• Korean Journal of Crystallography
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• v.15 no.1
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• pp.24-28
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• 2004

The structure of $C_{12}H_{15}N_3O_3$ has been determined by X-ray diffraction methods. The crystal system is monoclinic, space group $P2_1/c$, unit cell constants, a = 12.9955(9) ${\AA}$, b = 7.7137(5) ${\AA}$, c = 13.4699(11) ${\AA}$, ${\beta}$ = 107.86(1)$^{\circ}$, V = 1285.2(1) ${\AA}^3$, T = 296 K, Z = 4, $D_c$ = 1.350 $Mgm^{-3}$. The intensity data were collected on an Enraf-Nonius CAD-4 Diffractometer with graphite monochromated Mo $K{\alpha}$ radiation (${\lambda}$ = 1.71073 ${\AA}$). The molecular structure was solved by direct methods and refined by full-matrix least squares to a final R = 4.19% for 1644 unique observed $F_0\;>\;4{\sigma}(F_0)$ reflections 193 parameters.

• Journal of the Korean Chemical Society
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• v.28 no.4
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• pp.205-209
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• 1984

The crystal and molecular structure of thiosinamine, $H_2NCSNHCH_2CHCH_2$, has been determined by X-ray diffraction method. The crystals are monoclinic, space group $P2_1/a$ with four molecules in a unit cell of dimensions, a = 9.819(3), b = 8.553(3), c = 9.170(2)${\AA}$, ${\beta}$ = 127.3(1)$^{\circ}$, and z = 4. Intensity data for 814 reflections were collected with a Rigaku-Denki automatic four circle diffractometer. The structure was solved by direct and Fourier methods. Refinements were carried out by full matrix least-squares method to a final R value of 0.046. The thiourea unit is planar, and the bond lengths and angles in that unit agree well with those in the compounds which contain a thiourea moiety. The molecules are linked together by the two patterns of N-H${\cdots}$S hydrogen bonds along the b-axis.

• Journal of the Korean Chemical Society
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• v.24 no.3
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• pp.193-200
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• 1980

The crystal structure of N-acetyl-L-cysteine, $C_5H_9NO_3S,$ has been determined from three dimensional photographic intensity data $(CuK{\alpha}$ radiation) by single crystal X-ray diffraction analysis. There is one formula unit in the triclinic unit cell with a = 7.04(3), b = 5.14(2), c = 8.25(3) ${\AA}$, ${\alpha}$ = 106(2), ${\beta}$ = 51(1), ${\gamma}$ = 124(2)$^{\circ}$ and space group P$_1$, The structure was solved by the direct method and refined by the full matrix least-squares method. The final R value is 12.3% for 629 observed reflections. The C-carboxyl group and the N-acetyl group are very neary planar. The molecule appears to form with neighboring molecules a hydrogen bond, $O-H{\cdot}{\cdot}{\cdot}O(3)$ of length 2.59${\AA}$.

• Korean Journal of Crystallography
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• v.9 no.1
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• pp.71-76
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• 1998

Crystal structure of Bis(ethylenediamine)palladium(II)-Bis(oxalato)palladate(II0 has been determined by X-ray crystallography. Crystal data : (Pd(C2H8N2)2.Pd(C2O4)2), Fw=509.04, Monocline, Space Group P21/c (no=14), a=6.959(2), b=13.506(2), c=15.339(2) Å, β=99.94(3), Z=4, V=1420 Å3, Dc=2.380 gcm-3, μ=25.46cm-1, F(000)=992. The intensity data were collected with Mo-Kα radiation (λ=0.7107 Å) on an automatic four-circle diffractometer with a graphite monochromater. 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=0.021, Rw=0.030, Rall=0.032 abd S=2.1 for 1472 observed reflections. The essentially planar complex anions form diade of interplanar distances of 3.41 Å and their diads are stacked along aaxis with interplanar separation of 3.44 Å.

• Korean Journal of Crystallography
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• v.13 no.1
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• pp.21-24
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• 2002

The crystal structure of cholesteryl crotonate was investigated by X-ray diffraction. Crystallo-graphic data for the title compound: P2₁, a = 13.446(4) , b = 11.802(3) , c = 18.782(5) , β = 103.99(2)°, Z = 4. Reflections were collected with an Enraf-Nonius CAD-4 diffractometer equipped with a graphite monochromator. The structure was solved by direct methods and refined by least-squares analyses. The final R value was 0.092 for 1604 reflections. The cholesterol fragment of the title compound were in good agreement with those for related cholesterol derivatives. The molecules were stacked in clearly separated layers. At the center of the layers, there were cholesterol-cholesteryl interactions between the symmetry-related A molecules and the cholesteryl-C(17) side chain of B molecules. There were also interactions between the C(17) side chain of A molecules and the crotonate chains off and B molecules in the interface region between layers. The crystal structure of the title compound turned out to be isostructural with those of cholesteryl ethylcarbonate, cholesteryl propylcarbonate, and cholesterol crotylcarbonate. The crystals show the liquid crystalline state having the cholesteric phase.

• Korean Journal of Crystallography
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• v.7 no.2
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• pp.126-132
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• 1996

Cholesteryl isopropyl carbonate(C31O3H52) is orthorhombic, space group P212121, a=6.266(4), b=10.836(5), c=47.364(20)Å, Z=4, Dc=0.98 g/cm3 and Dm=1.01 g/cm3. The intensity data were collected on a Nonius CAD-4 diffractometer with a graphite-monochromatized MoKα radiation to a maximum 2θ value of 40°. The structure are solved by direct methods and refined by Fourier and full matrix least-squares methods. The present R factor was 0.22 for 1513 observed reflections. The further refinements are in progress. Compared with other cholesterol derivatives, the cholesteryl ring and tail region of the molecule are normal. The molecular long axes are parellel to the c-axis. There are close packings of cholesterol groups and loose packings of isopropyl carbonate chains forming monolayers.

