• Journal of the Korean Chemical Society
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• v.36 no.4
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• pp.536-539
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• 1992

Eight-membered ring spiro orthocarbonate (C$_{25}H_{20}O_4$, M$_r$ = 384) is monoclinic, space group C2/c, with a = 15.319(4), b = 9.057(3), c = 13.168(3)${\AA}$, ${\beta}$ = 98.53(3)$^{\circ}$, Z = 4, F(000) = 808, T = 290 K, ${\mu}$(Mo-K${\alpha}$) = 0.55 cm$_1$, D$_c$ = 1.36 g/cm$^3$ and D$_m$ = 1.40 g/cm$^3$. The intensity data were collected with Mo-K${\alpha}$ radiation (${\lambda}$ = 0.7107 ${\AA}$) on an automatic four-circle diffractometer with a graphite monochromater. The structure was solved by direct methods and refined by full matrix least-squares methods. The final R value was 0.052 for 1412 observed reflections. The molecule has C$_2$point symmetry. The eight-membered ring has a chair conformation with pseudo-C$_s$ symmetry. The naphthyl ring is planar with the C-C bond lengths being in the range of 1.352∼1.444${\AA}$ and bond angles of 117.2∼123.5$^{\circ}$. The bond lengths of C(1)-C(9), C(8)-C(9) and C(9)-C(10) are somewhat longer than those of the other C-C bonds.

• Bulletin of the Korean Chemical Society
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• v.15 no.1
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• pp.37-45
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• 1994

$(NH_4)_{4.5}[H_{3.5}{\alpha}-PtMo_6O_{24}]{\cdot}1.5\;H_2O(A),\;(NH_4)_4[H_4{\beta}-PtMo_6O_{24}]{\cdot}1.5\;H_2O(B),\;and\;K_{3.5}[H_{4.5}{\alpha}-PtMo_6O_{24}]{\cdot}3\;H_2O(C)$ have been synthesized and their molecular structures have been also determined by single-crystal X-ray diffraction technique. The space groups, unit cell parameters, and R factors are as follows: Compound A, monoclinic, $A_{2/a}$, a= 19.074 (3), b=21.490 (3), c=15.183 (2) ${\AA};\;{\beta}$=109.67 (1) ${\AA}$; z=8; R=0.075($IF_0I>4{\sigma}(IF_0I);$ Compound B, triclinic, P$bar{1}$, a=10.776 (2), b=15.174 (4), c=10.697 (3) ${\AA};\;{\alpha}$ =126.29 (2), ${\beta}$=111.55 (2), ${\gamma}$=93.18 (2) ${\AA}$; Z=2; R=0.046($IF_0I>3{\sigma}(IF_0I);$): Compound C, triclinic, Pl, a=12.426 (2), b=13.884 (2), c=10.089 (1) ${\AA}$; ${\alpha}$=102.59 (2), ${\beta}$=110.73 (1), ${\gamma}$=53.93 (1) ${\AA}$; Z=2; R=0.074 ($IF_0I>3{\sigma}(IF_0I)$. Compounds A and C contain the well-known Anderson structure (planar structure) heteropoly oxometalate having approximate $bar{3}_m(D_{3d})$ symmetry, while compound B contains the bent structure heteropoly oxometalate having appproximate $2_{mm}(C2_v)$ symmetry. The bent structure and the planar one are geometrical isomers. These compounds are rot only novel heteroply molybdates containing platinate(IV) but also the first example of geometrical isomerism in the hexamolybdoheteropoly oxometalates. That isomerization surprisingly occurred because of the change of only 0.5 non-acidic hydrogen atom attached to the polyanion such as $[H_{3.5}{\alpha} -PtMo_6O_{24}]^{4.5-}{\to}[H_4{\beta}-PtMo_6O_{24}]^{4-}{\to}[H_{4.5}{\alpha} -PtMo_6O_{24}]^{3.5-}$. It seems that the gradual protonation of the polyanion plays an important role in that isomerism. These heteropolyanions form dimers by strong hydrogen bonds between two heteropolyanions in the respective crystal system.

