• Bulletin of the Korean Chemical Society
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• v.23 no.11
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• pp.1527-1530
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• 2002

1,12-diazacyclodocosane-2,11-dione was first isolated from a plant Phyllanthus niruri Linn. Its structure has been determined by means of spectroscopy methods and X-ray crystallography. Two peptide groups in the big ring (lactam) are the main factors influencing intermolecular contacts. The hydrogen-bond interaction of these hydrophilic groups is observed in the crystal structure. Meanwhile, C-H···O hydrogen bonds in molecules contribute to the formation of the whole crystal. These two kinds of hydrogen-bond form six- member rings among molecules. This compound crystallizes in the triclinic space group P-1 with a= 9.588(1) $\AA$, b= $9.850(1)\AA$, c = $11.810(1)\AA$, $\alpha=$ 68.18(1)$^{\circ}C$ , $\beta=$ 84.98(1), $\gamma$ = 86.03(1)$^{\circ}C$ , V = $1030.66(17)\AA3$ , Z = 2. A disorder of five-member carbon chain in the whole ring is observed in the title compound. The bond angle 105.8(4) is determined for a extreme configuration C(14)-C(15)-C(16), and 117.7(10) for another extreme configuration C(14')-C(15')-C(16'). In this crystal, two molecules are tied each other by short intermolecular hydrogen bonds, the oxygen atom being tied by hydrogen bond to nitrogen atom of another two molecules. The NMR and IR spectral data coincides to the structure of the compound.

• Analytical Science and Technology
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• v.18 no.4
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• pp.278-286
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• 2005

The crystal structure of ($Tl_{71}$-Y ($Tl_{71}Si_{121}Al_{71}O_{384}$), ${\alpha}=24.706(3){\AA}$, dehydrated at 653 K and $8{\times}10^{-6}$ torr, has been determined by single-crystal X-ray diffraction techniques in the cubic space group $Fd\bar{3}m$ at 294(1) K. The structure was refined using all intensities to the final error indices (using only the 302 reflection for which $F_{\circ}$ > $4{\sigma}(F_0)$) $R_1=0.0602$ (based on F) and $R_w=0.1744$ (based on $F_2$). The 71 $Tl^+$ ions per unit cell are found at four crystallographically distinct positions. Site I' position in the sodalite cavity opposite D6Rs are each occupied by eighteen $Tl^+$ ions per unit cell; these $Tl^+$ ions are recessed ca. $1.45{\AA}$ into the sodalite cavity from their O(3) plane (Tl-O=2.701(15), $3.163(16){\AA}$ and O-Tl-O=$92.1(4)^{\circ}$). The 23 $T1^+$ ions fill site II in the supercage; these $T1^+$ ions are recessed ca. $1.58{\AA}$ into the supercage from their O(2) plane (Tl-O = 2.850(16), $3.156(16){\AA}$ and O-T1-O = $85.1(5)^{\circ}$). The 19 $Tl^+$ ions lie at site III' in the supercage near a triple 4-ring (Tl-O = 3.10(7), $3.39(5){\AA}$ and O-Tl-O = 47.8(9), $95.3(18)^{\circ}$) and the remaining II ions occupy another site III' near a triple 4-ring in the supercage (Tl-O = 2.81(4), $2.71(4){\AA}$ and O-Tl-O = $57.3(8)^{\circ}$).

• Bulletin of the Korean Chemical Society
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• v.6 no.4
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• pp.202-206
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• 1985

