• Bulletin of the Korean Chemical Society
• /
• v.6 no.6
• /
• pp.333-337
• /
• 1985

Cholesteryl formate$(HCOOC_{27}H_{45})$ is monoclinic, space group $P2_1$ with a=15.757(1), b=6.073(1), c=13.592(2) ${\AA},{\beta}=94.1(1)^{\circ},Z=2.$ Intensities were measured, using an automatic diffractometer with graphite-monochromated $Cu-K{\alpha}$ radiation. The structure was solved by a direct method and refined by least-squares method. The final R factor was 0.087 for 1640 observed reflections. There are no unusual bond distances and angles. The molecules are arranged in antiparallel array forming monolayers of thickness $d_{100}=15.757{\AA}.$ Adjacent cholesteryl ring groups by the translation operation along the b axis.

• Bulletin of the Korean Chemical Society
• /
• v.5 no.4
• /
• pp.158-162
• /
• 1984

The crystal structure of chloramphenicol base, $C_9H_{l2}N_2O_4$, the deacylated base of antibiotic chloramphenicol, has been determined by X-ray diffraction techniques using diffractometer data obtained by the ${\omega}-2{\theta}$ scan technique with CuK${\alpha}$ radiation from a crystal with space group symmetry $P2_12_12_1$ and unit cell parameters a = 22.322(6), b = 7.535(6), c = 5.781(5) ${\AA}$. The structure was solved by direct methods and refined by full-matrix least-squares to a final R = 0.051 for the 573 observed reflections. The overall conformation of the base is quite different from those of the chloramphenicol congeners which are similar despite the presence of many rotatable single bonds. The propane chain in the base is bent with respect to the phenyl ring, while it is extended in the chloramphenicol congeners. There is no intramolecular hydrogen bond between the hydroxyl groups of the propanediol moiety. All of the molecules in the crystal lattice are connected by a three-dimensional hydrogen bonding network.

• Journal of the Korean Chemical Society
• /
• v.20 no.1
• /
• pp.19-34
• /
• 1976

The crystal structure of sodium sulfisoxazole hexahydrate, $C_{11}H_{12}N_3O_3SNa{\cdot}6H_2O$,has been determined by X-ray diffraction method. The compound crystallizes in the monoclinic space group $$P2_1}c$$ with a = 15.68(3), b = 7.70(2), c = 17.94(4)${\AA}$, ${\beta}$ = $118(2)^{\circ}$ and Z = 4. A total of 1717 observed reflections were collected by the Weissenberg method with $CuK{\alpha}$ radiation. Structure was solved by heavy atom method and refined by block-diagonal least-squares methods to the R value of 0.14. The conformational angle formed by the S-C(l) bond with that of N(2)-C(7), when the projection in taken along the S-N(2), is $73^{\circ}.$ The benzene ring is planar and makes an angle of $60^{\circ}$ with the plane of the isoxazole ring, which is also planar. The sodium atom has a distorted octahedral coordination of N(l) and five oxygen atoms from hydrate molecules. Sodium sulfisoxazole hexahydrate shows fourteen different hydrogen bondings in the crystal. These are six $O-H{\cdots}O-H bonds, three $O-H{\cdots}O$ bonds, two $O-N{\cdots}N,$ one $N-H{\cdots}O,O-H{\cdots}N,N-H{\cdots}O-H$ bond, with the distances in the range of 2.71 to $3.04{\AA}.$.

• Bulletin of the Korean Chemical Society
• /
• v.23 no.5
• /
• pp.688-692
• /
• 2002

The aminomethylation of phenols with para-substituents by the Mannich reaction has successfully been accomplished to produce the Mannich bases 2-6. The compounds 7-8 have also been synthesized in order to identify the effect of the side arms and t he macrocycle in the complex formation. Protonation constants and stability constants of the double armed diaza-18-crown-6 ethers 2-7 with metal ions have been determined by potentiometric method at 25 $^{\circ}C$ in 95 % methanol solution. Under a basic condition (pH > 8.0), the double-armed crown ethers 2-6 revealed stronger interaction with divalent metal ions than the simple diazacrown ether 1. The stability constants with these metal ions were Co 2+ < Ni2+ < Cu2+ > Zn 2+ in increasing order, which are in accordance with the order of the Williams-Irving series. The stability constants with alkali earth metal ions were Ca 2+ < Sr 2+ < Ba 2+ in increasing order, which may be explained by the concept of size effect. It is noteworthy that the hosts 2-6, which have phenolic side arms and a macrocycle, bind stronger with metal ions than the hosts 1 and 7. On the other hand, the host 8, which has phenolic side arms with a pyperazine ring,provided comparable stability constants to those with the host 3. These facts demonstrate that phenolic side arms play a more important role than the azacrown ether ring in the process of making a complex with metal ions especially in a basic condition. In particular, the log KML values for complexation of divalent metal ions with the hosts 2-6 had the sequence, i.e., 2 (R=OCH3) < 3 (R=CH3) < 4 (R=H) < 5 (R=Cl) < 6 (R=CF3). The stability constants of the hosts 5 and 6 containing an electron-withdrawing group are larger than those of the hosts 2 and 3 containing an electron-donating group. This substituent effect is attributed to the solvent effect in which the aryl oxide with an electron-donating group has a tendency to be tied strongly with protic solvents.

