• Korean Journal of Crystallography
• /
• v.9 no.1
• /
• pp.15-20
• /
• 1998

Single crystals of lithium heptaborate, Li3B7O12(M=288.49), have been grown and their structure was determined by the x-ray powder diffraction and the single crystal diffraction technique. It is found that the borate anion consists of two(B3O7)3- and (B3O8)5- groups a unit cell. The space group was determined to be P-1(Ci1) with a=6.500(3) Å, b=7.839(2) Å, c=8.512(1) Å, α=92.07(2)˚, β=104.97(2)˚, γ=99.35(3)˚, V=412.0(2) Å3, Z=2 Dx=2.32 g cm-3, MoKα, λ=0.71069 Å, μ=2.15cm-1, T=293K. The structure was refined to R=0.0339 and wR=0.0882 for 2296 unique reflections by the single crystal diffraction. By the x-ray powder diffraction, we could obtain the similar results.

• Archives of Pharmacal Research
• /
• v.14 no.2
• /
• 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.

• Archives of Pharmacal Research
• /
• v.15 no.1
• /
• 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.

• Korean Journal of Crystallography
• /
• v.16 no.1
• /
• pp.1-5
• /
• 2005

The structure of the title compound has been determined by single-crystal X-ray diffraction work. The crystals are orthorhombic, space group $Pna2_1$ with a=11.095(3), b=21.834(7), c=12.574(4) $\AA$, and R1=0.0667. The average carbon bond length in aromaticity In the molecule is 1.386(1) $\AA$ and the average single bond length linking the central benEene ring and peripheral phenyl rings is 1.491(3) $\AA$. The average dihedral angle between the central benzene ring and each of six peripheral phenyl rings is $67.1(1)^{\circ}$ and the average dihedral angle between neighboring two phenyl rings is $55.0(1)^{\circ}$. Thus the molecule adopts a quasi-propeller configuration with approximate six-fold rotation symmetry.

• Journal of the Korean Magnetic Resonance Society
• /
• v.8 no.2
• /
• pp.86-95
• /
• 2004

A Cu(I) complex with an asymmetric TTF derivative (CET-EDTTTF) is prepared from the slow-diffusion method using CET-EDTTTF and Cu(I)Br solutions and characterized by X-ray crystallography and EPR spectroscopy. Structural analysis shows Cu(I) ions are tetrahedrally coordinated to two bridging bromides, one terminal bromide, and one S atom from CET-EDTTTF. Detailed geometrical and EPR analysis identified that the dimmer molecule contains [Cu$_2Br_4]^{2-}$ anion between two [CET-EDTTTF]$^+$ radical cations. Single-crystal EPR investigation of the complex reveals that the ganisotropy is unusually big, compared to those of the previously reported TTF+ cation radicals, implying that there is significant contribution of the Cu d-orbital to the HOMO of the complex.

• Bulletin of the Korean Chemical Society
• /
• v.27 no.10
• /
• pp.1572-1576
• /
• 2006

A dimeric precursor, $[Cu(dmae)(OCOCH_3)(H_2O)]_2$ for the CVD of copper metal films, (dmaeH = N,N-dimethylaminoethanol) was synthesized by the reaction of copper(II) acetate monohydrate ($Cu(OCOCH_3)_2{\cdot}H_2O$) and dmaeH in toluene. The product was characterized by m.p. determination, elemental analysis and X-ray crystallography. Molecular structure of $[Cu(dmae)(OCOCH_3)(H_2O)]_2$ shows that a dimeric unit $[Cu(dmae)(OCOCH_3)(H_2O)]_2$ is linked to another through hydrogen bond and it undergoes facile decomposition at 300 C to deposit granular copper metal film under nitrogen atmosphere. The decomposition temperature, thermal behaviour, kinetic parameters, evolved gas pattern of the complex, morphology, and the composition of the film were also investigated.

• Korean Journal of Crystallography
• /
• v.8 no.2
• /
• pp.144-148
• /
• 1997

the molecular and crystal 3-dimensional structure of bentazone, C10H12N2O3S, has been determined from single crystal x-ray diffraction study. Crystal system is monoclinic: a=8.7817(9)Å, b=9.6059(9) Å, c=13.574(9) Å, β=97.269(1)', V=1136.1(6)Å, space group : P21/c, z=4. The molecular structure model was solved by direct method and refined by full matrix least squares. The final reliable factor, R, is 0.045 for 1396 independent reflections(Fo2>4σFo2). A molecule has a staggered conformation with thiocarbazin ring and isopropyl functional group and the molecules by hydrogen bonds are cross stacked along the c-axis.

• Korean Journal of Crystallography
• /
• v.12 no.4
• /
• pp.222-226
• /
• 2001

The title complex, $Ni(L)_4(NCS)_2$(1) (L=2-ethylimidazole) has been synthesized and charac-terized by X-ray single crystallography. The complex 1 crystallizes in the tertragonal system P4nc space group with a=10.587(2), $c=12.927(3){\AA}$, Z=2m, $R_1$=0.581 and $wR_$=0.1675 for 672 independent reflection. The central Ni(II) atom of the complex has a regular octa-hedral coordination geometry, with the 2-ethylimidazole ligands bonding through nitrogen atom and the isothiocyanate ligands bonding through nitrogen atom in a trans arrangement.

• Korean Journal of Crystallography
• /
• v.3 no.2
• /
• pp.120-128
• /
• 1992

Single crysals of BaTiO3 were grown by TSSG technique at various cooling rates. Morpolo girts, defects and domain structures of the grown crystals were investigated. At the cooling rates below 0.5℃/hr, equant single crystals were obtained and the 11111 faces were dominantly developed. If the cooling rate was much faster or if the vortical temperature gradient in the so lotion was very large, the solution became unstable and the needle formed BasTil04 o crystals were precipitated. Two sets of parallel lamella domains are arranged perpendicular to each other and the irregularly shaped boundaries are fixed between them. These sets of domains show remarkable orientation contrast in x-ray topography. Heating the crystal above 127℃, the phase transition from tetragonal to cubic occurs. The phase transition front (PTF) moves in the direction of temperature gradient. Domains in the tetragonal phase are successively rearranged and regular strain patterns appear in the cubic phase. The habit plane of PTF in BaTi03 is found to deviate from a l1101 lattice plane by app roximately 9°.

• Korean Journal of Crystallography
• /
• v.1 no.1
• /
• pp.19-28
• /
• 1990

6H-SiC is a promising material (Eg=3.0eV) for blue light-emitting doide and high-temperature semiconducting device. In the experiment, single crystals of a-SiC have been grown by the sublimation method to fabricate blue light~emitting diode. During the growth of a-SiC single crystals, a temperature Vadient, yonh temperature and pressure ranges were kept 44℃/cm , 1800-1990℃ and 50-1000 mTorr, respectively. Single crystals obtained in Acheson furnace were used as seed crystals. Polarizing microscopy and back-reflection X-ray Laue diffraction showed that the a-SiC crystal was epitaxially and on the seed crytal. It was found by XRD analysis that when other growth conditions were the same, a-SiC was grown at the temperature above 1840℃ and 3C-SiC was gown at lower temperature or under low supersaturation of vapor. The carrier type. concentration and mobility were measured be hole(p-type), 7.6x1014cm-3 and 19cm2V-1sec-1, respectively, by van der Pauw method.