Crystal structures of 2-phenyl- and 2-benzyl-5,6-dihydro-6-hydroxy-7H-1,2,4-triazolo [3,2-b] 1,3-thiazines

The examined compounds crystallize in the monoclinic space groupsP2 ₁/c (phenyl derivative,1) andP2 ₁/a (benzyl derivative,2). The unit cell parametersa, b, c (Å) and (°) were: 6.402(1), 16.506(1), 10.144(1), 97.48(1) for1 and 12.099(2), 4.612(1), 21.712(4) and 105.20(2) for2. The finalR(Rw) factors were 0.043 (0.041) and 0.121 (0.126) for1 and2, respectively. Both molecules have similar geometry of the bicyclic system with flat 1,2,4-triazole rings, sofa conformations of 1,3-thiazole ones and axial hydroxy groups. In the crystals the molecules form infinite chains (by means of O–H...N(4) hydrogen bonds), enantiomeric in1 and racemic in2.     

Crystal Structure of 3,4-Dihydro-2-methoxy-2-methyl-4-phenyl-2H,5H-pyrano[3,2-c]chromen-2-one

Crystallography Reports - A new polymorph of 3,4-dihydro-2-methoxy-2-methyl-4-phenyl-2H,5H-pyrano[3,2-c]chromen-2-one (pyranocoumarin) was studied by X-ray diffraction. The crystallographic...     

Crystal and molecular structure of dimethylpyridazino[2,3-b]benzo-1,2,4-triazine-3,4-dicarboxylate radical,C14H11N4O4

The crystal and molecular structure of dimethylpyridazino[2,3-b]benzo-1,2,4-triazine-3,4-dicarboxylate radical, C₁₄H₁₁N₄O₄, has been determined from X-ray diffractometer data by direct methods and refined by least-squares methods toR=0.040 for 590 observed reflections. Crystals of C₁₄H₁₁N₄O₄ are monoclinic:a=9.222 (7),b=15.335(10),c=9.544(2) Å,=102.18(2)),Z=4, space groupP2₁/c. Bond distances and internal angles in the ring system have average values:C-C 1.387, C-N 1.358, and N-N 1.356 Å, and C--C 121.5, C--N 120.4, C- -C 117.8, N- -N 121.4, and N- -N 119.8°, respectively. All these bonds have a partial double-bond character, consistent with an extensive conjugation within the molecule, thus giving stability to the free radical. The condensed rings are nonplanar. The carbomethoxy groups show a different slant, owing to overcrowding.     

Crystal Structure of 2-<Emphasis Type="Italic">Exo</Emphasis>-Phenyl-2,3,4,5-Tetrahydro-1,4-Epoxinafto[1,2-b]azepine

Abstract  

The title compound, C₂₀H₁₇NO, crystallizes in the orthorhombic P2₁2₁2₁ space group with unit cell parameters a = 7.6903(7) ?, b = 18.979(2) ?, c = 19.753(2) ?, with two crystallographically independent molecules in the asymmetric unit, which differ from one another in the slight rotation of the phenyl ring; this allows the formation of three internal hydrogen bonds, two of the type C–H···N and one of the type C–H···O, in one of the molecules, in contrast with only two of the type C–H···N in the other. The compound is rich in aromatic π rings and therefore the crystal packing is entirely dominated by cohesive weak C–H···π interactions among neighboring molecules producing an efficient packing with 71.2% of occupied space.     