The crystal structure of The crystal structure of $Ag^+$-Exchanged Zeolite A, $Ag_{4.6}Na_{7.4}-A$, dehydrated, treated with $H_2$, and evacuated, all at $350^{\circ}C$, has been determined by single crystal x-ray diffraction methods in the cubic space group Pm3m at $24(1)^{\circ}C;$ a = $12.208(2)\AA.$ The structure was refined to the final error indices R1 = 0.088 and R2 (weighted) = 0.069 using 194 independent reflections for which II_0$ > $3{\sigma}(I_0)$. On threefold axes near the centers of 6-oxygen rings, $7.4 Na^+$ ions and $0.6 Ag^+$ ions are found. Two non-equivalent 8-ring $Ag^+$ ions are found off the 8-ring planes, each containing about $0.6 Ag^+$ ions. Three non-equivalent Ag atom positions are found in the large cavity, each containing about 0.6 Ag atoms. This crystallographic analysis may be interpreted to indicate that $0.6 (Ag_6)^{3+}$ clusters are present in each large cavity. This cluster may be viewed as a nearly linear trisilver molecule $(Ag_3)^0$ (bond lengths, 2.92 and 2.94 $\AA;$ angle, $153^{\circ})$ stabilized by the coordination of each atom to a Ag^+$ ion at 3.30, 3.33, and 3.43 $\AA$, respectively. In addition, one of the silver atoms approaches all of the 0(1) oxygens of a 4-ring at $2.76\AA.$ Altogether $7.4 Na^+$ ions, $1.8 Ag^+$ ions, and 1.8 Ag atoms are located per unit cell. The remaining $1.0 Ag^+$ ion has been reduced and has migrated out of the zeolite framework to form silver crystallites on the surface of the zeolite single crystal.

• Bulletin of the Korean Chemical Society
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• v.15 no.11
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• pp.940-944
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• 1994

The crystal structure of an ethylene sorption complex of dehydrated $Ag_{12}-A $reacted with bromine vapor has determined by single-crystal X-ray diffraction techniques in the cubic space group of Pm3m at 22(l)$^{\circ}$C (a=12.180(2) ${\AA}$). The crystal was prepared by dehydration of $Ag_{12}$-A at 400 $^{\circ}$C and $2 {\times} l0^{-6}$ Torr for 2 days, followed by exposure to 200 Torr of ethylene gas at 24(l) $^{\circ}$C for 1 hr. After the ethylene gas was evacuated for 1 hr, the crystal was exposed to 180 Torr of bromine vapor at 24(l) $^{\circ}$C for 1.5 h. The structure was refined to the final error indices, $R_1=0.066\;and\;R_2$ (weighted)=0.055, using 137 independent reflections for which I>3${\sigma}$I. About 55% of the sodalite unit contain two 6-ring $Ag^+$ ions and the remaining 45% contain $Ag_6$ molecules complexed to 2 $Ag^+$ ions at 6-ring sites to give $(Ag^+)_2(Ag_6).$ Upon sorption of ethylene, 4.75 ethylene molecules were sorbed per unit cell and of these, only 1.25 ethylene molecules were brominated by treatment of dibromine because of the limitation of the available space for the reaction products in the large cavity. In the large cavity, each of 3.5 $Ag^+$ ions forms a lateral ${\pi}$ complex with an ethylene molecule. About 2.5 8-ring $Ag^+$ ions per unit cell interact with 1.25 1,2-dibromoethane and each of ca. 1.25 6-ring $Ag^+$ ions also interacts with one of bromine atoms of 1,2-dibromoethane. Each bromine atom approaches a carbon atom with C-Br(l)=2.07(20) ${\AA}$ and C-Br(2)=2.07(10) ${\AA}$, respectively.

• 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.

• Journal of Integrative Natural Science
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• v.8 no.3
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• pp.192-203
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• 2015

In view of the growing medicinal importance of pyrazole and its derivatives, the single crystal X-ray diffraction study was carried out for the potential active 2-Benzyl-3-[3-(4-bromo-phenyl)-1-phenyl-1H-pyrazol-4yl]-4,6-dioxo-5-phenyl-octahydro-pyrrolo[3,4-C]pyrrole-1-carboxylic acid ethyl ester ($C_{37}H_{31}BrN_4O_4$, H2O). In the title compound are two molecules exist in the asymmetric unit. It crystallizes in the monoclinic space group $P{\hat{i}}$ with unit cell dimension $a=13.361(18){\AA}$, $b=13.424(17){\AA}$ and $c=21.649(2){\AA}$ [${\alpha}=80.745(9)^{\circ}$, ${\beta}=79.770(10)^{\circ}$ and ${\gamma}=60.788(6)^{\circ}$]. The pyrazole ring adopts planar conformation. The sum of the bond angles at nitrogen atom of the pyrazole ring indicates the $Sp^2$ hybridized state. The crystal structure is stabilized by intramolecular C-H...O hydrogen bond interaction.

