Synthesis and crystal structures of 2-amino-3-cyano-4-(2-chlorophenyl)-1,4-dihydro-2H-pyrano[3, 2-h]quinoline and 2-amino-3-cyano-4-(2-chlorophenyl)-8-(2-chlorobenzylidene)-1,4,5,6,7,8-hexahydrobenzo[b]pyran

The title compounds 2-amino-3-cyano-4-(2-chlorophenyl)-1,4-dihydro-2H-pyrano[3, 2-h]quinoline 1 (C₁₉H₁₂ClN₃O, M _r = 333.77) and 2-amino-3-cyano-4-(2-chlorophenyl)-8-(2-chlorobenzylidene)-1,4,5,6,7,8-hexahydrobenzo[b]pyran 2 were synthesized and crystallized. The crystals of compound 1 are triclinic, space group P-1, a = 7.488(2), b = 9.127(3), c = 12.252(3) Å, = 73.58(2), = 78.38(2)°, = 75.39(2), Z = 2, V = 769.5(4) ų; The compound 2 crystallizes in space group P2₁/n, with cell parameters a = 13.582(2), b = 8.974(1), c = 16.960(2) Å, = 103.34(1)° and D _calc = 1.352 g/cm^–3 for Z = 4. X-ray analysis reveals that atoms C(1)—C(5) and O form a pyran ring in compound 1, which adopts half-chair conformation. In compound 2 the atoms C(12)—C(16) and O form a pyran ring which adopts boat conformation, another six-membered ring (C(8)—C(13)) adopts a half-chair conformation. In addition, there are intermolecular hydrogen bonds in the crystal structures 1 and 2.     

Structure of 2-{2-[3-methyl-3-(2,4,6-trimethylphenyl) cyclobutyl]-2-oxoethyl}isoindole-1,3-dione

2-{2-[3-Methyl-3-(2,4,6-trimethylphenyl)cyclobutyl]-2-oxoethyl}isoindole-1,3-dione (C₂₄ H₂₅NO₃) was synthesized, and its crystal structure was determined by X-ray crystallographic techniques. The compound crystallizes in the triclinic space group P-1, with unit cell parameters: a = 14.109(9) Å, b = 14.130(8) Å, c = 12.152(6) Å, = 105.62(5)°, = 113.75(4)°, = 98.78(5)°, V = 2039.8(19) ų, D _c= 1.223 g/cm³, and Z = 4. The crystal structure has two crystallographically independent molecules, I and II. These molecules are held together by weak intermolecular C—H···O interactions, forming a continuous chain. The dihedral angles between the N-substituted phthalimide moiety and cyclobutane ring in molecules I and II are 60.37(14) and 68.18(18)°, respectively.     

Synthesis, characterization, and structural analysis of ethyl (2Z)-3-(4-chlorophenyl)-2-cyano-3-(methoxyamino)prop-2-enoate

Ethyl (2Z)-3-(4-chlorophenyl)-2-cyano-3-(methoxyamino)prop-2-enoate was prepared by reacting the lithium salt of ethyl cyanoacetate with (Z)-O-methyl-4-chloroben-zohydroximoyl fluoride. This compound crystallizes in space group Pbca,with lattice constants a=7.5740(15) ?, b=11.337(2) ?, and c=30.424(5) ? at 110 K. Characterizations include spectrometric identifications employing IR, UV, and ¹H and ¹³C NMR. The compound exists in the solid as the enamine tautomer, with the cyano group cis to the 4-chlorophenyl group (the Z configuration). The C=C and C–N bond distances are 1.3930(16) ? and 1.3278(16) ?, respectively. The N–H group forms a bifurcated hydrogen bond with acceptors C=O (intramolecular) and C≡N (intermolecular).Supplementary material CCDC-289444 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge via www.ccdc.cam.ac.uk/data_request/cif, by e-mailing data_request@ccdc.cam.ac.uk, or by contacting The Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; Fax: +44(0)1223-336033.     