Crystal structure of 2,3-dihydronaphto[2,3-b) [1,5] dioxepin

The X-ray single crystal structure of C₁₃H₁₂O₂ compound was determined. It crystallizes in the orthorombic space group P2₁2₁2₁ with a = 7.8847(7), b = 9.639(1), c = 13.432(2) Å, Z = 4 and V = 1020.8(3) ų. The final R converged to 0.037 for 1763 independent reflexions. The title compound forms layers parallel to (1 0 0) planes and the three dimensional cohesion of the crystal is assumed by Van der Waals interactions. The molecule consists of two six-membered rings (A and B) and a seven-membered ring (C). A and B rings are planar, whereas the C ring has a chair conformation     

Crystal structure of enantiomeric 3-amino-6,7-dihydro-6-hydroxy-5H-1,2,4-triazolo [3,4-b] 1,3-thiazine

The crystals of C₅H₈N₄OS are orthorhombic, space group P2₁2₁2₁ (Z=4),a=5.601(1),b=10.224(3), andc=12.233(2) Å. 1,2,4-Triazole ring is approximately planar while 1,3-thiazine ring adopts a C(5)-sofa conformation flattened at the N–C–S end with axial hydroxy group at the opposite side of the ring. The three intermolecular hydrogen bonds, N(3)...O(8), N(3)...N(2), and O(8)...N(1) form a three-dimensional hydrogen bonds network in the crystal. The structure is the first 5H-1,2,4-triazolo [3,4-b] 1,3-thiazine reported in the literature. It shows less aromatic character and smaller delocalization of electrons of the triazole ring than those in known analogs with [5,1-b] junction.     

Crystal structure of a furo-[3,2-g]-[1]-benzopyran-7-one derivative

The crystal structure of 9–(1,1-dimethyl–2-propenyl)-4-hydroxy-7H-Furo-[3,2-g]-benzopyran-7-one has been determined from X-ray diffraction data. The compound crystallizes in the monoclinic space group C2/c with unit cell parameters a = 8.976(3) Å, b = 16.621(2) Å, c = 17.818(2) Å, β = 95.79(2) Å. The gross structure was determined by direct methods and refined to a final value of R = 0.053. The three ring framework of the molecule is nearly planar. The side chain attached at the atomic position C(9) possesses significant foldings and has been found inclined to the ring system of the molecule.     

Crystal structures ofcis andtrans 7-phenylcarbamoyl-7,9-diazabicyclo [4.3.0] nonan-8-thiones

C₁₄H₁₇N₃OS,M _r+275.37, CAD4F diffractometer. CuK,T+293K.cis: orthorhombic, Fdd2,a+22.166(2),b+48.948(3), andc+5.165(1)Å: finalR+0.045 for 2519 observed reflections,trans: triclinic, ,a+11.375(2),b+11.388(2),c+11.823(1)Å, =110.72(1), =89.97(1) and =93.86(2)^o; final R=0.043 for 3993 observed reflections. Structures were wolved with direct methods and refined by full-matrix least-squares with anisotropic thermal parameters for non-H-atoms. The molecules of the studied isomers have very similar conformations, except for the obvious difference in the bicyclic system junction. Similar orientations of a flexible phenylcarbamoyl substituent results from an intramolecular hydrogen bond S...H–N(carbamoyl). Generally, molecules of thetrans form are flat and those ofcis are not. The observation may be of pharmacological importance as thetrans isomer is a far more potent tuberculostatic agent than thecis.     

Crystal and molecular structure of dimethylpyrazolo [1,2-a]pyrazolo[1,2-b]benzotriazole-3,4-dicarboxylate,C15H13N3O4

Crystals of dimethyl pyrazolo [1,2-a]pyrazolo[1,2-b]benzotriazole-3,4-di-carboxylate, C₁₅H₁₃N₃O₄, are triclinic:a=9.268(10),b=19.367(50),c=8.821(9) Å,=96.76(18),=115.39(10),=80.17(22)°,Z=4, space group P¯1 with two independent molecules in the asymmetric unit. The crystal and molecular structures have been determined from X-ray diffractometer data by direct methods, and refined by least-squares methods toR=0.047 for 2653 observed reflections. In a least-squares fitting procedure the two independent molecules show an almost perfect resemblance, except for the orientations of the 3-carbomethoxy groups. Their chiral structure is described asS. There is an appreciable puckering of the condensed five-membered rings. Bond distances and angles are found to be not comparable with those in the literature, and are discussed. The carbomethoxy groups of the same molecule show a different slant, owing to overcrowding. Close molecular packing is afforded by layers of molecules approximately parallel to the (001) plane.     