• Archives of Pharmacal Research
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• v.5 no.2
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• pp.79-86
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• 1982

Sulfisoxazole, $C-{11}H_{13}N_{3}S$, crystallized in the orthohombic system, space group Pbca, with a = 14.492(1), b = 11.563(1), c = 14.900(2) $\AA$ and Z = 8. Intensities for 1867(1360 observed) unique reflections were measured on a four-circle diffractometer wirh CuKa radiation ($\lambda$ = 1.5418$\AA$). The structure was solved by heavy atom methods and refined by full-matrix least-squares procedures to a final R of 0.094. The benzene ring plane makes an angle of $68^{\circ}C$ with the plane of the isoxazole ring, which is plannar. The conformational angle formed by the torsional angle C(4)-S-N(2)-C(7) is $54^{\circ}C$. There are two intermolecular hydrogen bonds in the structure. One of them is of the type N-H...H with the length 2.915$\AA$. Thus two dimensional networks of hydrogen bonds form infinite moelcular sheets parallel to the (001) plane. Adjacent sheets are bound together by van der Waals forces.

• Bulletin of the Korean Chemical Society
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• v.10 no.2
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• pp.191-196
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• 1989

We obtained the new complexes, $Fe{\eta}^4-R,R'-TPSCp](CO)_3$(R,R'-TPSCp = 1,1-disubstituted 2,3,4,5-Tetraphenyl-1-Silacyclopenta-2,4-diene; R = Ph, R' = Cl, R = R' = Cl) from the reaction of the corresponding R,R'-TPSCp with ironpentacarbonyl under reflux in toluene. Also, the analogous complexes with R = R' = Me and R = Me, R' = Cl were obtained in an identical manner. We have determined the crystal structure of $Fe[Ph(Cl)-TPSCp](CO_)3$ by using Mo ka, ${\lambda}$ = 0.71069${\AA}$, where the unit cell was found to be monoclinic with a = 9.042 (6)${\AA}$, b = 19.870 (9)${\AA}$, c = 17.426 (9)${\AA}$ and ${\beta}$ = 96.28(4)$^{\circ}$. The butadiene moiety of TPSCp ring is planar and the dihedral angle of the butadiene plane and C4-Si-C25 plane was opened up to 41.8$^{\circ}$. The C-C distances in the butadiene moiety were found to be 1.4346, 1.462, and 1.440 ${\AA}$, respectively. It may be said that the four ${\pi}$-electrons are delocalized over the four carbons in five membered ring through coordination with ironcarbonyl. In this complex Fe is either in distorted tetrahedron environment with the centroid of the four C-atom butadiene moiety and three carbons of the three carbonyls or in distorted square-pyramidal environment with two midpoints of double bonds of the butadiene moiety and two carbons of carbonyl defining the base of the pyramid and the carbon of remaining carbonyl the apex.

• Bulletin of the Korean Chemical Society
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• v.3 no.1
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• pp.9-13
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• 1982

Sulfametrole, $C_9H_{10}N_4O_3S_2$, crystallizes in the monoclinic system, space group $P2_1/n$ , with a = 8.145(2), b = 16.505(4), c = 9.637(1)${\AA},{\beta}=103.72(1)^{\circ},D_m=1.52gcm^{-3}$,Z=4.Intensities for 3594(2143 observed) unique reflections were measured on a four-circle diffractometer with Mo $K{\alpha}$ radiation $({\lambda}=0.71069{\AA})$. The structure was solved by direct method and refined by full-matrix least squares to a final R of 0.070. The geometrical features of the thiadiazole ring indicate some ${pi}$-electron delocalization inside the ring. The least squares planes defined by the benzene and thiadiazole rings are nearly perpendicular to each other(dihedral angle; $93.9^{\circ}$ ). All the potential hydrogen-bond donor atoms in the molecule, N(1) and N(2), are included in the hydrogen bonding. The molecules through hydrogen bonding form three dimensional network.

• 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.