• Journal of the Korean Crystal Growth and Crystal Technology
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• v.9 no.5
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• pp.475-479
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• 1999

Langasite ($La_{3}Ga_{5}SiO_{14}$) was found to have wide application as a promising piezoelectric material. It has high thermal stability of the frequency and large electromechanical coupling factor. For the further development of new compounds with langasite type structure, powders in the La-Al-Si-O system were synthesized by a modified Pechini process. The evolution of the crystalline phase during calcination was studied using TG-DTA, XRD and TEM for the precursor powders. Decomposition proceeded via dehydration and removal of excess solvents at low temperatures ($T<500^{\circ}C$), followed by the crystallization of lanthanum aluminum silicate ($T>800^{\circ}C$) and phase transformation to $LaAlO_{3}$ phase ($T>1200^{\circ}C$). Transmission electron microscopy (TEM) of the calcined powders showed diffuse hollow rings corresponding to an amorphous phase at $800^{\circ}C$ and clear diffraction patterns corresponding to a crystalline phase from the P321 space group ($T<1200^{\circ}C$) and the R3m ($T<1200^{\circ}C$).

• Korean Journal of Soil Science and Fertilizer
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• v.46 no.2
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• pp.87-91
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• 2013

The crystal structure of partially dehydrated fully $Zn^{2+}$-exchanged zeolite Y was determined by X-ray diffraction techniques in the cubic space group $Fd\bar{3}m$ at 294(1) K and refined to the final error indices $R_1/wR_2$ = 0.035/0.119 for $|Zn_{35.5}(H_2O)_{13}|[Si_{121}Al_{71}O_{384}]$-FAU. About 35.5 $Zn^{2+}$ ions per unit cell are found at six distinct positions; sites I, I', a second I', II', II, and a second II. In sodalite cavities, the 11 water molecules coordinate to Zn(I'b) and/or Zn(II') ions; each of two $H_2O$ bonds to a Zn(IIb) in supercages. Two different $Zn^{2+}$ positions near 6-oxygen ring are due to their Si-Al ordering in tetrahedral site by Si/Al ratio leading to the different kinds of 6-rings.

• Bulletin of the Korean Chemical Society
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• v.21 no.1
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• pp.101-104
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• 2000

Li-graphite intercalation compounds (GICs), synthesized at elevated temperature and pressure, were allowed to decompose spontaneously in the atmosphere. The decomposition processes were analyzed by of X-ray diffraction, DSC analysis, FT-IR measurements, UV/VIS spectrophotometry. The deintercalation reaction of the Li-GICs ceased after 6 weeks and only the residual compounds could be observed. A strong exothermic reaction was observed at 300 $^{\circ}C$ in thermal decomposition, and relatively stable decomposition curves were formed. A few endothermic curves have been observed at 1000 $^{\circ}C.$ After 6 weeks deintercalation reaction time of GICs, many exothermic and endothermic reactions were accompanied at the same time. In addition the reactions of the functional groups such as aromatic rings, nitrogen, $-CH_3$, $-CH_2$ etc. of GDIC obtained by the above reaction were confirmed by FT-IR spectrum. UV/VIS spectrophotometric measurement clearly shows the formation of a minimum energy value ($R_{min}$) for the compounds between Li-GICs as a starting material and Li-GDICs obtained until after 3 weeks of the deintercalation reaction, while they were no clear energy curves from 4 weeks of reaction time, because of the formation of the graphite structure, of high stages and of the Li compounds surrounding the graphite in the deintercalation reaction.

• Bulletin of the Korean Chemical Society
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• v.19 no.10
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• pp.1095-1099
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• 1998

The crystal structure of an acetylene sorption complex of dehydrated fully Mn(Ⅱ)-exchanged zeolite X, Mn46Si100Al92O384·30C2H2 (a=24.705(3) Å) has been determined by single-crystal X-ray diffraction techniques. The structure was solved and refined in the cubic space group Fd3 at 21(l) ℃. The complex was prepared by dehydration at 380 ℃ and 2 x 10-6 Torr for 2 days, followed by exposure to 300 Torr of acetylene gas for 2 h at 24 ℃. The structure was refined to the final error indices, R1=0.060 and R2=0.054 with 383 reflections for which I > 3σ(Ⅰ). In the structure, Mn2+ ions are located at two different crystallographic sites; sixteen Mn2+ ions at site I are located at the centers of the double six rings and thirty Mn2+ ions are found at site Ⅱ in the supercage, respectively. Each of these latter Mn2+ ions is recessed ca. 0.385(2) Å into the supercage from its three-oxygen plane. Thirty acetylene molecules are sorbed per unit cell. Each Mn2+ ion at site Ⅱ lies on a threefold axis in the supercage of the unit cell, close to three equivalent trigonally arranged zeolite framework oxygen atoms (Mn(Ⅱ)-O=2.135(9) Å) and symmetrically to both carbon atoms of a C2H2 molecules. At these latter distances, the Mn(Ⅱ)-C interactions are weak (Mn(Ⅱ)-C=2.70(5) Å), probably resulting from electrostatic attractions between the divalent cations and the polarizable π-electron density of the acetylene molecules.