• Journal of the Korean Chemical Society
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• v.19 no.2
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• pp.85-91
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• 1975

The crystal structure of piperidinothiosemicarbazide, $C_6H_{13}N_3S$, has been determined by single crystal X-ray analysis. The space group is P21/c with four molecules in the unit cell of dimensions $a=14.68{\pm}0.04,\;b=4.59{\pm}0.02,\;c=12.92{\pm}0.04{\AA}\;and\;{\beta}=109.4{\pm}0.2^{\circ}$. Three-dimensional photographic intensities were estimated visually. The structure has been solved by an interpretation of a Patterson synthesis and refined by block-diagonal least-squares methods to give a final R value of 0.14 for 378 observed independent reflections. There are two independent hydrogen bonds in the structure. One of them is of the type N-H${\ldots}$S with the length 3.28 and $3.39{\AA}$, and another is of the type N-H${\ldots}$N with the length $3.03{\AA}$. Apart from the hydrogen bonding system the molecules are held together in the crystal by van der Waals forces.

• Journal of the Korean Chemical Society
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• v.34 no.1
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• pp.29-36
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• 1990

Cholesteryl pentyl carbonate $(C_{33}H_{56}O_3)$ is monoclinic, space group P21, with a = 12.484(3), b = 9.043(3), c = 14.053(3)$\AA$, ${\beta} = 94.12(2)^{\circ}$ and z = 2. The intensity data were measured for the 2969 reflections within sin $\theta/\lambda = 0.52 {\AA}^{-1}$, using an automatic four--circle diffractometer and graphite monochromated Mo-K$\alpha$ radiation. The atomic coordinates from cholesteryl octanoate were used in an initial trial structure and the structure was refined by full-matrix least squares methods. The final R-factor was 0.12 for 1164 observed reflections. The pentyl group has shortened bond lengths due to the high thermal vibrations in this region. Adjacent molecules are related by $2_1$ screw axis so that they are arranged in an antiparallel array, corresponding to the Monolayer Type II packing mode. There are close packings of cholesteryl groups within the monolayers. This packing type is similar to those of cholesteryl hexanoate, octanoate, hexyl carbonate and oleate.

• Journal of the Korean Chemical Society
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• v.25 no.6
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• pp.343-350
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• 1981

The crystal and molecular structure of P-aminobenzaldehyde cyclohexylthiosemicarbazone, C14H20N4S, has been determined from 2712 integrated intensities measured on a computer controlled four circle diffractometer with monochromated $CuK_{\alpha}$, X-ray radiation. The crystals are monoclinic, space group C2/c with eight molecules in a unit cell of dimensions, a = 12.488(2), b = 12.276(4), c = 19.997(6)${\AA}$ and ${\beta}=103.55(3)^{\circ}$. The structure was solved by Patterson and Fourier method and refined by a full-matrix least squares method to a final R value of 0.058 for all reflections. The C(8)-S bond is trans to N(2)-N(3) and C(8)-N(1) is cis to N(2)-N(3) bond. The cyclohexane ring has chair conformation and makes an angle of $40.7^{\circ}$ with the benzene ring. The molecules are linked by N(2)H…S hydrogen bonds into dimer-like units which are held together by $N-H{\ldots}N$ hydrogen bonds. Sulfur accepts second rather weak hydrogen bond from N(4). An intramolecular hydrogen bond exists between N(1) and N(3) atoms.

• Journal of the Korean Chemical Society
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• v.34 no.6
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• pp.517-526
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• 1990

The crystal structures of two alditol acetates, D-glucitol hexaacetate and xylitol pentaacetate, have been determined by diffraction methods with Mo-K$\alpha$radiation, using direct methods for phase determinations. The crystal data are: for D-glucitol hexaacetate, P2$_1$, with a = 10.275 (2), b = 8.363 (1), c = 12.560 (5) $\AA;\beta$ = 95.97 $(2)^{\circ}$, Z = 2; for xylitol pentaacetate, P2$_1$/C with a = 18.126 (1), b = 11.422 (2), c = 8.649 (1) $\AA$, $\beta = 95.03 (1)^{\circ}$, Z = 4. Both molecules have extended zigzag carbon chain conformations which differ from previous studies of the structures of D-glucitol and xylitol and also differ from NMR studies on alditol acetates. The bond lengths and angles are normal, with mean values over both structures of C($sp^3)-C(sp^3): 1.514 (10),\; C(sp^3)-O: 1.444 (6),\; C(sp^2)-O: 1.347 (9),\; C(sp^2)=O: 1.197 (6),\; C(sp^2)-C(sp^3): 1.479(9){\AA},\; C(sp^3)-C(sp^3)-C(sp^3): 114.6 (17),\; O-C(sp^3)-C(sp^3): 109.4 (23),\; C(sp^2)-O-C(sp^3): 117.4 (6),\; O=C(sp^2)-O: 122.6 (6),\; C(sp^3)-C(sp^2)-O: 111.8 (7),\; C(sp^3)-C(sp^2)=O: 125.5 (4)^{\circ}$. The atoms of acetate groups are in coplanar. There are no particularly short intermolecular contacts and the molecules are held together by van der Waals force only.