Ni(Ⅱ)5-溴水杨醛缩氨基甲磺酸席夫碱-邻菲咯林三元配合物的合成

本文采用Ni(Ⅱ)盐和氨基甲磺酸缩5-溴水杨醛席夫碱以及1,10-邻菲咯林(phen)在甲醇和水溶液中合成了三元配合物,通过元素分析、红外光谱对配合物进行了表征,并X射线衍射测定了其结构.结构解析表明,该标题配合物属三斜晶系,空间群P-1,晶胞参数为a=1.2868(3)nm,b=1.4536(3)nm,c=1.4705(3)nm;α=85.79(3)°,β=67.62(3)°,γ=77.21(3)°,V=2.4799(9)mm3,Z=2,Dc=1.580 g·cm-3,F(000)=1196,μ=2.521, 最终偏差因子(对Ⅰ>2σ(Ⅰ)的衍射点)R1=0.0604,ωR2=0.1446,对全部衍射点R1=0.1531,ωR2=0.1914,ω-1=[s2(Fo2)+(0.0884P)2],P=(Fo2+2Fc2)/3.     

Crystal structure and IR and electronic spectra of 3-o-tolyl-5,5-dimethyl-5,6-dihydro-1,2,4-triazolo[3,4-a]isoquinoline hemihydrate

The crystal and molecular structures of 3-o-tolyl-5,5-dimethyl-5,6-dihydro-1,2,4-triazolo[3,4-a]isoquinoline hemihydrate L · 0.5H₂O are determined. The crystal is built of the 2L · H₂O dimers, which are formed by the O-H?N hydrogen bonds between the water molecule and the nitrogen atoms in the 1-position of the L molecules. IR and electronic spectra of the compound are studied. Model quantum-chemical calculations are performed.     

Crystal Structure of 1-Phenyl-3-Methyl-5-Pyrazolone Perchlorate (ES-1)

The crystal of ES-1 belongs to the orthorhombic system, space group Pbca. Unit cell parameters were determined by least squares method and found to be: a = 16.256(8), b = 15.359(8), and c = 9.918(5) Å. The structure was solved by direct methods using the program SHELX86. The refinement was carried out using isotropic thermal parameters then followed by several cycles of anisotropic least squares to a final value of R₀ = 0.073 for 1226 observed reflections. The hydrogen atoms were located from a difference Fourier map. Torsion angles calculation showed that rings A and B are planar as expected. All the calculations were carried out on a PC-Computer at physics department, Tanta University.     

Crystal and molecular structure of 2-bromo-5,6-dihydro-6-methyl-4H,8H-pyrido [3,2,1-de]phenanthridin-8-one

Crystals of the title compound, C₁₇H₁₄BrNO, are monoclinic, with space groupP2₁/a,a = 14.314(5),b = 15.009(11),c = 6.596(3) Å, and = 102.39(3) °. Diffraction data were collected with CuK radiation to a Bragg angle of 77 °. The structure was solved by the heavy-atom method and refined to anR index of 0.059 for 2129 reflections. In agreement with NMR results, the C=O group is orientedanti to the benzene ring, and the methyl group at C(6) is axial. Unlike 1-(p-bromobenzoyl)-2-methyl-1,2,3,4-tetrahydroquinoline, the heterocyclic ring assumes a well defined half-chair conformation. Except for C(5) and the methyl group at C(6), the whole molecule is very nearly planar.     

Crystal and molecular structure of 1-chlorobenz[a]phenazine-7N-oxide

Crystals of 1-chlorobenz[a]phenazine-7N-oxide, C₁₆H₉N₂OCl, are orthorhombic,a =15·04,b = 3·91,c = 20·50 Å,Z = 4, space groupPna2₁. The crystal structure has been determined from two- and three-dimensional X-ray photographic data and refined by Fourier and least-squares methods toR = 0·095 for 715 observed reflexions. The molecule is slightly non-planar. Bond lengths and angles compare well with those of other molecules. Close molecular packing is given by layers of molecules parallel to (001) plane.We are grateful to Professor V. Riganti for assistance with the data collection.     

