• Bulletin of the Korean Chemical Society
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• 제32권1호
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• pp.49-52
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• 2011

A dinuclear copper(II) complex of [$Cu_2(aceace)_4$(dipyph)] [aceace = acetylacetone, dipyph = 1,4-di(4-pyridylethene-2-yl-)benzene] has been synthesized and characterized by elemental analysis, IR and X-ray single crystal diffraction. It crystallizes in the monoclinic system, space group P21/c, with lattice parameters a = 7.9584(16) $\AA$, b = 18.594(4) $\AA$, c = 15.063(4) $\AA$ $\beta=120.97(2)^o$ and $M_r$ = 807.85 ($C_{40}H_{44}Cu_2N_2O_8$), Z = 2. Each of the $Cu^{2+}$ ion adopts a square pyramid geometry and coordinates with four oxygen atoms from two aceace ligands and one nitrogen atom from dipyph bidentate ligand. Magnetic measurement shows that the Weiss constant and Curie constant for the title compound are -0.22 K and 0.1154 emu K/mol, respectively. Thermal stability data indicate that the title complex undergoes two steps decomposition and the residue is $Cu_2O_4$. In the potential range of -1.5 ~ 0.8 V, the title complex represents an irreversible electrochemical process.

• 한국광물학회지
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• 제11권1호
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• pp.1-12
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• 1998

In Pohang area, basaluminite accompanying a little amounts of hydrobasalumnite, super-genetically occurs as whitish cryptocrystalline (2-4 $\mu\textrm{m}$) clay-like aggregates in the vicinity of altered carbonate concretions embedded within mudstones of the Tertiary Yeonil Group. A hydrobasaluminite changed readily into a basaluminite at room temperature in air, and, in turn, into a metabasaluminite when heating to 150$^{\circ}$~30$0^{\circ}C$. For the basaluminite, a monoclinic unit-cellparameters (a=14.845$\AA$, b=10.006$\AA$, c=11.082$\AA$, $\beta$=122.15$^{\circ}$) were calculated by X-ray powder diffraction data. Its basal reflections (001 and 002) are XRD analyses strongly indicate that the aluminum sulphate mineral has a layer structure and, at least, three types of water, i.e., (1) interlayer water (9.0 wt %), (2) crystal water (8.0 wt %), and (3) structural water (19.0 wt %). may present in its lattice. Based on TG-DTG data combined with EDS and IR analyses, a new chemical formula of Al5SO4(OH)134H2O was given to the basaluminite. Field occurrence and stable isotope data ($\delta$18O, $\delta$D, $\delta$34S) for the basaluminite seem to reflect that it was formed by the leached meteoric solution from surrounding mudstones during or after uplifting. An interaction of the acid solution with carbonate concretion and the resultant local neutralization of the fluid rich in Al3+ and SO42- are major controls on the basaluminite formation.

• 한국산학기술학회논문지
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• 제1권1호
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• pp.27-32
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• 2000

인산염계 Ag₂OㆍLi₂OㆍCaOㆍTiO₂ㆍP₂O/sub 5/ 조성에 CuO를 0.05∼l.5 mole 첨가하여 다공성 글래스 세라믹스를 제조하였으며. 제조된 모유리는 최적 핵형성을 위해 610℃. 최고 결정성장을 위해 840℃에서 열처리하였다. 1N-HC1에서 β-Ca₃(PO₄)결정상만을 선택적으로 용출하였으며 LiTi₂(PO₄)₃상과 AgTi₂(PO₄)₃결정상이 존재하는 Glass Ceramics를 제조하였다. 다공성 글래스 세라믹스의 항균효과 및 특성을 평가하였다. Staphylococcus aureus와 Salmonella typhi 균이 본 연구에 사용되었으며, 탁월한 항균효과를 나타내는 것으로 평가되었다.

• 한국표면공학회지
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• 제37권6호
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• pp.307-312
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• 2004

Extensive efforts have been made in an attempt to utilize photocatalytic properties of $TiO_2$ in visible range. $TiO_2$ and TiO-N thin films were made by the DC reactive magnetron sputtering method at $300^{\circ}C$. Various gases (Ar, $O_2$ and $N_2$) were used and Ti target was impressed by 0.6 kW-5.8 kW power range. The hysteresis phenomenon of the $TiO_2$ thin film as a function of the discharge voltage characteristic was observed to be higher as applied power increases. That of TiO-N thin film was occurred at the 5.8 kW power. The cross section and surface roughness of thin films were observed by FE-SEM and AFM. Average surface roughness of TiO-N thin film was observed as $15.9\AA$ and that of $TiO_2$ as $13.2\AA$. The crystal phases of both $TiO_2$ and TiO-N thin films were found to be anatase structure. The atomic $\beta$-N (396 eV peak in N 1s XPS) was shown in the rutile crystal of TiO-N and was considered acting as the origin of wavelength shift to the visible light.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2009년도 제38회 동계학술대회 초록집
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• pp.403-403
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• 2010

