• Bulletin of the Korean Chemical Society
• /
• 제31권7호
• /
• pp.1875-1880
• /
• 2010

A dicycle pyrazoline derivative, 1-phenyl-5-(p-fluorophenyl)-3,4-($\alpha$-p-fluoro-tolylenecyclohexano) pyrazoline, was synthesized and characterized by elemental analysis, IR, UV-vis, fluorescence spectra and X-ray single crystal diffraction. Density function theory (DFT) calculations were performed by using B3LYP method with 6-$311G^{**}$ basis set. The optimized geometry can well simulate the molecular structure. Vibrational frequencies were predicted, assigned and compared with the experimental values, which suggest that B3LYP/6-$311G^{**}$ method can well predict the IR spectra. Both the experimental electronic absorption spectra and the predicted ones by B3LYP/6-$311G^{**}$ method reveal three electron-transition bands, with the theoretical ones having some red shifts compared with the experimental data. Natural bond orbital analyses indicate that the absorption bands are mainly derived from the contribution of n $\rightarrow\pi^*$ and $\pi\rightarrow\pi^*$ transitions. Fluorescence spectra determination shows that the title compound can emit blue-light at about 478 nm. On the basis of vibrational analysis, the thermodynamic properties of title compound at different temperature have been calculated, revealing the correlations between $C^0_{p,m}$, $S^0_m$, $H^0_m$ and temperature.

• 통합자연과학논문집
• /
• 제8권1호
• /
• pp.30-39
• /
• 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.

• Archives of Pharmacal Research
• /
• 제14권2호
• /
• pp.137-142
• /
• 1991

The structure of a $\beta$-allyl type phenylpropanoid was determined by single crystal X-ray diffraction analysis. The compound was recrystallized from a mixture of n-hexane and benzene in monoclinic crystal system with a = 24.782 (2), b = 10.537 (1), c = 7.871 (1) ${\AA}, \beta=95.74$ (1)$^\circ, $D_x$=1.216, $D_m$=1.22g/$cm^3$, space group $P2_1/a$, and Z=4. The structure was solved by direct method and refined by least-squares procedure to the final R value of 0.054 for 2824 observed reflections {$F{\geq}3\sigma(F)$}. The molecular geometry shows a most stable trans-form with respect to the bulky phenyls, and this conformation is settled by an intramolecular hydrogen bond. In the crystal, the molecules are arranged along with the screw axis, and stabilized by the $O{\cdot}H{\cdots}O$ type intermolecular hydrogen bonds. The other intermolecular contacts appear to be the normal van der Waals' interactions. The compound is a dimeric phenylpropanoid, and belongs to the neolignan analogues.

• 한국결정성장학회지
• /
• 제7권2호
• /
• pp.244-252
• /
• 1997

$LiCO_3, Al_2O_3, Fe_2O_3$ 혼합물을 1620K에서 반응시켜 리튬전지의 음극재료로 응용이 가능한 스핀넬형 $LiAl_{2.5}/Fe_{2.5}O_8$를 합성하였다. XRD의 Rietveld 해석을 통하여 결정구조 해석을 하였다. 고용체의 공간군은 $P4_3$32(a=8.1293$\AA$)이고, 결정구조해석의 최종 Residual index는 약 5%정도이었다. 역 스핀넬구조에서 양이온 $Al^{3+}, Fe^{3+}$은 4-배위와 6-배위로 위치하고, $Li^+$은 4b, 12d의 6-배위자리에 존재하였다.

• Archives of Pharmacal Research
• /
• 제15권1호
• /
• pp.52-57
• /
• 1992

The molecular structure of a natural compound was determined by single crystal X-ray diffraction analysis. The compound was isolated by methanol extraction and repeated chromatography from the stem of Paulownia tomentosa. Yellow prismatic crystals of the compound, which were recrystallized from tetrahydrofuran, are triclinic, with a = 7.310 (6), b = 10.753(6), c = 11.586(5) ${\AA}.\;\alpha= 93.30(6),\;\beta=105.62(10),\;\gamma=109.49(7)^\circ,\;D_x=1.514,\;D_m=1.51 g/cm^3$, space group P1 and Z = 2. The structure was solved by direct method, and refined by least-squares procedure to the final R-value of 0.032 for 1271 independent reflections $(F\le3\sigma{(F))}$. The compound is one of new furanquinone analogue. The molecule has a nearly planar conformation with an intramolecular hydrogen bond. In the crystal, the planar molecules are arranged as a prallel sheet-like pattern, and these stackings are stabilized by the O-H...O type intermolecular hydrogen bonds. The other intermolecular contacts appear to be the normal van der Waals interactions.