• Journal of the Korean Chemical Society
• /
• v.21 no.1
• /
• pp.3-15
• /
• 1977

Crystals of salicylaldehyde-4-morpholinothiosemicarbazone, $C_{12}H_{15}O_2N_3S$, are orthorhombic with space group Pna21. Unit-cell dimensions are a = 11.85(5), b = 15.45(5) c = 7.18(3)${\AA}$ with z = 4. Three-dimensional intensity data were collected from the multiple-film equi-inclination Weissenberg photographs taken with $CuK{\alpha}$ radiation. The intensities were estimated visually. The structure was solved by Patterson and Fourier methods and refined by the block-diagonal least-squares methods until the final R value becomes 0.11 for the 1064 observed independent reflections. The morpholine ring has a chair form. The rest atoms of salicylaldehyde-4-morpholinothiosemicarbazone molecule excluding morpholine ring and sulfur atom approximately lie on a plane. The hydroxyl group of the salicylaldehyde and the nitrogen atom of the thiosemicarbazone form an intramolecular hydrogen bond, $O-H{\cdot}{\cdot}{\cdot}N$, of 2.67${\AA}$. The short intermolecular distances all appear to be normal van der Waals contacts.

• Korean Journal of Materials Research
• /
• v.27 no.7
• /
• pp.386-391
• /
• 2017

Using a customized diffusion bonder, we executed diffusion bonding for ring shaped white gold and red gold samples (inner, outer diameter, and thickness were 15.7, 18.7, and 3.0 mm, respectively) at a temperature of $780^{\circ}C$ and applied pressure of 2300 N in a vacuum of $5{\times}10^{-2}$ torr for 180 seconds. Optical microscopy, field emission scanning electron microscopy (FE-SEM), and energy-dispersive X-ray spectroscopy (EDS) were used to investigate the microstructure and compositional changes. The mechanical properties were confirmed by Vickers hardness and shear strength tests. Optical microscopy and FE-SEM confirmed the uniform bonding interface, which was without defects such as micro pores. EDS mapping analysis confirmed that each gold alloy was 14K with the intended composition; Ni and Cu was included as coloring metals in the white and red gold alloys, respectively. The effective diffusion coefficient was estimated based on EDS line scanning. Individual values of Ni and Cu were $5.0{\times}10^{-8}cm^2/s$ and $8.9{\times}10^{-8}cm^2/s$, respectively. These values were as large as those of the melting points due to the accelerated diffusion in this customized diffusion bonder. Vickers hardness results showed that the hardness values of white gold and red gold were 127.83 and 103.04, respectively, due to solid solution strengthening. In addition, the value at the interface indicated no formation of intermetallic compound around the bonding interface. From the shear strength test, the sample was found not to be destroyed at up to 100,000 gf due to the high bonding strength. Therefore, these results confirm the successful diffusion bonding of 14K white-red golds with a diffusion bonder at a low temperature of $780^{\circ}C$ and a short processing time of 180 seconds.

• Bulletin of the Korean Chemical Society
• /
• v.24 no.3
• /
• pp.269-273
• /
• 2003