• Bulletin of the Korean Chemical Society
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• v.14 no.4
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• pp.439-444
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• 1993

The aerobic oxidation of the Fe(II) complex of 1,4,8,11-tetraazacyclotetradecane, [Fe(cyclam)$(CH_3CN)_2](ClO_4)_2$, in MeCN in the presence of a few drops of $HClO_4$ leads to low spin Fe(III) species [Fe(cyclam)$(CH_3CN)_2](ClO_4)_3$. The Fe(III) cyclam complex is further oxidized in the air in the presence of a trace of water to produce the deep green binuclear bismacrocyclic Fe(II) complex $[Fe_2(C_{20}H_{36}N_8)(CH_3CN)_4](ClO_4)_4{\cdot}2CH_3CN$. The Fe(II) ions of the complex are six-coordinated and the bismacrocyclic ligand is extensively unsaturated. $[Fe_2(C_{20}H_{36}N_8)(CH_3CN)_4](ClO_4)_4{\cdot}2CH_3CN$ crystallizes in the monoclinic space group $P2_1/n$ with a= 13.099 (1) ${\AA}$, b= 10.930 (1) ${\AA}$, c= 17.859 (1) ${\AA}$, ${\beta}$= 95.315 $(7)^{\circ}$, and Z= 2. The structure was solved by heavy atom methods and refined anisotropically to R values of R= 0.0633 and $R_w$= 0.0702 for 1819 observed reflections with F > $4{\sigma}$ (F) measured with Mo K${\alpha}$ radiation on a CAD-4 diffractometer. The two macrocyclic units are coupled through the bridgehead carbons of ${\beta}$-diimitie moieties by a double bond. The double bonds in each macrocycle unit are localized. The average bond distances of $Fe(II)-N_{imine}$, $Fe(II)-N_{amine}$, and $Fe(II)-N_{MeCN}$ are 1.890 (5), 2.001 (5), and 1.925 (6) ${\AA}$, respectively. The complex is diamagnetic, containing two low spin Fe(II) ions in the molecule. The complex shows extremely intense charge transfer band in the near infrared at 868 nm with ${\varepsilon}$= 25,000 $M^{-1}cm^{-1}$. The complex shows a one-electron oxidation wave at +0.83 volts and two one-electron reduction waves at -0.43 and-0.72 volts vs. Ag/AgCl reference electrode. The complex reacts with carbon monoxide in $MeNO_2$ to form carbonyl adducts, whose $v_{CO}$ value (2010 $cm^{-1}$) indicates the ${\pi}$-accepting property of the present bismacrocyclic ligand.

• The Journal of Korean Academy of Prosthodontics
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• v.59 no.2
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• pp.190-200
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• 2021

Purpose. The aim of this study was to evaluate biaxial flexural strength and hardness of colored monolithic zirconia after dipping in different time intervals of coloring solution. Materials and Methods. Disk shaped specimens were prepared from monolithic zirconia (Eclipse V2.0, AMS, Gimpo, Korea). Four experimental groups were categorized (n = 12) due to coloring time (PU (0s); ST (8s); OV (1 min); PS (preshade)), to evaluate biaxial flexural strength and Vickers hardness. After fracture, X-ray diffraction analysis was performed using fractured specimens. Results were analyzed with one-way ANOVA test. Results. There was no significant difference between groups in the biaxial flexural strength test. However, in the Vickers hardness test, the group with standard dipping time (ST) showed significantly higher value than the group without dipping in coloring liquid (PU)(P=.038). Also, there was no significant difference in the rest of the groups (P>.05). As a result of X-ray diffraction analysis, specific peaks of tetragonal phase were shown and the volume of monoclinic phase fraction was lower than 25%. Conclusion. Although this study has several limitations, coloring liquids had no significant effect on biaxial flexural strength. Vickers hardness was significantly different between the group to which the coloring liquid was applied and the group to which the coloring solution was not applied, but there was no significant difference between the other groups. Also, the flexural strength of monolithic zirconia corresponds to Class 5 of the minimal flexural strength standard according to the use of dental ceramics.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.33 no.5
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• pp.167-173
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• 2023

Li₃V₂(PO₄)₃ and Li₃V₂(PO₄)₃/C composite with single phase monoclinic structure for the cathode materials are successfully synthesized by direct co-precipitation method using N₂H₄·H₂O as the reducing agent and alginic acid as the carbon source, and their electrochemical properties were compared. The particles with approximately 1~2 ㎛ size and the uniform spherical-like morphology of the narrow particle size distribution were obtained. In addition, the residual carbon can also improve the electrical conductivity. The Li₃V₂(PO₄)₃/C composite has improved initial specific discharge capacity and excellent cycle characteristics to maintain capacity stably than Li₃V₂(PO₄)₃. The results indicate that the reducing agent and carbon composite can affect the good crystallinity and electrochemical performance of the cathode materials.

