• Bulletin of the Korean Chemical Society
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• 제33권5호
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• pp.1647-1652
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• 2012

With the objective to design and synthesis of Schiff's base symmetrical liquid crystal dimmers and to study the effect of molecular structure variation ($o-ortho$, $m-meta$, $p-para$) and change in alkoxy terminal chain length on mesomorphic properties of liquid crystals, We have synthesized Schiff base dimers from dialdehyde derivative containing 2-hydroxy-1,3-dioxypropylene as short spacer with aniline derivatives having different lengths of terminal alkoxy chains ($n$ = 5, 7, 9). The chemical structure of the final products was characterized by proton nuclear magnetic resonance ($^1H$ NMR) spectroscopy and fourier transform infrared (FT-IR) spectroscopy. The mesomorphic properties and optical textures of the resultant dimers were characterized by differential scanning calorimetry (DSC) and polarized optical microscopy (POM). The existence of smectic A phase transition was confirmed by the observation of batonnets and fan shaped textures in optical microscopy when compound were heated from crystalline phase. All of the dimers of this series, with the exception of $\mathbf{2S_5}$ -ortho, -meta, -para, were thermotropic liquid crystal. The compound $\mathbf{2S_9}$ -meta was monotropic, while the rest were enantiotropic. It was found that the change in terminal alkoxy chain length has pronounced effect on the mesomorphic properties. The temperature range of smectic A phase window widens with increasing alkoxy chain length.

• Bulletin of the Korean Chemical Society
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• 제30권5호
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• pp.1113-1117
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• 2009

The one-dimensional coordination polymers, $[Cu^{II}(L)(NO_3)_2]_n$ (1) and {$[Cu^{II}(L)(NO_3)]{\cdot}2H_2O}_{2n} (2), were synthesized from $Cu(NO_3)_2{\cdot}3H_2O$ and 2-[(pyridin-3-ylmethyl)amino]ethanol (L, PMAE) in methanol by controlling the molar ratio of copper(II) salt. Copper(II) ion in 1 has one pyridine group of PMAE whose an aminoethanol group coordinates adjacent copper(II) ion. As the pyridine group is bonded to neighboring copper(II) ion, 1 becomes a one-dimensional chain. Contrary to 1, the structure of 2 shows that the oxygen atom of ethoxide group is bridged between two copper(II) ions, which forms a dinuclear complex. Additionally, the pyridine group of PMAE included one dinuclear unit is coordinated to the other dimeric one each other, which leads to a one-dimensional polymer. Due to the structural differences, 1 exhibits weak antiferromagnetic interaction, while 2 shows strong antiferromagnetic interaction. Due to direct spin exchange via oxygen of PMAE 2 has a much strong spin coupling than 1.

• Bulletin of the Korean Chemical Society
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• 제31권6호
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• pp.1665-1668
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• 2010

The spin exchange interactions of $(VO)_2(H_2O){O_3P-(CH_2)_3-PO_3}{\cdot}2H_2O$ were examined by spin dimer analysis based on extended Huckel tight binding method. The strongest spin exchange interaction occurs through the super-superexchange path $J_2$ and the second strongest spin exchange interaction occurs through the superexchange interaction path $J_1$. There are two strongly interacting spin exchange paths in $(VO)_2(H_2O){O_3P-(CH_2)_3-PO_3}{\cdot}2H_2O$. Therefore, magnetic susceptibility curve of $(VO)_2(H_2O){O_3P-(CH_2)_3-PO_3}{\cdot}2H_2O$ can be well reproduced by an alternating onedimensional antiferromagnetic chain model rather than an isolated spin dimer model.

• Advances in materials Research
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• 제3권2호
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• pp.117-128
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• 2014

Processable conducting polyaniline derivative with free amine functional groups was successfully synthesized from the monomer o-phenylenediamine in aqueous hydrochloric acid medium using ammonium persulfate as an oxidative initiator. The synthesized poly(o-phenylenediamine) (PoPD) in critical condition was found to be completely soluble in common organic solvents like dimethyl sulfoxide, N,N-dimethyl formamide etc. From the intrinsic viscosity measurement, the optimum condition for the polymerization was established. The polymer was characterized by ultraviolet visible spectroscopy, Fourier transform infrared spectroscopy, proton magnetic resonance spectroscopy ($^1HNMR$) and thermogravimetric (TGA) analyses. The weight average molecular weights of the synthesized polymers were determined by the dynamic light scattering (DLS) method. From the spectroscopic analysis the structure was found to resemble that of polyaniline derivative with free amine functional groups attached to ortho/meta position in the phenyl ring. However, very little ladder unit was also present with in the polymer chain. The moderate thermal stability of the synthesized polymer could be found from the TGA analysis. The average DC conductivity of $2.8{\times}10^{-4}S/cm$ was observed for the synthesized polymer pellet after doping with hydrochloric acid.

