• Bulletin of the Korean Chemical Society
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• v.12 no.5
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• pp.525-529
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• 1991

A simple route is described for the selective functionalization of calixarene at the para positions of phenyl rings. Calix[4]arene tetraacetate 2, obtained from the treatment of calix[4]arene with acetic anhydride, undergoes Fries rearrangement to yield the diametrically para substituted p-diacetylcalix[4]arene 3 in 80% yield. The crystal and molecular strucutre has been determined by X-ray diffraction method. The crystals are orthorhombic, space group Pna21, with a = 11.121 (3), b = 10.374 (3), c = 21.690 (6) $\AA$ and Z = 4. The structure was solved by direct method and refined by full-matrix least-squares methods to final R of 0.036 for 1795 observed reflections. Each hydroxyl hydrogen atom is disordered over two positions. The macrocycle exists in the cone conformation which is determined by the strong circular intramolecular flip-flop type hydrogen bonds of phenolic OH, while crystal packing effects of the diametrically para-acetyl substituents seem to be responsible for the distortion of the cone conformation.

• Journal of the Korean Applied Science and Technology
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• v.25 no.3
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• pp.380-387
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• 2008

The effects of the applied stretch and MgADP binding on the structure of the actin and myosin cross-bridges in rabbit fibers in the rigor state have been investigatedwith improved resolution by x-ray diffraction using synchrotron radiation. To clarify the structure of the ATP hydrolysis intermediates formed by actin and myosin cross-bridges,the effects of various phosphate analogs in the of MgADP on the structure of the thin and thick filaments in glycerinated rabbit muscle fibers in the rigor state investigated by x-ray diffraction with a short exposure time using synchrotron radiation. These results strongly suggest that when MgADP and phosphate analogs such as metallofluorides(BeF3 and AlF4)and vanadate(VO4(Vi)) were added the rigor fibers in the presence of the ATP-depletion backup system, the intensities of the actin-based layer lines were markedly weakened. We found that the intensity of the 14.5 nm-based meridional reflections increase by 20-50% when phosphate analogs such as metallofluorides(BeF3 and AlF4) and vanadate(VO4(Vi)) was added to the rigor muscle.

• Textile Coloration and Finishing
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• v.14 no.5
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• pp.268-276
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• 2002

Poly(trimethylene terephthalate)(PTT) and Poly(ethylene terephthalate)(PET) fibers were annealed at various temperatures ranging from $100^\circ{C}$ to $230^\circ{C}$ for 10 min under tension and tension free. Dyeing rates and absorption isotherms of both fibers were obtained with C.I. Disperse Red 60 at 100, 120 and $130^\circ{C}$ in water system. Also X-ray diffraction pattern, moisture regain and water absorption were investigated. The dyeing rate of PTT fiber is faster than PET fiber, and dyeing of PTT fiber begin at lower temperature compared to PET fiber. The absorption isotherms from both fibers with disperse dye we nearly linear up to the saturation dye uptake, which increase with dyeing temperature. Equilibrium dye uptake of PTT fiber annealed under tension above $180^\circ{C}$ was remarkably decreased because of a changes in the fine structure of fiber. The intensities of X-ray diffraction peaks of both annealed fibers were increased with increasing in annealed temperature. The reflections observed at $2\theta$=$15.8^\circ$, $24^\circ$ and $25.2^\circ$ were assigned reflection of crystal at the planes of (010), $(1\bar02,\;\bar112),\;and\;(\bar13,\; \bar113)$ respectively, and the peak became sharp with heat setting temperature.

