• Journal of Integrative Natural Science
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• v.8 no.1
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• pp.30-39
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• 2015

The crystal structure of the potential active 2-amino-4-(4-hydroxy-3-methoxyphenyl)-7, 9-dimethyl-5-oxo-4, 5, 6, 7-tetrahydropyrano [2, 3-d] pyrazolo [3, 4-b] pyridine-3-carbonitrile ($C_{21}H_{22}N_5O_6S$) has been determined from single crystal X-ray diffraction data. In the title compound crystallizes in the monoclinic space group P-1 with unit cell dimension a=8.1201(9)${\AA}$, b=12.2684(4)${\AA}$ and c=12.387(2)${\AA}$ [${\alpha}=69.573^{\circ}$, ${\beta}=12.168^{\circ}$ and ${\gamma}=76.060^{\circ}$]. In the structure the pyrazole, pyridine and pyran are almost coplanar each other. The crystal packing is stabilized by intermolecular C-H...O and N-H... O hydrogen bond interaction.

• 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.14 no.1
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• pp.1-6
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• 1991

The crystal structure of licarin-B, a component of Myristicae Semen was determined by single crystal X-ray diffraction analysis. Crystal of the compound, which was recrystallized from the mixture of hexane and ether, is monoclinic with a=12.740(1), b=7.219(1), c=9.284(1) ${\AA}$, ${\beta}=94.75(1)^{\circ}$, $D_x=1.26$, $D_m=1.27\;g/cm^3$, space group P21, and Z=2. The structure was solved by direct method and refined by least-squares procedure to the final R value of 0.040 for 1532 independent reflections ${F{\ge}3{\sigma}(F)}$. The compound is a dimeric phenylpropanoid, and belongs to the neolignan analogues. The molecules are arranged along with the screw axis. The intermolecular contacts appear to be the normal van der Waals' forces.

• Korean Journal of Crystallography
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• v.11 no.3
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• pp.162-166
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• 2000

KD₂PO₄ single crystals were grown from D₂O with reagent KH₂PO₄ and the crystal structure was determined by X-ray and neutron diffraction methods. The crystals are tetragonal at room temperature, I42d, with lattice parameters of a=7.4633(7), c=6.9785(5) Å and Z=4. Intensity data were collected on an Enraf-nonius CAD4 diffractometer with a graphite monochromated MoK/sub α/ radiation (λ=0.7107Å) and on the neutron four circle single crystal diffractometer with Ge(331) monochromated neutron beam (λ=0.997Å). The structure was refined by full-matrix least-square to final R and wR values of 0.030 and 0.072, respectively, for 204 observed reflections with I>2σ(I) by X-ray diffraction and to final R=0.041 and wR=0.096 for 144 observed relfecdtions by neutron diffraction. The O…O distance of 2.516(4)Å obtained by X-ray diffraction is the same as that of 2.515(4)Å by neutron diffraction. On the other hand, the O-D/H distance of 0.84(4)Å by X-ray diffraction is considerably shorter than 1.029(7) Åby neutron diffraction. Hydrogen and deuterium can be readily distinguished by neutrons. In this crystal 66% of H-positions were substituted by D and the rest 34% occupied by H. The phase transition temperature of DKDP obtained with deuteration levels is f193K. This value agrees fairly well with the result of DSC measurement. The nuclear density distribution by neutron diffraction provides an observation of the disordered state of D/H in KD₂PO₄ at room temperature.