Crystal structure of 1-(2-hydroxyphenyl)-3-(2-thiomethoxyphenyl)-1,3-propanedione,C16H14O3S

The crystal structure of the enol tautomer of 1-(2-hydroxphenyl)-3-(2-thiomethoxyphenyl)-1,3-propanedione C₁₆H₁₄O₃S, was determined from X-ray crystallography. The finalR value was 5.99% based on 1945 unique observed reflections. The crystals are monoclinic,P2₁/c, witha=7.406(6),b=8.585(6),c=21.992(4) Å,=93.42(2),D _c =1.36 g cm^–3 forz=4. The compound is present in the solid state as a unique enol tautomer.There are two short, intramolecular OO contacts of 2.553(4) and 2.577(4) Å. Both the phenol and the enol H atoms are asymmetrically located with respect to the O atoms.     

Crystal Structures of 2-Chloro-3-((3-(trifluoromethyl)phenyl)amino)naphthalene-1,4-dione and 2-Chloro-3-((4-(trifluoromethyl)phenyl)amino)naphthalene-1,4-dione

Crystallography Reports - 2-Chloro-3-((3-(trifluoromethyl)phenyl)amino)naphthalene-1,4-dione (1) and 2-chloro-3-((4-(trifluoromethyl)phenyl)amino)naphthalene-1,4-dione (2) were obtained according...     

Synthesis and Molecular Structure of 2-(4-Chlorophenyl)-3-(phenyl-amino)-5-(thiophen-2-ylmethylidene)-3,5-dihydro-4H-imidazol-4-one

Crystallography Reports - 2-(4-Chlorophenyl)-3-(phenylamino)-5-(thiophen-2-ylmethylidene)-3,5-dihydro-4H-imidazol-4-one, C20H14N3OSCl was synthesized and its crystal structure was determined by...     

Structures of 2-, 3-, and 4-methyl-9-oxothioxanthenes

The structures of 2-, 3-, and 4-methyl-9-oxothioxanthenes (2-, 3-, and 4-TX, respectively) were determined by single crystal x-ray methods. The molecules are folded by 2–3° about their SC=O lines. Bond distances and angles vary only slightly as a function of the methyl substitution position, and reveal no inherent structural reason for the long-range nmr couplings observed between the ring and methyl protons. The molecular packings exhibit interesting similarities as well as subtle differences that result from variation of the methyl position. Crystals of 2-TX are orthorhombic, space groupPn2₁ a,a=10.807(1),b=4.024(2),c=24.827(3) Å,Z=4,R=0.059 for 715 observed reflections. Crystals of 3-TX are orthorhombic, space groupPbc2₁,a=3.999(1),b=25.051(2),c=10.758(1)Å,Z=4,R=0.041 for 1382 observed reflections. Crystals of 4-TX are triclinic, space groupP¯1,a=7.118(1),b=7.907(2),c=10.415(2) Å,=77.74(1),=74.35(1), =73.96(1)°,Z=2,R=0.043 for 1542 observed reflections.Deceased.     

Crystal structures of difluoro[2-(4-methoxyphenyl)-3-oxo-3-phenylpropanalato]boron(III), [BF2(C16H13O3)], and bis[2-(4-methoxyphenyl)-3-oxo-3-phenylpropanalato]copper(II), [Cu(C16H13O3)2]

The crystal structures of difluoro[2-(4-methoxyphenyl)-3-oxo-3-phenylpropanalato]boron(III), [BF₂(C₁₆H₁₃O₃)], and bis[2-(4-methoxyphenyl)-3-oxo-3-phenylpropanalato]copper(II), [Cu(C₁₆H₁₃O₃)₂], have been determined by single-crystal X-ray diffraction methods. The structures were solved by direct methods and electron density calculations and were refined by the full-matrix least-squares method. Difluoro[2-(4-methoxyphenyl)-3-oxo-3-phenylpropanalato]-boron(III) crystallizes as yellow rhombs in the monoclinic space groupP2₁/c witha=11.429(3),b=11.364(4),c=11.412(4) Å,=92.19(2)°,V=1481.0(8) ų andZ=4. A total of 2754 unique reflections were collected. Of these 1342 were considered observed [I>3(I)] leading to a finalR-value of 0.045. Boron is tetrahedrally coordinated to the two fluorine atoms and to two oxygen atoms of the bidentate 2-(4-methoxyphenyl)-3-oxo-3-phenylpropanalato ligand, C₁₆H₁₃O ₃ ^– . Average bond distances: C-C (aromatic) 1.378(10) Å, B-O 1.473(7) Å and B-F 1.343(4) Å. bis[2-(4-Methoxyphenyl)-3-oxo-3-phenylpropanalato]copper(II) crystallizes as dark yellow-green plates in the monoclinic space groupC2/c witha=23.410(7),b=13.856(3),c=8.039(3) Å,=101.79(2)°,V=2553(1) ų andZ=4. Of the unique set of 3076 scanned reflections 2401 hadI>3(I) for whichR became 0.040. Copper is coordinated to four oxygen atoms, two from each of the two bidentate 2-(4-methoxyphenyl)-3-oxo-3-phenylpropanalato ligands, in a distorted square planar manner. The molecule hasC ₂ symmetry. Average bond distances: C-C (aromatic) 1.383(6) Å and Cu-O 1.896(8) Å. The crystals of both compounds consist of monomeric molecular complexes held together by van der Waals forces.     

