Crystal structure of tetracarbonyl(2,2'-dipyridylamine)tungsten.

Tetracarbonyl(2,2'-dipyridylamine)tungsten was prepared from W(CO)6 and 2,2'-dipyridylamine in toluene. The structure was determined by an X-ray diffraction analysis. Crystal data: triclinic; space group, P-1 (No.2); a = 8.454(1)A, b = 13.369(2)A, c = 6.9452(9) A, a= 85.88(1) degrees, beta = 68.28(1) degrees, gamma = 80.93(1) degrees, V= 720.0(1)AI; Z = 2.     

Synthesis of 3-(4-chlorophenyl)oxirane-2,2-dicarboxamide

Oxidation of (E)-3-(4-chlorophenyl)-2-cyanoprop-2-enethioamide with hydrogen peroxide or the H₂O₂-KOH system gave 3-(4-chlorophenyl)oxirane-2,2-dicarboxamide. This compound was also obtained by an independent “one pot” synthesis from p-chlorobenzaldehyde and 2-cyanoacetamide through in situ oxidation of their adduct (E)-3-(4-chlorophenyl)-2-cyanoprop-2-eneamide with the H₂O₂-KOH system. The structure of 3-(4-chlorophenyl)oxirane-2,2-dicarboxamide was confirmed by X-ray diffraction and spectroscopic data. Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 7, pp. 1417–1419, July, 2007.     

The crystal structure of 1-(4-chlorophenyl)-3-(4-methylbenzoyl)thiourea

1-(4-Chlorophenyl)-3-(4-methylbenzoyl)thiourea was synthesized and characterized by IR,¹H and ¹³C NMR, mass spectroscopy and the elemental analysis. The crystal structure was confirmed from single crystal X-ray diffraction data. It crystallizes in the monoclinic space group P2₁/c with unit cell dimensions a=12.038(3), b=6.330(6), c=18.912(5) Å and β=100.32(3)°. There is a strong intramolecular hydrogen bond of the type N?H...O, with distance N1...O1=2.659(3) Å. The structure is composed of dimers related by inversion centers. The dimers are formed by intermolecular interactions of the type N?H...S with N...S separation of 3.440(2) Å. The mass fragmentation pattern has also been discussed.     

Crystal structure of N-(3-nitrocinnamoyl)-N-(2-chlorophenyl)hydroxylamine

All-Union Scientific-Research Institute of Chemical Reagents and Specially Pure Chemicals. Translated from Zhurnal Strukturnoi Khimii, Vol. 31, No. 5, pp. 161–164, September–October, 1990.     

Crystal structure of 1-(4-chlorophenyl)-3-{4-[2-(5-ethyl-pyridin-2-yl)-ethoxy]-phenyl}-propenone

The title compound C₂₄H₂₂ClNO₂ belongs to the orthorhombic system, space group Pca2₁ with a = 12.1771(10) Å, b = 4.9305(4) Å, c = 34.419(3) Å, α = β = γ = 90°, V = 2066.5(3) ų, Z = 4, D_c = 1.260 g/cm³, F(000) = 824, R = 0.0402 and wR = 0.1144, S = 1.034, T = 293 K. The compound is a chalcone with 4-chlorophenyl and [(5-ethyl-pyridin-2-yl)-ethoxy]-phenyl substituents bonded at the opposite ends of a propenone group, the biologically active region. The propenone bridge makes dihedral angles of 10.61(23)° and 62.75(22)° respectively, with 4-chlorophenyl and the [(5-ethyl-pyridin-2-yl)-ethoxy]-phenyl group.     

Crystal structure and luminescence of 2,2-difluoro-4,6-(4-methylphenyl)-1,3,2-dioxaborine

The crystal structure, luminescence properties of 2,2-difluoro-4,6-(4-methylphenyl)-1,3,2-dioxaborine (CH₃C₆H₄COCHCOC₆H₄CH₃BF₂) crystals and solutions at different concentrations are examined at T 296 K and 156 K.     

Crystallization of polyterephthalates of bis(4-hydroxy-3-chlorophenyl)-2,2-propane

Crystallization of polyterephthalates of bis(4-hydroxy-3-chlorophenyl)-2,2-propane synthesized by an acceptor–catalytic polyesterification has been investigated quantitatively. It was found that in a homogeneous medium (in solvents for the polymer) amorphous polymers are formed, while polycondensation in a heterogeneous system (in nonsolvents for the polymer) gives rise to crystalline polyarylates, their degree of crystallization being dependent on synthesis conditions. Secondary treatment of resulting polymers can result in their crystallization and amorphization. Along with molecular weight the physicomechanical properties are significantly affected by the preparation method.     

5-甲基-3-对甲苯基-2-对氯苯硫基-1H茚酮的合成及晶体结构

单质碘与三苯基膦促进的对氯苯亚磺酸钠与1,3-二对甲苯基丙炔-1-醇的自由基加成-分子内氧化碳氢键环化的多步骤串联反应,以70%的产率得到化合物5-甲基-3-对甲苯基-2-对氯苯硫基-1H-茚酮。化合物经¹H NMR、¹³C NMR、 IR和HR-MS等表征,其结构经X-射线单晶衍射分析确证。晶体属于三斜晶系,空间群P-1,晶细胞参数：a=10.7305(7)?,b=13.0234(8)?,c=14.7071(9)?,α=105.289(3)°,β=101.273(3)°,γ=98.623(3)°,V=1899.7(2)?³,Z=4, Dc=1.318 mg/m³,μ=0.320 mm^-1,F(000)=784。结构偏离因子R₁=0.0705, wR₂=0.1903,共收集到8687个独立衍射点,其中I>2σ(I)的可观测点为5542个。