Synthesis and Crystal Structure of 5-Chloro-3-Methyl-1-Phenyl-1H-Pyrazole-4-Carbaldehyde

Abstract  

The title compound, 5-chloro-3-methyl-1-phenyl-1H-pyrazole-4-carbaldehyde 2, was prepared in a series of syntheses to produce new pyrazole derivatives, and its crystal structure was determined by X-ray diffraction method. The crystal belongs to monoclinic, space group P2₁/c with unit cell parameters a = 6.7637(4) ?, b = 6.8712(3) ?, c = 22.4188(10) ?, β = 93.8458(14)o, V = 1039.56(9) ?³ and Z = 4. X-Ray reveals that the aldehydic fragment is almost coplanar with the adjacent pyrazole ring, but the two ring planes are inclined at 72.8(1)o. The molecule is linked to its neighbor by two directionally specific C–H···O interactions.     

Crystal and molecular structure of 6-phenyl-13H-pyrimido [4,3-b:6,1-b] bis-benzothiazolium-12 triiodide

Crystals of the synthesized title compound (C₂₂H₁₅I₃N₂) are monoclinic. Space group P2₁/a,a=15.072(2),b=10.936(1),c=15.363(2) Å,=108.49(1)°. The structure was solved by direct methods and refined by block-matrix least-squares procedure to giveR=0.059 and Rw=0.043 for 3658 reflections above 2(I). The central hexaatomic ring is in a very flattened envelope conformation being the methylene group very little deviated from the plane defined by the other five atoms. The phenyl group is rotated 63.40° from that plane.     

Crystal and Molecular Structure of the Smectogen 1-[4-n-heptylbenzoyl]-2-[cyanoacetyl]-hydrazine

The compound 1-[4-n-heptylbenzoyl]-2-[cyanoacetyl]-hydrazine crystallizes in the triclinic space group Pl̄ with two molecules in the unit cell and the lattice parameters a = 4.702, b = 8.640, c = 20.906 Å, a = 97.50, β = 92.79, γ = 100.19°. The structure was solved by direct methods and refined by full-matrix least squares calculations to the final residual value R = 0.039.     

Crystal structure of 10-oxa-3,4 benzobicyclo [5.3.0] deca-1 (7) ene-8,9 dione,C13H10O3

The crystal and molecular structure of the title compound, C₁₃H₁₀O₃, determined by single crystal X-ray diffraction is reported. Crystals are triclinic, space groupP¯1,a=9.251(1),b=8.837(1),c=7.091(1)Å;=85.6(1)°,=108.2(1)°, =110.1(1)°;V=517(3)ų;Dx=1.38 mg m^–3, (MoK)=0.7107 Å;=0.91 mm^–1;F(000)=224. The structure was solved by direct methods and the finalR value is 0.059 (R=0.078) for 1393 independent observed relfections. In the crystal the cycloheptadienic moiety adopts an approximate twist chair conformation with a pseudo-twofold axis and presents disorder.     

二维配位聚合物[Cd(C8H7NO2)2]n 的水热合成与晶体结构

在中温水热条件下,利用醋酸镉和3-(3-吡啶基)丙烯酸反应,合成了一种新型的二维配位聚合物[Cd(C8H7NO2)2]n.对其进行了元素分析、红外光谱表征和X射线单晶衍射测定.该配位聚合物属三斜晶系,P-1空间群,晶胞参数为:a=0.5031(2)nm,b=0.8109(3)nm,c=0.9531(4)nm,α=69.411(6)°,β=80.554(6)°,γ=76.020(7)°,V=0.3519(2)nm3,Z=1,dc=1.929g/cm3,μ=1.575 mm-1,F(000)=202,R1=0.0313,wR2=0.0641.