• Bulletin of the Korean Chemical Society
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• 제33권1호
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• pp.60-64
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• 2012

Silver(I) [bis(alkylthio)methylene]malonates were synthesized from the reaction of silver nitrate and potassium [bis(alkylthio)methylene]malonates. The structures of the Ag complexes were characterized with nuclear magnetic resonance (NMR), inductively coupled plasma atomic emission spectrometry (ICP-AES) and elemental analysis. Ag nanoparticles (NPs) were obtained from the decomposition of the Ag complexes in 1,2-dichlorobenzene at $110^{\circ}C$ without an additional surfactant. The average sizes of the Ag NPs are in the range of 5.1-6.3 nm and could be controlled by varying the length of the alkyl chain. The optical properties, crystalline structure and surface composition of Ag NPs were characterized with ultraviolet-visible (UV-visible) spectroscopy, transmission electron microscopy (TEM), X-ray diffraction (XRD), gas chromatography-mass spectrometry (GC-MS), X-ray Photoelectron Spectroscopy (XPS) and thermal gravimetric analysis (TGA).

• Elastomers and Composites
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• 제55권4호
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• pp.263-269
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• 2020

Novel flexible terpolymers with a reactive moiety were synthesized by coordination polymerization with a metallocene catalyst and a cocatalyst system. C2-symmetric rac-Et(Ind)2ZrCl2 and tri-iso-butylaluminum/dimethylanilinium tetrakis (pentafluorophenyl) borate were employed as the catalyst and cocatalyst, respectively. We synthesized reactive terpolymers consisting of ethylene, a high α-olefin content (1-hexene, 1-octene, 1-decene, and 1-dodecene), and divinylbenzene. The structure and composition of the terpolymers were characterized by 1H-nuclear magnetic resonance analysis. The catalytic activity, polymer yield, molecular weight, and molecular weight distribution were measured as functions of the chain length and high content of α-olefins. Furthermore, the thermal properties and crystallinity of the terpolymers were determined by differential scanning calorimetry and wide-angle X-ray scattering.

• Bulletin of the Korean Chemical Society
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• 제33권8호
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• pp.2508-2512
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• 2012

Cold shock proteins (CSPs) are a family of proteins induced at low temperatures. CSPs bind to single-stranded nucleic acids through the ribonucleoprotein 1 and 2 (RNP 1 and 2) binding motifs. CSPs play an essential role in cold adaptation by regulating transcription and translation via molecular chaperones. The solution nuclear magnetic resonance (NMR) or X-ray crystal structures of several CSPs from various microorganisms have been determined, but structural characteristics of psychrophilic CSPs have not been studied. Therefore, we optimized the purification process to obtain highly pure Lm-Csp and determined the three-dimensional structure model of Lm-Csp by comparative homology modeling using MODELLER on the basis of the solution NMR structure of Bs-CspB. Lm-Csp consists of a ${\beta}$-barrel structure, which includes antiparallel ${\beta}$ strands (G4-N10, F15-I18, V26-H29, A46-D50, and P58-Q64). The template protein, Bs-CspB, shares a similar ${\beta}$ sheet structure and an identical chain fold to Lm-Csp. However, the sheets in Lm-Csp were much shorter than those of Bs-CspB. The Lm-Csp side chains, E2 and R20 form a salt bridge, thus, stabilizing the Lm-Csp structure. To evaluate the contribution of this ionic interaction as well as that of the hydrophobic patch on protein stability, we investigated the secondary structures of wild type and mutant protein (W8, F15, and R20) of Lm-Csp using circular dichroism (CD) spectroscopy. The results showed that solvent-exposed aromatic side chains as well as residues participating in ionic interactions are very important for structural stability. Further studies on the three-dimensional structure and dynamics of Lm-Csp using NMR spectroscopy are required.