The Crystal Structure of a RAS (N–CH3-2-NH2-5-Cl–Py)(TCNQ)(CH3CN) Solvate

Crystallography Reports - The structure of the radical anion salt (RAS) of 7,7,8,8-tetracyanedimethane (TCNQ) with a cation based on 2-amin-5-chloro-pyridine (2-NH2-5-Cl–Py, Am), that is,...     

X-Ray crystal structure determination of a series of 1-aryl- 2-[3-(3-[2-aryl-1-diazenyl]-1,3-diazepan-1-ylmethyl)-1, 3-diazepan-1-yl]-1-diazenes obtained from the reaction of diazonium salts with mixtures of formaldehyde and 1,4-diaminobutane

A new series of bis-triazenes, the 1-aryl-2-[3-(3-[2-aryl-1-diazenyl]-1,3-diazepan-1-ylmethyl)-1,3-diazepan-1-yl]-1-diazenes has been synthesized from the reaction of diazonium salts with a mixture of 1,4-diaminobutane and formaldehyde. The structures of 1-(p-bromophenyl)-2-[3-{3-[2-(p-bromophenyl)-1-diazenyl]-1,3-diazepan-1-ylmethyl}-1,3-diazepan-1-yl]-1-diazene(1), 1-(p-cyanophenyl)-2-[3-{3-[2-(p-cyanophenyl)-1-diazenyl]-1,3-di azepan-1-ylmethyl}-1,3-diazepan-1-yl]-1-diazene(2), and 1-(p-methoxyphenyl)-2-[3-{3-[2-(p-methoxy-phenyl)-1-diazenyl]-1,3-diazepan-1-ylmethyl}-1,3-diazepan-1-yl]-1 diazene(3) have been unequivocally determined by X-ray crystallography. The new bis-triazenes are important since the structure contains the novel saturated heterocycle, 1,3-diazepane. The general conclusion of this study is that alkanediamines with 3 or 4 carbon atoms in the spacer link between the nitrogen atoms give rise to the linear bicyclic molecules of type 5, in contrast to the case of ethylenediamine (spacer link 2 carbon atoms), which affords molecules of type 6, which exemplify the general cage structure of type 4. The crystal structures of 1, 2 and 3 are compared with the previously reported structure of the hexahydropyrimidine analogue 8a(X=CN); compounds 2 and 8a(X=CN) are homologous with respect to the alkane spacer moiety. The structures of 2 and 8a(X=CN) are very different in one respect; in 2 the aryldiazenyl-1,3-diazepanyl groups are in the s-trans orientation around the central methylene group whereas in 8a(X=CN) the arrangement of the aryldiazenyl-hexahydropyrimidinyl groups is the s-cis orientation.Crystal data: 1 C₂₃H₃₀N₈Br₂, triclinic, space group P-1, a=8.3979(2), b=10.7828(3), c=14.4692(5) ?, α=83.670(1), β=78.662(1), γ=78.758(1)°, V=1256.48(6) ?³, for Z=2. 2 C₂₅H₃₀N₁₀, monoclinic, space group P2 ₁ /n, a=13.4046(6), b=9.4482(4), c=10.6913(4)?, β=103.239(2)°, V=2490.5(2) ?³, for Z=4. 3 C₂₅H₃₆N₈O₂, triclinic, space group P-1, a=8.5223(3), b=10.6913(4), c=14.4034(7)?, α=85.657(2), β=78.731(2), γ=80.153(1)°, V=1266.88(9) ?³, for Z=2.     