• Journal of the Mineralogical Society of Korea
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• v.24 no.4
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• pp.265-278
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• 2011

Clayey ores of the Jeonnam province mainly consist of pyrophyllite (monoclinic), kaolinite (1T), and minor amounts of quartz, muscovite, and feldspars. Mineralogical studies revealed that two kinds of clay minerals were mainly produced from the volcanic sediments with similar ages and compositions. Kaolinite deposits sometimes contain neither diaspore nor corundum, but alunites are often found in the upper portions of the kaolin ore bodies. On the other hand, corundum and diaspore are commoner in the pyrophyllite deposits than the kaolin deposits. As ages of rock formations are becoming younger, amounts of pyrophyllite and kaolinite are rather radically decreased, and finally disappeared. But muscovite, quartz, and plagioclase feldspars are inclined to be preserved because of weak alteration. Most of clay ore bodies contain purple tuff beds on the uppermost portion, and silicified beds, tuff, and lapillistone are found in an ascending order in the most of clay quarries. Chemical analyses show that higher contents of $Al_2O_3$ might not necessarily be due to the argillization, since some tuffs contain higher $Al_2O_3$ contents originated from feldspars. $SiO_2$ contents are fairly higher in the silicified beds than in those of adjacent formations, which might have been introduced from the ore bodies. And $K_2O$ contents are obviously lower than those of $Na_2O$ and CaO in the ores and their vicinities. Ignition losses of some of clays represent much higher contents than those of the ordinary ones because of the sporadic presence of alunite, diaspore and corundum which are accompanied with lots of $SO_4$ and $Al_2O_3$ contents. REE (rare earth element) abundances of most of volcanics and clay ores show rather higher LREE (light rare earth elements) contents, and represent small to moderately negative Eu anomalies. Though most of ores ususally show milky white color, fine-grained and well bedded formations which could be easily discernible in the most of outcrop. But more distinct characteristics are desirable where rather massive ore bodies exist. Purple tuffs and silicified beds above the ore bodies would be useful as marker horizons/key beds since they have rather obvious lithology, extension and mineralogy than those of other adjacent formations.

• Progress in Medical Physics
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• v.20 no.2
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• pp.80-87
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• 2009

Phase transformation, superelastic characteristics and variation of surface residual stress were studied for Nitinol shape memory alloy through application of UNSM technology, and life extension methods of stent were also studied by using elastic resilience and corrosion resistance. Nitinol wire of ${\phi}1.778$ mm showed similar surface roughness before and after UNSM treatment, but drawing traces and micro defects were all removed by UNSM treatment. It also changed the surface residual stress from tensile to compressive values, and XRD result showed less intensive austenite peak and clear martensite and additional R-phase peaks after UNSM treatment. Fatigue resistance could be greatly improved through removal of surface defects and rearrangement of surface residual stress from tensile to compressive state, and development of surface modification system to improve not only bio-compatability but also resistance to corrosion and wear will make it possible to develop vascular stent which can be used for circulating system diseases which run first cause of death of recent Koreans.

• Economic and Environmental Geology
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• v.30 no.4
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• pp.303-312
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• 1997

The massive, fractured and porous-type of glauconite, which is subdivided by surface morphology, occur in subtidal sand and semiconsolidated intertidal sand/mud from continental shelf of the southeastern Yellow Sea. This area is presumed to be a part of Holocene transgressive tidal systems tract. The glauconite, pellet-like grains with diameter of 0.1 to 1 mm, is scattered in surface sand sediments. Results of X-ray diffraction data of the minerals are monoclinic with $a=5.242{\AA}$, $b=9.059{\AA}$, $c=10.163{\AA}$, ${\beta}=100.5^{\circ}$, $V=474.53{\AA}^3$. Thermal treatments on the oriented glauconite increase the X-ray diffraction intensity near $10{\AA}$ (001), suggesting the presence of some expandable layers. Specific gravity of the glauconite is $2.60{\pm}0.45gm/cc$ on the basis of chemical composition and unit-cell dimensions. Based on $O_{10}(OH)_2$, chemical composition of glauconites, octahedral Fe content ranges from 1.19 to 2.06 atoms, corresponding octahedral AI is 0.18 to 0.76 atoms, which progressively substitute Fe for AI with increasing from porous to massive-type. The Mg content ranges from 0.35 to 0.54 atoms, and shows higher with increasing Al contents. A systematic increase of interlayer K from 0.34 to 0.71 is also observed with apparent increases from porous to massive-type, and related to a proportion of expandable layers. The clay preserved in glauconite, which is recognized as ordered/disordered (massive to fractured-type). The interstratified illite/smectite (porous-type), contains 7 to 27 % expandable layers. The glauconite seems to originate from post depositional authigenic growth in reducing environments promoted by the dissolution of clay minerals and biogenic debris.

