• 약학회지
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• 제26권1호
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• pp.9-23
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• 1982

The structure of 1-butyl-3-sulfanyl urea, ($C_{11}H_{17}N_{3}O_{3}S$) carbutamide has been determined from 575 significant independent reflections collected on an automated four-circle diffractometer. The crystals are orthorhomic, space group, $P2_{1}2_{1}2_{1}$, Z=4, with unit cell dimensions a=9.257 (2), b=9.928 (2), c=15.287 (3)${\AA}$. The structure was solved by the direct methods and refined by least-squares procedure to a final R value of 0.062. Features of the structure include layers of molecules joined by N-H....O hydrogen bond distances ranging from 2.745 to 3.100${\AA}$ involved in a bifurcated hydrogen bond across two fold screw along a and b axes. The atoms forming the urea system are essentially planar.

• 한국결정학회지
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• 제6권2호
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• pp.75-79
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• 1995

The crystal structure of Tris(ethylenediamine)nickel(II)Chromate has been determined by X-ray crystallography. Crystal data : a=9.027(2)Å, c=9.751(5)Å이며, Z=2, V=687.9(2)Å3, Dc=1.714gcm-3, μ=21.635-1. The intensity were collected with Mo-Kα radiation (λ=0.7107Å) on an automatic four-circle diffractometer with a graphite monochromator. The structure was solved by Patterson method and refined by full matrix least-square methods using unit weights. The final R and S values were R=0.029, Rw=032, Rall=0.049 andS=0.018 for 342 observed reflections. The chromate ions are located at position of point of point symmetry 32 and their oxygens are sixfold disodered in an unusual way. Extensive strong hydrogen bonds between complex cations and chromatic anions are found in axial and equatorial directions.

• Bulletin of the Korean Chemical Society
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• 제3권1호
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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.

• 약학회지
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• 제24권2호
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• pp.135-141
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• 1980

The crystal and molecular structure of 2-methyl-3-(N-trimethyl ammonium)phenol iodide, $C_{10}H_{16}NOI, was determined by X-ray diffraction method. The compound crystallizes in the orthorhombic space group $P_{na2}_{1}$ with a=13.327(3), b=12.496(3), C=7.227(2)A and Z=4. A total of 489 independent observed reflections were collected by the automated Four-circle diffractometer and was solved by heavy atom method and refined by anisotropic block-diagonal least-squares method to the R value of 0.04. The benzene ring is slightly distorted from regular hexagon. The I atom and 2-methyl-3-(N-trimethyl ammonium)phenol group is held together by van der Waals forces in the crystal. Intermolecular hydrogen bond is of the type O-H....I with the length 3.35.angs.. Apart from the hydrogen bonding system the molecules are held together by van der Waals forces in the crystal.

• 대한화학회지
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• 제25권6호
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• pp.343-350
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• 1981

P-Aminobenzaldehyde cyclohexylthiosemicarbazone의 결정 및 분자구조를 Computer controlled four circle diffractometer에 의한 X-선 회절방법으로 해명하였다. 결정은 공간군 C2/c의 단사형계에 속하며 단위세포 상수는 a = 12.488(2), b = 12.276(4), c = 19.997(6)${\AA}$, ${\beta}=103.55(3)^{\circ}$이고 z = 8이다. 구조는 중원자법과 Fourier 방법으로 규명하였으며 full-matrix 최소자승법으로 정밀화하였다. 최종 R값은 2712개의 회절반점에 대하여 0.058이었다. 분자는 N(2)-N(3)결합에대하여 C(8)-S는 trans, C(8)-N(1)은 cis형으로 놓여 있으며 N(1)과 N(3) 원자들이 분자내 수소결합을 만들고 있다. 의자모양의 cyclohexane 고리는 benzene 고리와 $40.7^{\circ}$의 면각을 이루고 있다. 결정내의 분자들은 수소 결합들로 모여져 있는데 $N(2)-H{\ldots}S$ 수소결합이 분자들을 이합체 꼴을 만들며 이들 분자들을 $N-H{\ldots}N$ 수소결합들이 이어주고 있다.

• 한국결정학회지
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• 제11권3호
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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.

• Bulletin of the Korean Chemical Society
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• 제15권3호
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• pp.245-249
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• 1994

NaMg[$Cr(C_2O_4)_3]{\cdot}10H_2O$ crystallizes in the trigonal space group P$\bar{3}$c1, with a=b= 16.969(3), c=12.521(3) ${\AA}$, ${\alpha}={\beta}=90^{\circ},\;{\gamma}=120^{\circ},\;{\rho}=1.734 \;gcm^{-3},\;{\mu}=6.46\;cm^{-1}$, Z=6. Intensities for 1062 unique reflections were measured on a four-circle diffractometer with Mo K${\alpha}$ radiation (${\lambda}=0.71069\;{\AA}$). The structure was solved by direct methods and refined to a final ${\omega}$R value of 0.084. X-ray crystal structure showed that magnesium ion appears to be occupied over two sites with the occupancy ratio of 2:1. The crystal possesses 10 water molecules instead of previously estimated 9 water molecules.