Design of molecules and noncentrosymmetric crystals of 3-(4-nitrophenyl)-2-phenylacrylic acid derivatives

The derivatives of 3-(4-nitrophenyl)-2-phenylacrylic acid are synthesized. It is shown that the chemical modification of this acid results in a change in the symmetry of the supramolecular fragment formed by molecules in the crystal. In turn, this change leads to a change in the crystal symmetry and favors the formation of a noncentrosymmetric crystal structure. The crystal structures of 3-(4-nitrophenyl)-2-phenylacrylic acid (I), 3-(4-nitrophenyl)-2-phenyl-triethyl aminoacrylate (II), and 3-(4-nitrophenyl)-2-phenylacrylic acid (3-methoxy)phenyl ester (III) are investigated by X-ray diffraction.     

Methyl 4-((E)-2-{3-[(3-{ (E)-2-[4-(methoxycarbonyl)phenyl]- 1-diazenyl}-5,5-dimethylhexahydro-1-pyrimidinyl)methyl]-5,5-dimethylhexahydro-1-pyrimidinyl-1-diazenyl) benzoate. X-ray crystal structure

Methyl 4-((E)-2-{3-[(3-{(E)-2-[4-(methoxycarbonyl)phenyl]-1-diazenyl}-5, 5-dimethyl hexahydro-1-pyrimidinyl)methyl]-5, 5- dimethylhexahydro-1- pyrimidinyl}-1- diazenyl) benzoate (1) has been synthesized by reaction of a mixture of formaldehyde and 2,2-dimethyl-1,3-propanediamine with p-methoxycarbonylbenzenediazonium chloride. The crystal structure of 1 has been determined by single crystal X-ray diffraction analysis. The crystals of 1 displayed problems of disorder; the asymmetric unit is built up by two independent molecules, which display disorder within a methoxycarbonyl group. The two independent molecules in the asymmetric unit are very similar, differing only slightly about the mutual orientation of the aryltriazenyl groups. With respect to the N–C–N bridge between the hexahydropyrimidinyl rings, the two equivalent fragments containing the triazene moieties are in a cis orientation. The N–N single bonds, in the range 1.319(4)–1.348(4) Å, and the N=N double bonds, in the range 1.255(5)–1.275(4) Å, indicate significant conjugations within the triazene moieties. All the hexahydropyrimidine six-membered rings adopt a chair conformation as shown by their puckering parameters. The crystal packing is determined only by simple van der Waals interactions. The crystal structure of 1 is compared with the previously reported structure of the unbranched hexahydropyrimidine analogue 2. Crystal data: 1 C29H40N8O4, triclinic, space group P-1, a = 13.9652(2), b = 14.2908(3), c = 16.6129(4) Å, = 97.279(1), = 90.872(1), = 107.385(1), V = 3133.6(1) ų, for Z = 4.     

Synthesis and crystal structure of 3-[2-oxo-2-(4-methyloxyphenylsulfonamidophenyl)ethylidene]-3,4-dihydro-1H-quinoxalin-2-one

3-[2-Oxo-2-(4-methyloxyphenylsulfonamidophenyl)ethylidene]-3,4-dihydro-1H-quinox-alin-2-one (4) was synthesized and characterized by ¹H NMR,¹³C NMR, IR, and single-crystal X-ray diffraction techniques. The crystallographic results show that the composition of the title compound is C₂₃H₁₉N₃O₅S. It belongs to triclinic crystal system and P-1 space group, with a=7.273(6) ?, b=9.092(7) ?, c=15.928(13) ?; α=85.135(11)°, β=78.297(10)°, γ=84.619(11)°, V=1024.4(14) ?³, Z=2, D _c=1.457 mg/m³, μ = 0.201 mm⁻¹, F(000)=468, R=0.0597, wR=0.1438. Supplementary material CCDC-281953 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge at www.ccdc.cam.ac.uk/retrieving.html or from the Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44-1223-336033; e-mail: deposit@ccdc.cam.ac.uk.     