• Journal of the Korean Chemical Society
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• v.45 no.3
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• pp.242-246
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• 2001

The quaternary thiophosphates, $A_2NiP_2S_6$ (A=Rb, Cs), have been synthesized with halide fluxes and structurally characterized by single-crystal X-ray diffraction technique. These compounds crystallize in the space group $C_{2h}^5-P2_1/n$ of the monoclinic system with two formula units in a cell of dimensions a=5.960(2), b=12.323(4), $c=7.491(3)\AA$, $\beta=97.05(3)^{\circ}$, and $V=546.0(3)\AA^3$ for Rb2NiP2S6 and a=5.957(4), b=12.696(7), $c=7.679(4)\AA$, $b=93.60(5)^{\circ}$, and $V=579.7(5)\AA^3$ for $Cs_2NiP_2S_6.$ These compounds are isostructural. The structure of $Cs_2NiP_2S_6$ is made up of one-dimensional $_\infty^1[NiP_2S_6^{2-}]$ chains along the a axis and these chains are isolated by $Cs^+$ ions. The Ni atom is octahedrally coordinated by six S atoms. These Ni$S_6$ octahedral units are linked by sharing three m-S atoms of the $[P_2S_6^{4-}]$ anions to form the infinite one-dimensional $_\infty^1[NiP_2S_6^{2-}]$ chain. For $Cs_2NiP_2S_6$, the magnetic susceptibility reveals an antiferromagnetic exchange interaction below 8K,which corresponds to the Neel temperature ($T_N$). Above $T_N$, this compound obeys Curie-Weiss law. The magnetic moment, C, and ${\theta}forCs_2NiP_2S_6$ are 2.77 B.M., 0.9593 K, and -19.02 K, respectively. The effective magnetic moment obtained from the magnetic data is agreed with the spin-only value of $Ni^{2+}d^8$(2.83 B.M.) system.

• Journal of the Korean Chemical Society
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• v.37 no.3
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• pp.351-354
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• 1993

Z-1-Ethyl-2-nitro-l-butenyl-(4'-methyl)-phenyl sulfone, C$_{13}$H$_{17}$NO$_4$S, Mr = 293.4, monoclinic space group P2$_1$/c, a = 12.194(7), b = 7.290(4), c = 16.532(14)${\AA}$, ${\beta}$ = 103.4(2)$^{\circ}$, V = 1429.5 ${\AA}^3$, Z = 4, D$_c$ = 1.32 gcm$^{-3}$, ${\lambda}$(Mo K${\alpha}$) = 0.71069 ${\AA}$, ${\mu}$ = 2.2 cm$^{-1}$, F(000) = 600, T = 298 K, R = 0.030 for 1762 unique observed reflections with I > 1.0${\sigma}$(I). A molecule has a cis-typed molecular structure having the form of "the substituted butene backbone, C-C(S)=C(NO$_2$)-C, connecting to a sulfur atom with the methylbenzene ring and to a nitro group. The methylbenzene ring and the substituted butene moiety are nearly planar with the maximum deviations from their own molecular planes, 0.018 ${\AA}$ for the C(1) atom of the benzene group and 0.045 ${\AA}$ for the N atom of the NO$_2$ group, respectively. The angles to the plane of the butene backbone are 88.5$^{\circ}$from the plane of the methyl-benzene and 78.6$^{\circ}$from the plane of the nitro group. Rotation of the nitro group from the butene plane seems to reduced contribution of resonance structure involving the nitro group, and resultant repulsion between the O(2) atom of SO$_2$ and the O(3) atom of NO$_2$ appears to be 2.894 ${\AA}$ longer than an expected van der Waals distance of 2.80 ${\AA}$.