• Bulletin of the Korean Chemical Society
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• 제10권2호
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• pp.177-184
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• 1989

The structure of cholesteryl isobutyrate, $(CH_3)_2CHCOOC_{27}H_{45}$, was determined by single crystal X-ray diffraction methods. Cholesteryl isobutyrate crystallized monoclinic space group $P2_1$, with a = 15.115 (8)${\AA}$, b = 9.636 (5)${\AA}$, c = 20.224 (9)${\AA}$, ${\beta}$ = 93.15 (5)$^{\circ}$, z = 4, $D_c = 1.03 g/cm^3 $and Dm= 1.04 g/$cm^3$. The intensity data were measured for the 3417 reflections, within $sin{\theta}/{\lambda} = 0.59{\AA}^{-1}$, using an automatic four-circle diffractometer and graphite monochromated Mo-$K_{\alpha}$ radiation. The structure was solved by fragment search Patterson methods and direct methods and refined by full-matrix least-squares methods. The final R factor was 0.129 for 2984 observed reflections. The two symmetry-independent molecules (A) and (B) are almost fully extended. The molecules are in antiparallel array forming monolayers with thickness $d_{100}$ = 15.2${\AA}$, and molecular long axes are nearly parallel to the [$\bar{1}$01] directions. The two distinct molecules form separate stacks with almost the same orientations, but with differing degrees of steroid overlap. Thers is a close packing of cholesteryl groups within the monolayers. The packing type is similar to those of cholesteryl hexanoate and cholesteryl oleate.

• 대한화학회지
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• 제28권4호
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• pp.205-209
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• 1984

Thiosinamine, $H_2NCSNHCH_2CHCH_2$의 결정 및 분자구조를 X-선 회절법으로 규명하였다. 이 결정은 공간군 $P2_1/a$의 단사정계에 속하며 단위세포상수는 a = 9.819(3), b = 8.553(3), c = 9.170(2)${\AA}$, ${\beta}$ = 127.3(1)$^{\circ}$이고 z = 4이다. 814개의 회절 반점에 대한 강도 data는 Rigaku-Denki 자동 4축 회절기를 써서 얻었다. 구조는 직접법과 Fourier법으로 규명하였으며 좌표의 정밀화는 Full Matrix 최소 자승법에 의하여 행하였고 최종의 R값은 0.046이다. Thiourea moiety는 평면이며, 결합길이와 결합각은 thiourea unit를 포함하는 화합물에서 얻어진 값들과 잘 일치하고 있다. 분자들은 결정내에서 b축을 따라 두 종류의 N-H${\cdots}$S수소결합에 의하여 상호 결합하고 있다.

• Bulletin of the Korean Chemical Society
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• 제14권6호
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• pp.713-717
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• 1993

The crystal structure of the potassium salt of penicillin V has been studied by the X-ray crystallographic methods. Crystal data are as follows; potassium 3,3-dimethyl-7-oxo-6-phenoxyacetoamido-4-thia-1- azabicyclo[3.2.0]-heptane-2${\alpha}$-carboxylate, $K^+{\cdot}C_{16}H_{18}N_2O_5S^-$, $M_r$= 388.5, triclinic, Pl, a= 9.371 (1), b= 12.497 (2), c= 15.313 (2) ${\AA},\;{\alpha}= 93.74\;(2),\;{\beta}=99.32\;(1),\;{\gamma}=90.17\;(1)^{\circ},\;V=1765.7\;(2)\;{\AA}^3$, Z=4, $D_m=1.461\;gcm^{-1},\;{\lambda}(Cu\;K{\alpha})=1.5418\;{\AA},\;{\mu}=40.1\;cm^{-1}$, F(000)=808, T=296 K. The structure was solved by the heavy atom and difference Fourier methods with intensity data measured on an automated four-circle diffractometer. The structure was refined by the full-matrix least-squares method to a final R= 0.081 for 3563 observed $[I_0{\geq}2{\sigam}(I_0)]$ reflections. The four independent molecules assume different overall conformations with systematically different orientations of the phenyl groups although the penam moieties have the same closed conformations. There are intramolecular hydrogen bonds between the exocyclic amide nitrogen and phenoxy oxygen atoms. The penam moiety is conformationally very restricted although the carboxyl and exocyclic amide groups apparently have certain rotational degrees of freedom but the phenyl group is flexible about the ether bond despite the presence of the intramolecular N-H${\cdots}$O hydrogen bond. There are complicated pseudo symmetric relationships in the crystal lattice. The penam moieties are related by pseudo 20.5 screw axes and the phenyl groups by pseudo centers of symmetry. The potassium ions, related by both pseudo symmetries, form an infinite zigzag planar chain parallel to the b axis. Each potassium ion is coordinated to seven oxygen atoms in a severely distorted pentagonal bipyramid configuration, forming the infinite hydrophilic channels which in turn form the molecular stacks. Between these stacks, there are only lipophilic interactions involving the phenyl groups.