The synthesis and properties of 2,13-bis(3'-pyridylmethyl) $(L^3)$, 2,13-bis(4'-pyridylmethyl) $(L^4)$, and 2,13-bis(phenylmethyl) $(L^5)$ derivatives of 5,16-dimethyl-2,6,13,17-tetraazatrcyclo$[16.4.0.^{1.18}0^{7.12}]$docosane are reported. The 3- or 4-pyridylmethyl groups of $[ML^3](ClO_4)_2\;or\;[ML^4](ClO_4)_2$ (M = Ni(Ⅱ) or Cu(Ⅱ)) are not involved in coordination, and the coordination geometry (square-planar) and ligand field strength of the complexes are quite similar to those of $[ML^5](ClO_4)_2$, bearing two phenylmethyl pendant arms. However, the complex formation reactions of $L^3\;and\;L^4$ are strongly influenced by the pyridyl groups, which can interact with a proton or metal ion outside the macrocyclic ring. The macrocycle $L^5$ exhibits a high copper(Ⅱ) ion selectivity against nickel(Ⅱ) ion; the ligand readily reacts with copper(Ⅱ) ion to form $[CuL^5]^{2+}$ but does not react with hydrated nickel(Ⅱ) ion in methanol solutions. On the other hand, $L^3\;and\;L^4$ form their copper(Ⅱ) and nickel(Ⅱ) complexes under a similar condition, without showing any considerable metal ion selectivity. The ligands $L^3\;and\;L^4$ react with copper(Ⅱ) ion more rapidly than does $L^5$ at pH 6.4. At pH 5.0, however, the reaction rate of the former macrocycles is slower than that of the latter. The effects of the 3- or 4-pyridylmethyl pendant arms on the complex formation reaction of $L^3\;and\;L^4$ are discussed.

• Journal of the Korea Academia-Industrial cooperation Society
• /
• v.7 no.5
• /
• pp.805-810
• /
• 2006

Defects in the conventional casting process of silver jewelry can result in famished products of mediocre hardness. To overcome the shortcomings of conventional methods, we proposed new press forming process, which involves applying uniaxial pressure on casting 92.5%Ag-6.5%Cu-1%Zn ring elements and shaping with a lath. We investigated Vickers hardness, density, and microstructure evolution by changing the applied uniaxial pressure. We report that our newly proposed process can increase the hardness up to 2.3 times and decrease average grain size by 50%. Our method leads to drastic mechanical property enhancements, and is thus suitable for casting tension-style jewelry.

• Bulletin of the Korean Chemical Society
• /
• v.19 no.6
• /
• pp.671-676
• /
• 1998

The formation and dissociation rates of $Ce^{3+}$ Complexes of the 1,4,7,10-tetraaza-13,16-dioxacyclooctadecane-NN', N",N"'-tetraacetic acid (1), 1,4,7,10-tetraaza-13,16-dioxacyclooctadecane-N,N',N",N"'-tetramethylacetic acid (2), and 1,4,7,10-tetraaza-13,16-dioxacyclooctadecane-N,N',N",N"'-tetrapropionic acid (3) have been measured by the use of stopped-flow spectrophotometry. Observations were made at 25.0±0.1 ℃ and at an ionic strength of 0.10 M $NaClO_4$. The complexation of $Ce^{3+}$ ion with 1 and 2 proceeds through the formation of an intermediate complex $(CeH_3L^{2+})^*$ in which the $Ce^{3+}$ ion is incompletely coordinated. This may then lead to be a final product in the rate-determining step. Between pH 4.76 and 5.76, the diprotonated $(H_2L^{2-})$ from is revealed to be a kinetically active species despite of its low concentration. The stability constants $(logK(CeH_3L^{2+}))$ and specific water-assisted rate constants $(k_{OH})$ of intermediate complexes have been determined from the kinetic data. The dissociation reactions of $Ce^{3+}$ complexes of 1, 2, and 3 were investigated with $Cu^{2+}$, ions as a scavenger in acetate buffer. All complexes exhibit acid-independent and acid-catalyzed contributions. The effect of buffer and $Cu^{2+}$ concentration on the dissociation rate has also been investigated. The ligand effect on the dissociation rate of $Ce^{3+}$ complexes is discussed in terms of the side-pendant arms and the chelate ring sizes of the ligands.

• Journal of the Korean Chemical Society
• /
• v.28 no.1
• /
• pp.41-46
• /
• 1984

To preconcentrate trace elements, microgram amounts of 5 heavy metals (Cu, Co, Ni, Zn and Cd) were precipitated with 8-hydroxyquinoline (oxine) and metal oxinates were extracted with stearic acid. And then each of the molten stearic acid extract with stearic acid. And then each of the molten stearic acid extract was poured into a glass ring and cooled for specimen preparation. The obtained specimens were analyzed by X-ray fluorescene spectrometry. And then conditions of precipitation formation and extraction, reproducibility, sensitivity and detection limit were observed. The relative standard deviation of specimen preparation was 1.0~5.7% and the detection limit was 5~$50{\mu}g$/100ml. The proposed preconcentration procedure exhibited a considerable inhancement and simplicity in preparing specimens.