• Bulletin of the Korean Chemical Society
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• v.17 no.7
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• pp.643-647
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• 1996

1,2-Disubstituted chiral calix[4]arene "25-(3,5-dinitrobenzoyloxy)-26-methoxy-27,28-dihydroxycalix[4]arene" was synthesized by the reaction of 25-(3,5-dinitrobenzoyloxy)-calix[4]arene with methyl iodide in the presence of K2CO3. Methylation was occurred at the 26-position of calix[4]arene. The partial cone conformation and 1,2-substitution were characterized based on the 1H NMR, 13C NMR and X-ray diffraction analysis. The crystal structure has been determined by X-ray diffraction method. The crystals are orthorhombic, Pbca, a=10.652(1), b=17.687(1), c=32.247(3) Å, Z=8, V=6075.4(9) Å3, Dc=1.38gcm-3. The intensity data were collected on an Enraf-Nonius CAD-4 Diffractometer with a graphite monochromated Cu-Kα radiation. The structure was solved by direct method and refined by full-matrix least-squares methods to a final R value of 0.050 for 2368 observed reflections. The molecule is in the partial cone conformation. It has two strong intramolecular hydrogen bonds of O(1D)-H…O(1C)-H…O(1B).

• Bulletin of the Korean Chemical Society
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• v.23 no.12
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• pp.1759-1764
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• 2002

Two crystal structures of dehydrated $Ag^+-andTl^+$-exchanged zeolite X$Ag_{27}Tl_{65-}X\;and\;Ag_{23}Tl_{69-}X$have been determined by single-crystal X-ray diffraction techniques in the cubic space group Fd3 at 21(1) $^{\circ}C(a=24.758(4)\AAa=24.947(4)$, ${\AA}respectively).$, Their structures were refined to the final error indices $R_1$=0.055 and $wR_2$=0.057 with 375 reflections, and $R_1$=0.057 and $wR_2$=0.057 with 235 reflections, respectively, for which I > $3\sigma(I).$ In the structure of $Ag_{27}Tl_{65-}X,\;27\;Ag^+$ ions were found at two crystallographic sites: 15$Ag^+$ ions at site I at the center of the hexagonal prism and the remaining 12$Ag^+$ ions at site II' in the sodalite cavity. Sixty-five $Tl^+$ ions were located at three crystallographic sites: 20$Tl^+$ ions at site II opposite single six-rings in the supercage, 18$Tl^+$ ions at site I' in the sodalite cavity opposite the D6Rs, and the remaining 27$Tl^+$ ions at site III' in the supercage. In the structure of $Ag_{23}Tl_{69-}X$, 23$Ag^+$ ions were found at two crystallographic sites: 15 at site I and 8 at site II'. Sixty-nine $Tl^+$ ions are found at four crystallographic sites: 24 at site II, 17 at stie I', and the remaining 28 at two III' sites with occupancies of 22 and 6.

• Korean Journal of Crystallography
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• v.11 no.2
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• pp.84-88
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• 2000

The crystal of cholesteryl crotylcarbonate was investigated by X-ray diffraction method. Crystallographic data for the title compound: P21, a=13.510(2)Å, b=11.843(2)Å, c=19.882(2)Å, β=106.88(1)°, Z=4. Reflections were collected with an Enraf-Nonius CAD-4 diffractometer equipped with a graphite monochromator. The structure was solved by direct methods and refined by least-squares analyses. The final R value was 0.125 for 2607 reflections. The cholesterol fragment of the title compound were in good agreement with those for related cholesterol derivatives. The molecules were stacked in clearly separated layers. At the center of the layers, there were cholesteryl-cholesteryl interactions between the symmetry-related B molecules and the cholesteryl-C(17) side chain of A molecules. There were also interactions between the C(17) side chain of B molecules and the crotylcarbonate chain in the interface region between layers. The crystal structure of the title compound turned out to be isostructural with those of cholesteryl ethylcarbonate and cholesteryl propylcarbonate.

• Textile Coloration and Finishing
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• v.4 no.3
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• pp.91-96
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• 1992

The crystalline character of NaOH and KOH-cellulose complex having different tension ratio was studied using X-ray diffraction analysis. Cellulose crystalline lattices in tension alkali treatment cotton were identified by measuring and indexing the 101, 101, and 002 reflections. According as alkali treatment tension ratio increased on, cellulose gave rise to the formation of I rather than cellulose II. It seemed that a part of the fine structure of cellulose increased orientation with antiparaell and parallel chain crystal structure. The high tension ratio alkali treatment cotton resulted in lower dye sorption and in higher breaking strength and crease recovery.