• Korean Journal of Crystallography
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• v.11 no.3
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• pp.137-146
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• 2000

The stoichiometric mix of evaporating materials for he CuInS₂ single crystal thin films was prepared. To obtain the single crystal thin films, CuINS₂ mixed crystal was deposited on etched semi-insulator GaAs(100) substrate by the hot wall epitaxy(HWE) system. The source and substrate temperature were 640℃ and 430℃, respectively and the thickness of the single crystal thin films was 2 ㎛. The crystalline structure of single crystal thin films was investigated by the photoluminescence and double crystal X-ray diffraction(DCXD). The carrier density and mobility deduced from Hall data are 9.64x10/sup 22//㎥ and 2.95x10/sup -2/ ㎡/V·s, respectively at 293 K. he optical energy gap was found to be 1.53 eV at room temperature. From the photocurrent spectrum obtained by illuminating perpendicular light on the c-axis of the thin film, we have found that the values of spin orbit coupling splitting ΔSo and the crystal field splitting ΔCr were 0.0211 eV and 0.0045 eV at 10K, respectively. From PL peaks measured at 10K, were can assign the 807.7 nm (1.5350 eV) peak to E/sub x/ peak of the free exciton emission, the 810.3 nm(1.5301 eV) peak to I₂ peak of donar-bound exciton emission and the 815.6 nm(1.5201 eV) peak to I₁ peak of acceptor-bound excition emission. In addition, the peak observed at 862.0 nm(1.4383 eV) was analyzed to be PL peak due to donor-acceptor pair(DAP).

• Korean Journal of Crystallography
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• v.16 no.2
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• pp.107-127
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• 2005

Five Cu(II) compounds were obtained from different copper salts with btp ligands, and their structures were determined by X-ray crystallography. The structure of coordination polymer 2 contains btp-bridged tetranuclear Cu(II) units weakly connected by nitrate ions, and the structure of a discrete Cu(II) molecule 1 contains acetates and btp ligands. With perchlorate anions, two btp ligands bridge Cu(II) ions to form a double zigzag chain 3, while a single zigzag chain 4 is created with sulfate anions. The reaction of $Cu(NO_{3})_{2}$ containing $NH_{4}PF_{6}$ with btp ligands also produced a polymeric compound 5 containing $Cu(H_{2}O)_{2}^{2+}$ and $Cu(NO_{3})_{2}$ units alternatively bridged by btp ligands with H-bonds between copper bonded water and nitrate oxygen atoms. Five Zn(II) compounds were obtained from different zinc salts with btp ligands, and the structures of polymeric compounds (6, 7 and 8) and monomeric compounds (9 and 10) were determined by X-ray crystallography. With nitrate, chloride and bromide anions, btp ligands bridge Zn(II) ions to form polymeric compounds (6, 7 and 8), but btp ligands coordinate to a Zn(II) ion to form monomeric complexes (9 and 10) with $PF_{6}^{-}$ and perchlorate anions. Four silver salts and btp ligands produced two kinds of structures, dinuclear 20-membered rings and one-dimensional zigzag chain depending on different anions. For $ClO_{4}^{-}$ and OTf anions, weak interactions between Ag(I) and anions make dinuclear 20-membered rings construct polymeric compounds (11 and 13). For $PF_{6}^{-}$ anion, there are also weak interactions between Ag(I) and $F(PF_{6}^{-})(12)$, but they do not construct a polymeric compound. For $O_{2}CCF_{3}^{-}$ anion, btp ligands bridge Ag(I) atoms to make one-dimensional zigzag chain (14), and there are also interactions between Ag(I) and anions.

• Korean Journal of Crystallography
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• v.11 no.1
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• pp.16-21
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• 2000

(Yb/sub x/Y/sub 1-x/)Ca₄O(BO₃)₃ single crystals where x=0.3,8,15,20% were grown by Czochralski Method. The crystals grown under the optimum conditions were transparent and colorless with good crystal form. Using polarizing microscope, crystal defects such as parasite crystals and bubbles were detected depending on the composition of melts and pulling rates. The optimum growth parameters for high quality of single crystals were 15∼20 rpm of rotation rate and 2mm/h of pulling rate at the flow rate of 2 l/min of Nitrogen gas. The relationship between crystal axes and optical axes was investigated by optical crystallographic method, polarization technique and single crystal X-ray method. From the spectroscopic measurements, it was confirmed that there were strong absorption bands at 900 and 976.4 nm and strong emission band at 976.4 nm in Yb/sup 3+/ ion doped YCa₄O(BO₃)₃ crystal. For the application of second harmonic generation of 1.064 ㎛ laser, non-linear optical devices with θ=32.32° and Ψ=0°, λ/10 of flatness and the size of 6x8x5.73 mm were fabricated from the grown YCa₄O(BO₃)₃ crystal.