• Journal of the Korean Chemical Society
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• v.63 no.1
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• pp.29-36
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• 2019

A potentially tetradentate Schiff base ligand, 2-((2-((pyridin-2-ylmethylene)amino)ethyl)amino)ethan-1-ol (PMAE), and its cadmium(II) complex, [$Cd(PMAE)I_2$] (1), were prepared and characterized by elemental analysis, FT-IR, Raman, $^1H$ and $^{13}C$ NMR spectroscopies and single-crystal X-ray diffraction. In the crystal structure of 1, the cadmium atom has a slightly distorted square-pyramidal geometry and a $CdN_3I_2$ environment in which the PMAE acts as an $N_3$-donor. In the crystal packing of the complex, the alcohol and amine groups of the coordinated ligands participate in hydrogen bonding with iodide ions and form $R^2{_2}(14)$ and $R^2{_2}(8)$ hydrogen bond motifs, respectively. In addition to the hydrogen bonds, the crystal network is stabilized by ${\pi}-{\pi}$ stacking interactions between pyridine rings. The thermodynamic stability of the isolated ligand and its cadmium complex along with their charge distribution patterns were studied by DFT and NBO analysis.

• Bulletin of the Korean Chemical Society
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• v.9 no.5
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• pp.303-308
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• 1988

Four crystal structures of dehydrated Ag(I) and Tl(I) exchanged zeolite A, $Ag_{12-x}Tl_x$-A, x = 2, 3, 4, and 5, have been determined by single-crystal x-ray diffraction techniques. Their structures were solved and refined in the cubic space group Pm3m at $21(1)^{\circ}C$. All crystals were ion exchanged in flowing streams of mixed $AgNO_3\;and\;TlNO_3$ aqueous solution, followed by dehydration at $350^{\circ}C$ and $2{\times}10^{-6}$ Torr for 2 days. In all of these structures, one-sixth of the sodalite units contain octahedral hexasilver clusters at their centers and eight $Ag^+$ ions are found on threefold axes, each nearly at the center of a 6-oxygen ring. The hexasilver cluster is stabilized by coordination to eight $Ag^+$ ions. The Ag-Ag distance in the cluster, ca. 2.92 ${\AA}$, is near the 2.89 ${\AA}$ bond length in silver metal. The remaining five-sixths of the sodalite units are empty of silver species. The first three $Tl^+$ ions per unit cell preferentially associate with 8-oxygen rings, and additional $Tl^+$ ions, if present, are found on threefold axes in the large cavity.

• Bulletin of the Korean Chemical Society
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• v.11 no.4
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• pp.328-331
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• 1990

Three crystal structures of dehydrated Cd(II) and Rb(I) exchanged zeolite A, $Cd_{4.0}Rb_{4.0}-A (a = 12.204(3) {\AA}), Cd_{5.0}Rb_{2.0}-A (a = 12.202(1) {\AA}),$ and $Cd_{5.95}Rb_{0.1}-A (a = 12.250(2) {\AA}),$ have been determined by single-crystal X-ray diffraction techniques. Their structures were solved and refined in the cubic space group Pm3m at $21(1)^{\circ}C.$ All crystals were ion exchanged in flowing streams of mixed $Cd(NO_3)_2·4H_2O$ and $RbNO_3$ aqueous solution with total concentration of 0.05 M. All crystals were dehydrated at ca. $450^{\circ}C$ and $2×10^{-6}$ Torr for 2 days. In all of these structures, $Cd^{2+}$ ions are found on threefold axes, each nearly at the center of a 6-oxygen ring. The first three $Rb^+$ ions per unit cell preferentially associate with 8-oxygen rings, and additional $Rb^+$ ions, if present, are found on threefold axes in the large cavity. The final $R_1$ and $R_2$ values for the three structures are 0.087 and 0.079, 0.059 and 0.067, and 0.079 and 0.095, respectively.