• 한국자기공명학회논문지
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• 제19권2호
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• pp.74-82
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• 2015

Ryanodine receptor (RyR) is one of the two major $Ca^{2+}$ channels in membranes of intracellular $Ca^{2+}$ stores and is found in sarcoplasmic reticulum (SR), endoplasmic reticulum (ER). RyR1 is also the major calmodulin-binding protein of sarcoplasmic reticulum membranes. Residues 4064-4210 in the RyR1 polypeptide chain has similar primary sequence with calmodulin (CaM) and was designated as CaM-like domain (CaMLD). When expressed as a recombinant peptide, CaMLD showed several CaM-like properties in previous studies. Still, previous studies of CaMLD were focused on protein-protein interactions rather than its own properties. Here, we studied the expression of CaMLD and its sub-domains corresponding to each lobe of CaM in Escherichia coli. CaMLD could be obtained only as inclusion body, and it was refolded using urea solubilization followed by dialysis. Using spectroscopic approaches, such as NMR, circular dichroism, and gel filtration experiment, we found that the refolded CaMLD exists as nonspecific aggregate, even though it has alpha helical secondary structure. In comparison, the first half of CaMLD (R4061-4141) could be obtained as natively soluble protein with thioredoxin fusion. After the removal of the fusion tag, it exhibited folded and helical properties as shown by NMR and circular dichroism experiments. Its oligomeric status was different from CaMLD, existing as dimeric form in solution. However, the second half of the protein could not be obtained as soluble protein regardless of fusion tag. Based on these results, we believe that CaMLD, although similar to CaM in sequence, has quite different physicochemical properties and that the second half of the protein renders it the aggregative properties.

• 한국수소및신에너지학회논문집
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• 제33권3호
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• pp.209-218
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• 2022

Recently, research on the development of anion exchange membranes (AEMs) has received considerable attention from the scientific community around the world. Here, we fabricated a series of AEMs with branched structures with different alkyl spacers and conducted comparative evaluations. The introduction of these branched structures is an attempt to overcome the low ionic conductivity and stability problems that AEMs are currently facing. To this end, branched polymers with different spacer lengths were synthesized and properties of each membrane prepared according to the branched structure were compared. The chemical structure of the polymer was investigated by proton nuclear magnetic resonance, Fourier transform infrared, and gel permeation chromatography, and the thermal properties were investigated using thermogravimetric analysis. The branched anion exchange membrane with (CH₂)₃ and (CH₂)₆ spacers exhibited ionic conductivities of 8.9 mS cm^-1 and 22 mS cm^-1 at 90℃, respectively. This means that the length of the spacer affects the ionic conductivity. Therefore, this study showing the effect of the spacer length on the ionic conductivity of the membrane in the polymer structure constituting the ion exchange membrane is judged to be very useful for future application studies of AEM fuel cells.

• 대한화학회지
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• 제45권3호
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• pp.242-246
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• 2001

사성분계 thiophosphates, $A_2NiP_2S_6>(A=Rb$, Cs)를 halide fluxes 법으로 합성하였으며 단결정 X-ray 회절방법으로 결정 구조를 해석하였다. 이 화합물들을 $C_{2h}^5-P2_1/n$ 의 공간군을 가지며, $Rb_2NiP_2S_6$의 경우 a=5.960(2), b=12.323(4), $c=7.491(3)\AA$, $\beta=97.05(3)^{\circ}$, $V=546.0(3)\AA^3$이고$Cs_2NiP_2S_6$의 경우 a=5.957(4),b=12.696(7), $c=7.679(4)\AA$, $\beta=93.60(5)^{\circ}$, $V=579.7(5)\AA^3$인 격자상수를 갖는다. 이 두화합물은 동일한 결정 구조를 갖는다. 이들의 구조는 결정학적인 a축을 따라 성장한 1차원적인 무한사슬 $_{\infty}^1[NiP_2S_6^{2-}]$로 구성되어 있으며 이 사슬들은 알칼리 금속과의 정전기적 인력을 통하여 안정화 되어있다. Ni원자는 6개의 S원자에 의해 팔면체 배위를 하고 있고, Ni$S_6$팔면체는 $[P_2S_6^{4-}]$ 음이온 3개의 $\mu-S$ 원자들에 의해 연결되어 무한 1차원적인 사슬을 형성한다. $Cs_2NiP_2S_6$에 대한 자화율 측정결과 Neel temperature($T_N$)에 상응하는 8K 이하에서 superexchange를 통한 반자기성 magnetic coupling을 발견하였다. $T_N$이상의 온도에서는 Curie-Weiss법칙을 따른다. 자기 모멘트, C(Curie), 그리고 $\theta$(Weiss Constant)는 각각 2.77 B.M., 0.9593K, 그리고 -19.02K 이다. 측정 결과로부터 얻은 유효 자기 모멘트는 spin-only $Ni^{2+}d^8$(2.83 B.M.)계의 결과와 일치한다.