• Korean Journal of Crystallography
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• v.12 no.4
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• pp.207-211
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• 2001

The crystal structure of the title complex, Cd(SCN)₂{CH/sub 6/H/sub 10/(NH₂)₂}₂(1) has been analyzed by X-ray single crystallography. The complex 1 crystallizes in the monoclinic system P2₁/ space group with a=11.842(2), b=7.926(2), c=11.291(2) Å, β=106.73(3)°V=1014.8(4)Ų, Z=2, R₁=0.0518 and ωR₂=0.1315 for 1775 independent reflections. The central Cd(II) atom of this com-plex has a slightly distorted octahedral coordination geometry, with the 1,2-Diaminocyclohexane ligands functioning as an N,N'-bidentate and the thiocyanate ligands bonding through the sulfur atom in a trans arrangement.

• Analytical Science and Technology
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• v.11 no.1
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• pp.42-46
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• 1998

The reaction of $({\eta}^5-C_5Me_5)_2K$ with $BiCl_3$ yielded $({\eta}^5-C_5Me_5)_2BiCl$[I], the first organobismuth compound with ${\pi}$-bonded cyclopentadienyl ring. The compound I which was the violet crystal (yield, 30%) was decomposed to $PCpBiCl_2$. The Structure of $({\eta}^5-C_5Me_5)_2BiCl$ was identified as single crystal by X-ray diffraction method. The eliminated product $C_{20}H_{30}$, triclinic crystal of space group p1(Z=2) which was attached with C-C ${\sigma}$-bond of two cyclopentadienyl was defined by the structural analysis.

• Korean Journal of Crystallography
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• v.11 no.4
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• pp.212-223
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• 2000

A stochiometric mix of CuInTe₂ polycrystal was prepared in a honizonatal furnace. To obtain the single crystal thin films, CuInTe₂ mixed crystal was deposited on throughly etched GaAs(100) by the HWE system. The source and substrate temperatures were 610℃ and 450℃ respectively, and the thickness of the deposited single crystal thin film was 2.4㎛. CuInTe₂ single crystal thin film was proved to be the optimal growth condition when the excition emission spectrum was the strongest at 1085.3 nm(1.1424 eV) of photoluminescence spectrum at 10 K, and also FWHM of Double Crystal X-ray Rocking Curve (DCRC) was the smallest, 129 arcsec. The Hall effect on this sample was measured by the method of Van der Pauw, and the carrier density and mobility dependent on temperature were 9.57x10/sup 22/ electron/㎥, 1.31x10/sup -2/㎡/V·s at 293 K, respectively. The ΔCr(Crystal field splitting) and the ΔSo (spin orbit coupling splitting( measured at f10K from the photocurrent peaks in the short wavelength of the CuInTe₂ single crystal thin film were about 0.1200 eV, 0.2833 eV respectively. From the PL spectra of CuInTe₂ single crystal thin film at 10 K, the free exciton (E/sub x/) was determined to be 1064.5 nm(1.1647 eV) and the donor-bound exciton(D/sup 0/, X) and acceptor-bound exciton (A/sup 0/, X) were determined to be 1085.3 nm(1.1424 eV) and 1096.8 nm(1.1304 eV0 respectively. And also, the donor-acciptor pair (DAP)P/sub 0/, DAP-replica P₁, DAP-replica P₂ and self-activated (SA) were determined to be 1131 nm (1.0962 eV), 1164 nm(1.0651 eV), 1191.1 nm(1.0340 eV) and 1618.1 nm (0.7662 eV), respectively.