title tetra-alkylated derivatives, 7,13,21,27-tetra-phenyl-29,30,31,32-tetraalkyloxy-2,3,16,17-tetrahomo-3,17-dioxacalix [4]arenes, their preferred conformations were determined by NMR spectra as C-1,2-alternate. The molecular structure of allyl derivative has been solved by X-ray diffraction methods. The molecules have a conformation with pseudo center of symmetry. The benzene ring A is up, ring C is down, B and D rings are flat with respect to the plane of the macrocyclic ring.