• 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.36 no.6
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• pp.812-817
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• 1992

Fluorometholone $(C_{22}H_{29}FO_4)$, M.W. = 376.5, monoclinic, $P2_1$, a = 6.410(4), b = 13.431(3), c = 10.996(3)$\AA$, $\beta$ = 92.81$(3)^{\circ}$, Z = 2, F(000) = 404, T = 292K, $\lambda$(Mo-$K_\alpha$) = 0.7107$\AA$, $\mu$ = 0.57$cm^{-1}$, $D_c$ = 1.32 $g/cm^3$, $D_m$ = 1.31 $g/cm^3$ and final R = 0.032 for 1769 observed reflections. All bond lengths and angles are within normal limits. Ring A is almost planar, B ring has a highly symmetrical chair conformation and C ring is in a distorted chair conformation. Ring D is in a intermediate conformation between 13$\alpha$-14$\beta$-half-chair and 13$\alpha$-envelope. Torsion angle C(16)-C(17)-C(20)-O(20) of $-7.9^{\circ}$ is a lower value than those of $-31.9^{\circ}$ and $-16.5^{\circ}$ for 9-fluoro-6-methylprednisolone I and II respectively.

• 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.

• Journal of the Korean Chemical Society
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• v.37 no.3
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• pp.344-350
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• 1993

25,26,27,28-Tetraacetoxycalix[4]arene·monohydrate is orthorhombic, space group Pbca with a = 14.979(4), b = 15.154(4), c = 27.890(3) ${\AA}$, Z = 8, V = 6330.6 ${\AA}^{-3}$, D$_c$ = 1.28 $g{\cdot}cm^{-3}$, (Mo K${\alpha}$) = 0.71069 ${\AA}$, ${\mu}$ = 0.86 cm$^{-1}$, F(000) = 2600, and R = 0.069 for 3376 unique observed reflections with I > 1.0 ${\sigma}$(I). The structure was solved by direct methods and refined by cascade diagonal least-squares refinement. All the C-H bond lengths(= 0.96 ${\AA}$), the methyl groups and the methylene groups are fixed and refined as the rigid groups with ideal geometry. The macrocycle exists in the 1,3 alternate conformation (by Conforth) making the angles of 110.7, 684, 113.7 and 68.8$^{\circ}$ between the benzene rings and the methylenic mean plane, and four each acetoxy groups are twisted away from their own benzene rings with the angles of 68.2, 97.6, 78.9 and 71.3$^{\circ}$, respectively. The relative dihedral angles between two opposite side of the benzene rings are 135.6$^{\circ}$ for the rings (1) and (3) and 135.2$^{\circ}$ for (2) and (4). A water molecule which has nearly the same height of the methylenic plane of the macrocycle in the c-axis, is located within the distances of 2.942(5) ${\AA}$ from the O(8) atom of the carbonyl group and 2.901 ${\AA}$ from, another O(2)(1/2-x, -1/2＋y, z). The shortest contact between the molecule is 3.193 ${\AA}$ from the O(4) to the C(3)(1/2＋x, 1/2-y,-z).