The Pt-Ni alloy is an electro-catalyst of interest in the low temperature direct methanol fuel cells(DMFCs). It has been already reported that the Pt-Ni alloy catalysts may even have enhanced activity compared to pure platinum catalyst, depending on how the surfaces are prepared. The order-disorder transition in bimetallic alloy such as $\beta$-CuZn, Cu3Au, and CuAu have been investigated greatly by x-ray diffraction. After annealing the bimetallic alloy, the crystal structure changes as observed in the order-disorder transition of Cu3Au which changes from the face centered cubic to a simple cubic structure. Pt-Ni bimetallic alloy has been already reported to have the face centered cubic structure. However, in nano-scale Pt-Ni bimetallic alloy crystals the crystal structures changes to a simple cubic structure. In this experiment, we have studied the order-disorder transition in Pt-Ni bimetallic nanocrystals. Pt/Ni thin films were deposited on sapphire(0001) substrates by e-beam evaporator and then Pt-Ni alloy were formed by RTA at 500, 600, and $700^{\circ}C$ in a vacuum environment and Pt-Ni nano particles were formed by RTA at $1059^{\circ}C$ in a vacuum environment. We measured the structure of Pt-Ni bimetallic alloy films using synchrotron x-ray diffraction and SEM.

• Molecules and Cells
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• 제42권6호
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• pp.460-469
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• 2019

Bacterial ${\alpha}-type$ carbonic anhydrase (${\alpha}-CA$) is a zinc metalloenzyme that catalyzes the reversible and extremely rapid interconversion of carbon dioxide to bicarbonate. In this study, we report the first crystal structure of a hyperthermostable ${\alpha}-CA$ from Persephonella marina EX-H1 (pmCA) in the absence and presence of competitive inhibitor, acetazolamide. The structure reveals a compactly folded pmCA homodimer in which each monomer consists of a 10-stranded ${\beta}-sheet$ in the center. The catalytic zinc ion is coordinated by three highly conserved histidine residues with an exchangeable fourth ligand (a water molecule, a bicarbonate anion, or the sulfonamide group of acetazolamide). Together with an intramolecular disulfide bond, extensive interfacial networks of hydrogen bonds, ionic and hydrophobic interactions stabilize the dimeric structure and are likely responsible for the high thermal stability. We also identified novel binding sites for calcium ions at the crystallographic interface, which serve as molecular glue linking negatively charged and otherwise repulsive surfaces. Furthermore, this large negatively charged patch appears to further increase the thermostability at alkaline pH range via favorable charge-charge interactions between pmCA and solvent molecules. These findings may assist development of novel ${\alpha}-CAs$ with improved thermal and/or alkaline stability for applications such as $CO_2$ capture and sequestration.

• Bulletin of the Korean Chemical Society
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• 제14권2호
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• pp.200-206
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• 1993

Structures of two polymorphs of ${\alpha},{\alpha}$-trehalose octaacetate monohydrate, $C_{28}H_{38}O_{19}\;{\cdot}\;H_2O$, have been studied by X-ray diffraction method. ${\alpha},{\alpha}$-trehalose (${\alpha}$-D-glucopyranosyl ${\alpha}$-D-glucopyranoside) is a nonreducing disaccharide. The polymorph I belongs to the monoclinic $P2_1$, and has unit cell parameters of a=10.725(l), b=15.110(4), c=11.199(5) ${\AA}$, ${\beta}=108.16(2)^{\circ}$ and Z=2. The polymorph II is orthorhombic $P2_12_12_1$, with a=13.684(4), b=15.802(4), c=17.990(9) ${\AA}$ and Z=4. The final R and R$_w$ values for monoclinic polymorph I are 0.043 and 0.048 and for orthorhombic polymorph II are 0.116 and 0.118, respectively. Those R values of polymorph II are high because the large thermal motions of acetyl groups and the poor quality of the crystal. The molecular conformations in the two polymorphs are similar. Both D-glucopyranosyl rings have chair $^4C_1$ conformations and atoms of glycosidic chain ${\alpha}(1{\rightarrow}1)$ linkage are coplanar. The primary acetate groups of the pyranose residues assume both gauche-trans conformations. The molecules of two polymorphs have pseudo-C$_2$ symmetry at glycosidic O(1) atom. The bond lengths and angles are normal compared with those in other acetylated sugar compounds. The molecules in the monoclinic crystal are held by the hydrogen bonds with the water molecules and by van der Waals forces.