• Bulletin of the Korean Chemical Society
• /
• 제22권11호
• /
• pp.1224-1230
• /
• 2001

Single crystals of nanocomposite [GaO4Al12(OH)24(H2O)12][Al(OH)6Mo6O18]2(OH)${\cdot}$30H2O, 2, were obtained by the reaction between [GaO4Al12(OH)24(H2O)12]7+ and [Mo7O24]6- clusters in an aqueous solution, analogously to the [AlO4Al12(OH)24(H2O)12][Al(OH)6Mo6O18]2(OH)${\cdot}$29.5H2O nanocomposite, 1. The crystal structure of 2 was determined by single crystal x-ray diffraction; space group $C2}c$ (No. 15), a = 27.418(2) $\AA$, b = 15.647(2) $\AA$, c = 23.960(4) $\AA$, $\beta$ = $102.850(9)^{\circ}$, V = 10,021.5(20) $\AA3$ , Z = 4. Detailed analysis of the structural data show that the clusters are held by intimate hydrogen bondings of the surface O2- and OH- groups of the clusters as well as the ionic interactions between the oppositely charged cluster ions.

• Journal of Microbiology and Biotechnology
• /
• 제31권10호
• /
• pp.1393-1400
• /
• 2021

Acetone-butanol-ethanol (ABE) fermentation by the anaerobic bacterium Clostridium acetobutylicum has been considered a promising process of industrial biofuel production. Phosphotransbutyrylase (phosphate butyryltransferase, PTB) plays a crucial role in butyrate metabolism by catalyzing the reversible conversion of butyryl-CoA into butyryl phosphate. Here, we report the crystal structure of PTB from the Clostridial host for ABE fermentation, C. acetobutylicum, (CaPTB) at a 2.9 Å resolution. The overall structure of the CaPTB monomer is quite similar to those of other acyltransferases, with some regional structural differences. The monomeric structure of CaPTB consists of two distinct domains, the N- and C-terminal domains. The active site cleft was formed at the interface between the two domains. Interestingly, the crystal structure of CaPTB contained eight molecules per asymmetric unit, forming an octamer, and the size-exclusion chromatography experiment also suggested that the enzyme exists as an octamer in solution. The structural analysis of CaPTB identifies the substrate binding mode of the enzyme and comparisons with other acyltransferase structures lead us to speculate that the enzyme undergoes a conformational change upon binding of its substrate.

• 한국분말야금학회:학술대회논문집
• /
• 한국분말야금학회 2006년도 Extended Abstracts of 2006 POWDER METALLURGY World Congress Part 1
• /
• pp.60-61
• /
• 2006

In this contribution, we attempted a theoretical analysis on the validity of the widely-accepted idea that rough and singular surfaces can coexist in a crystal at equilibrium. By manipulating the Cahn and Hoffman capillarity vector, the conclusion that a crystal at equilibrium should be composed either of singular surfaces or of rough ones was reached.

• 분석과학
• /
• 제36권4호
• /
• pp.198-203
• /
• 2023

The reaction of cis-protected (Me4en)Pd(II) species with potentially multidentate bis(benzylthio)methylenepropanedioate (L) was carried out to obtain a monometallic compound, [(Me₄en)Pd(L)], in O,O'-coordination mode. The bis(benzylthio)methylene group was bent strikingly from the palladium square plane at the dihedral angle of 70.40°. The physicochemical properties of the present palladium(II) compound were fully characterized by means of infrared and nuclear magnetic resonance spectroscopy, thermogravimetric analysis, and single-crystal X-ray diffraction measurement.

• Applied Microscopy
• /
• 제41권1호
• /
• pp.75-79
• /
• 2011

For quantitative analysis of nano-crystal structure, we reported the accuracy improvement method of lattice parameters measured from electron diffraction. For calculation of Au lattice parameters used as a standard crystal structure, it was considered two different acquisition methods (detector and enegy-filter) and three different calculation methods (conventional, least-square and regression fit). As a result, the measurement reliability could be enhanced by using CCD camera which gives higher performance, while energy-filtering did not affect the improvement the camera constant accuracy. Also, the accuracy of lattice parameters could be improved up to $10^{-4}$ order by regression fitting with correction formula. Finally, it is expected that the combination of regression fitting and intensity extraction from energy-filtered precession electron diffraction gives a solution of quantitative structure analysis for unknown nano-crystals.