• Bulletin of the Korean Chemical Society
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• v.7 no.5
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• pp.331-334
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• 1986

The crystal structure of thiamin tetrahydrofurfuryl disulfide, one of the ring-opened derivatives of thiamin, has been determined by the X-ray diffraction methods. The crystal is monoclinic with cell dimensions of a = 8.704 (1), b = 11.207 (2), c = 21.260 (3) ${\AA}$ and ${\beta}$ = 92.44 (2)$^{circ}$, space group P2$_{1}$/c and Z = 4. The structure was solved by direct methods and refined to R = 0.076 for 1252 observed reflections measured on a diffractometer. The molecule assumes a folded conformation in which the pyrimidine and the tetrahydrofurfuryl rings are on the same side of the ethylenic plane. The pyrimidinyl, N-formyl and ethylenic planes are mutually perpendicular to each other and the N(3)-C(4) bond retains a single bond character. The structure is stabilized by an intramolecular N(4'${\alpha})-H{\cdots}O(2{\alpha}$) hydrogen bond. The molecules are connected via N(4'${\alpha}$)-H{\cdots}(N3')$ and O(5${\gamma})-H{\cdots}(N1')$ hydrogen bonds, forming a two-dimensional hydrogen-bonding network. The tetrahydrofurfuryl ring is dynamically disordered. The overall conformation as well as the packing mode is very similar to that of thiamin propyl disulfide.

• Analytical Science and Technology
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• v.20 no.5
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• pp.448-451
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• 2007

A new bis(dicyclohexylammonium) chromate dihydrate complex, $[(C_6H_{11})_2NH_2]_2[CrO_4]{\cdot}2H_2O$, (I), has been synthesized and its structure analyzed by FT-IR, EDS, elemental analysis, ICP-AES, and single crystal X-ray diffraction methods. The Cr(VI) complex (I) is tetragonal system, I${\bar{4}}$2d space group with a = 12.5196(1), b = 12.5196(1), c = $17.3796(3){\AA}$, a = ${\beta}$ = ${\gamma}$ = $90^{\circ}$, V = $2724.09(6){\AA}^3$, Z = 4. The crystal structure of complex (I) consists of tetrahedral chromate $[CrO_4]^{2-}$ anion, two organic dicyclohexylammonium $[(C_6H_{11})_2NH_2]^+$ cations and two lattice water molecules. The chromate anion and protonated dicyclohexylammonium cation is mainly constructed through the ionic bond. The cyclohexylammonium rings of the dicyclohexylammonium cation take the chair form and vertical configuration with each other. The N-H${\cdot}$O and O-H${\cdot}$O hydrogen bond networks between the $N_{dicyclohexylammonium}$, $O_{water}$ and $O_{chromate}$ atom lead to self-assembled molecular conformation and stabilize the crystal structure.

• Korean Journal of Mineralogy and Petrology
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• v.33 no.3
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• pp.251-258
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• 2020

Single crystal of fully dehydrated and partially Ca²⁺-exchanged zeolites A (|Ca₄Na₄|[Si₁₂Al₁₂O₄₈]-LTA) was brought into contact with Se in fine pyrex capillary at 523 K for 5 days. Crystal structure of Se-sorbed |Ca₄Na₄|[Si₁₂Al₁₂O₄₈]-LTA has been determined by single-crystal X-ray diffraction techniques at 294 K in the cubic space group $Pm{\bar{3}}m$ (a = 12.2787(13) Å). The crystal structure of yellow |Ca₄Na₄Se₄|[Si₁₂Al₁₂O₄₈]-LTA has been refined to the final error indices of R₁/wR₂ = 0.0960/0.3483 with 327 reflections for which F_o > 4s(F_o). In this structure, 4 Na⁺ and 4 Ca²⁺ ions fill every 6-ring site: These ions are all found at three crystallographic positions, on 3-fold axes equipoints of opposite 6-rings. Selenium atoms are found at three crystallographically distinct positions: 2 Se atoms per unit cell at Se(1) are located opposite 6-rings in the sodalite cavity (Se(1)-Na(1) = 2.53(5) Å) and 1 at Se(2) opposite 4-rings (Se(2)-O(1) = 2.76(10) Å) and 1 at Se(3) opposite 6-rings in the large cavity (Se(3)-Na(1) = 2.48(5) Å). Two molecular of Se₂ (Se(1)-Se(1) = 2.37(7) or 2.90(8) Å and Se(2)-Se(3) = 2.91(5) ) Å) are found in all sodalite cavity and large cavity. Other clusters such as Se₄ and Se₈ could be existed in large cavity. The inter-selenium distances turned out to be longer that of gases Se₂ molecule.