• Bulletin of the Korean Chemical Society
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• 제14권2호
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• pp.266-271
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• 1993

The reaction of $(CO_5$)M=C(OMe)Tol (M=Cr, Mo, W and $Tol=p-C_6H_4Me)$ and $BBr_3$ followed by treatment with tetramethylethylenediamine (TMEDA) yields a mixture of two diastereomers, trans, $cis-Br(CO)_2(tmeda)M{\equiv}$CTol [M=Cr(1a), Mo(2a), W(3a)] and cis, $trans-Br(CO)_2(tmeda)M{\equiv}$CTol [M=Cr(1b), Mo(2b), W(3b)], respectively. These compounds have been isolated as crystalline solids and characterized by spectroscopic (infrared, mass, $^1H$ and $^{13}C-NMR)$ data. The trans, cis-Br(CO)2(tmeda)Cr${\equiv}$CTol (1a), has been examine via a single crystal X-ray diffraction study : $BrCrO_2N_2C_{16}H_{23}$, Mr=407.27, triclinic, $P{\bar{1}},\;a=12.792(2),\;b=13.400(5),\;c= 11.645(4)\;{\AA},\;{\alpha}=101.26(2)^{\circ},\;{\beta}=103.04(2)^{\circ},\;{\gamma}=91.88(2)^{\circ},\;{\nu}=1907(1){\AA}^3,\;Z=2,\;{\rho}(calcd)=1.418\;gcm^{-3},\;{\lambda}(MoK{\alpha})=0.71069\;{\AA},\;{\mu}=26.25 cm^{-1},\;F(000)=831.97,\;T=295K,\;R=0.0977$ for 1332 significant reflections $[F_0>5{\sigma}(F_0)]$. There are two essentially equivalent molecules in the crystallographic asymmetric unit. Each molecule is octahedral with the bromide ligand trans to the alkylidyne carbon, the two cis-carbonyl ligands, and the bidentate TMEDA ligand.

• Bulletin of the Korean Chemical Society
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• 제13권4호
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• pp.363-367
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• 1992

The crystal structure of (1,3,6,9,11,14-hexaazatricycol[12.2.1.$1^{6,9}$]octadecane)copper(Ⅱ) perchlorate, Cu($C_{12}H_{26}N_6$)$(ClO_4)_2$, has been determined by the X-ray diffraction methods. The crystal data are as follows: Mr=516.9, triclinic, ${\alpha}=8.572\;(2)$, b=8.499 (3), c=15.204 (3) ${\AA}$, ${\alpha}=80.42\;(5),\;{\beta}=73.57\;(3),\;{\gamma}=69.82\;(4)^{\circ},\;V=994.2\;{\AA}^3,\;D_C=1.726\;gcm^{-3}$, space group $P{\tilde{1}},\;Z=2,\;{\mu}=21.27\;cm^{-1}&, F(000)=534 and T=297 K. The structure was solved by direct methods and refined by full-matrix least-squares methods to and R value of 0.081 for 1608 observed reflections measured with graphite-mono-chromated Mo Ka radiation on a diffractometer. There are two independent complexes in the unit cell. The two copper ions lie at the special positions (1/2, 0, 0) and (0, 1/2, 1/2)and each complex possesses crystallographic center of symmetry. Each Cu ion is coordinated to four nitrogen donors if the hexaazamacrotricyclic ligand and weakly interacts with two oxygen atoms of the perchlorate ions to form a tetragonally distorted octahedral coordination geometry. The Cu_N (sec), Cu_N(tert) and Cu_O coordination distances are 1.985 (14), 2.055 (14) and 2.757 (13) ${\AA}$ for the complex A and 1.996 (10), 2.040 (11) and 2.660 (13) ${\AA}$ for the complex B, respectively. The macrocycles in the two independent cations assume a similar conformation with the average r.m.s. deviation of 0.073 ${\AA}$. Two 1,3-diazacyclopentane ring moieties of the hexaazamacrotricyclic ligand are placed oppositely and almost perpendicularly to the square coordination plane of the ruffled 14-membered macrocycle. The secondary N atoms are hydrogen-bonded to the perchlorate O atoms with distances of 3.017 (23) and 3.025 (19) ${\AA}$ for the complexes A and B, respectively.

• 분석과학
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• 제21권6호
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• pp.562-568
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• 2008

A novel two-dimensional cadmium(II)-nickel(II) bimetallic host clathrate, $[Cd{NH_2CH_2CH_2OH}_2Ni(CN)_4]{\cdot}3C_6H_5NH_2{\cdot}H_2O$, 1, has been synthesized and structurally characterized by X-ray single crystallographic method. The clathrate 1 crystallizes in the monoclinic system, space group $P2_1/c$ with a = 14.370(3), b = 7.728(1), c = 28.172(4) ${\AA}$, ${\beta}=97.58(1)^{\circ}$, V = 3101.1(9) ${\AA}^3$, Z = 4. The host framework of the clathrate 1 is built of the cyanide bridges between octahedral Cd(II) atom and square planar Ni(II) atom. The octahedral Cd atoms ligated by two 2-aminoethanol molecules and four cyanide ligands bridged with square planar Ni atoms. The Ni atoms bridges to four Cd atoms via cyanides is made up of puckered quadrangles of composition $\{CdNi(CN)_2\}_2$, all edges are shared. This cyanide bridges form an infinite two-dimensional host networks stacking along b axis. 2-Aminoethanol ligands bond to Cd atom through N atom as a monodentate ligand in the axial position and four cyanides take an equatorial plane with all in trans-configurations. The aniline guest molecules and water molecules are located in between the host layer sheets, respectively.