• Journal of the Korean Ceramic Society
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• v.11 no.3
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• pp.14-18
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• 1974

Magnesite single crystals up to 250 microns were synthesized from an equi-molar solution of MgCl2 and Na2CO3 in the micro-autoclave at 180-20$0^{\circ}C$. The lattice constant of synthetic magnesite was obtained a=4.6369(7), c=15.0230(10)A.U. by a least squares analysis based on the UNICS Program (Sakurai 1967) was applied to 28 reflections. Results of X-ray powder diffraction and of DTA, TGA, IRA, and EPMA studies indicate that synthesized magnesite has properties to those of natural magnesite.

• Bulletin of the Korean Chemical Society
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• v.10 no.6
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• pp.582-585
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• 1989

Two crystal structures of dehydrated $Sr^{2+}\;and\;Tl^+$ exchanged zeolite A, $Sr_xTl_{12-2x}-A$ (x = 1.6 and 5.45), have been determined by single-crystal X-ray diffraction techniques. Their structures were solved and refined in the cubic space group Pm3m at $21(1)^{\circ}C.$ Both crystals were ion exchanged in flowing streams of mixed $Sr(NO_3)_2\;and\;TlNO_3$ aqueous solution, followed by dehydration at $360^{\circ}C\; and\; 2${\times}$10^{-6}$ Torr for 2 days. Full-matrix least-squares refinements of the dehydrated $Sr_{1.6}Tl_{8.8}-A (a = 12.214(2){\AA})\; and\;Sr_{5.45}Tl{1.1}-A (a=12.291(2){\AA})$ have converged to final error indices, $R_1=0.055\; and\;R_2=0.061$ with 286 reflections, and R1 = 0.072 and R2 = 0.090 with 217 reflections, respectively, for which$\;I\;{>}\;3{\sigma}(I)$. In both structures, all Sr(II) ions are coordinated by three framework oxygens; Sr(II) to O(3) distances are $2.21(2){\AA}\;for\;Sr_{1.6}Tl_{8.8}-A \;and\;2.31(1){\AA} \;for\;Sr_{5.45}Tl_{1.1}-A,$and Tl(I) to O(3) distances are $2.657(6){\AA}\;for\;Sr_{1.6}Tl_{8.8}-A\;and\;2.845(8){\AA}\;for\;Sr_{5.45}Tl_{1.1}-A,$ respectively. In each structure, the angle subtended at Sr(II), O(3)-Sr(II)-O(3) is $118.7(4)^{\circ}\;for\; Sr_{1.6}Tl_{8.8}-A \;and\;120.0(4)^{\circ}\;for\;Sr_{5.45}Tl_{1.1}-A.\;Sr^{2+}$ ions prefer to 6-ring sites and $Tl^+$ ions to 8-ring sites when total number of ions per unit cell is more than 8.

• Korean Journal of Crystallography
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• v.13 no.2
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• pp.96-100
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• 2002

The title compound, (H/sub 3/NCH/sub 2/CH/sub 2/NH/sub 3/)HPO/sub 4/ (Ⅰ), has been synthesized by hydrothermal technique for the first time and its novel structure analyzed by X-ray single crystallography. The compound (Ⅰ) crystallizes in the monoclinic system, P2/sub 1//c space group with a＝10.209(1), b＝7.891(1), c＝ 8.039(1) (equation omitted), β＝ 92.138(9)°, V＝: 647.2(2) (equation omitted), Z＝4, R/sub 1/＝0.0295 and ωR/sub 2/＝0.0811 for 1141 independent reflections. The compound (Ⅰ) is interconnected to give a three-dimensional network through hydrogen-bonding interactions.