ε-(AlxGa1-x)2O3/ε-Ga2O3异质结电子输运性质研究

Ga₂O₃是一种新兴的宽带隙半导体,在电力和射频电子系统中具有潜在的应用前景。前期研究以β-Ga₂O₃为主,并且已经对β-(Al_xGa_1-x)₂O₃/Ga₂O₃异质结构中的二维电子气(2DEG)进行了理论计算,本文主要研究ε-(Al_xGa_1-x)₂O₃作为势垒层对ε-(Al_xGa_1-x)₂O₃/ε-Ga₂O₃异质结电子输运性质的影响,首先介绍了ε-(Al_xGa_1-x)₂O₃/ε-Ga₂O₃异质结的结构和性质,分析计算了由于ε-(Al_xGa_1-x)₂O₃/ε-Ga₂O₃异质结的自发极化和压电极化所产生的极化面电荷密度,以及极化对2DEG浓度产生的影响,接着分析了在不同Al摩尔组分下,ε-(Al_xGa_1-x)₂O₃势垒层厚度与合金无序散射、界面粗糙度散射和极性光学声子散射之间的关系。最后通过计算得出结论:界面粗糙度散射和极性光学声子散射对ε-(Al_xGa_1-x)₂O₃/ε-Ga₂O₃异质结的电子输运性质有重要影响,合金无序散射对异质结的输运性质影响较小;2DEG浓度、合金无序散射、界面粗糙度散射和极性光学声子散射的电子迁移率强弱由ε-(Al_xGa_1-x)₂O₃势垒层的厚度和Al摩尔组分共同决定。     

4-(E)-2-[3-(3-[(E)-2-(4-cyanophenyl)-1-diazenyl]perhydrobenzo[d]imidazol-1-ylmethyl)perhydrobenzo[d]imidazol-1-yl]-1-diazenylbenzonitrile: X-ray crystal structure

4-(E)-2-[3-(3-[(E)-2-(4-Cyanophenyl)-1-diazenyl]perhydrobenzo[d]imidazol-1-ylmethyl) perhydrobenzo[d]imidazol-1-yl]-1-diazenylbenzonitrile (1) has been synthesized by reac- tion of p-cyanobenzene diazonium chloride with a mixture of formaldehyde and trans-1,2-cyclohexanediamine. The crystal structure has been determined by single crystal X-ray diffraction analysis. The bis-triazene (1) does not adopt a folded conformation, unlike previously studied ethylenediamine analogues, and there is no indication of -stacking in the crystal packing. The dominant interaction between molecules is the van der Waal's attraction between cyclohexane rings. This result establishes the structure of the product of this diazonium coupling reaction as the 1-(1-imidazolidinylmethyl)imidazolidine derivative and not the alternate tetraazabicyclo[4.4.1]undecane derivative. Crystal data: 1 C₂₉H₃₄N₁₀, orthorhombic, space group Pbca, a = 17.946(1), b = 13.106(1), c = 24.108(1) Å, V = 5670.6(3) ų, for Z = 8.     

Bis[3-(2-pyridyl)-2-thienyl]di-p-tolylstannane,an example of a six-coordinate tetraorganotin compound

The tin atom is bis[3-(2-pyridyl)-2-thienyl]di-p-tolylstannane is six-coordinate in a distortedcis-octahedral geometry owing to coordination by the pyridyl nitrogen atoms (Sn< –N=2.620(5), 2.631(5)Å).     

Crystal structure of the molecular complex of 3-[1-(4-nitrophenyl)-3-oxobutyl]-4-hydroxychromen-2-one with ethanol

The crystal structure of 2,3H-2-methyl-4-(4-nitrophenyl)-5-oxobenzopyrano[3,4-e]dihydropyran-2-ol is investigated using X-ray diffraction. The unit cell contains an ethanol molecule that forms hydrogen bonds with O-H and C-O groups of two molecules of the main compound and acts as a proton donor and a proton acceptor in these hydrogen bonds. Owing to these interactions, infinite chains are formed in the crystal. The crystallographic data for the structure of C₁₉H₁₅NO₆·C₂H₅OH (M = 399.39) are as follows: the crystals are triclinic, space group P1, a = 5.5340(3) Å, b = 8.0109(4) Å, c = 11.0112(5) Å, α = 88.773(2)°, β = 84.788(2)°, γ = 79.958(2)°, and Z = 1.     

Synthesis and Crystal Structure of bis [2-(3-(2-((2-Hydroxybenzylidene) Amino)Ethyl)Oxazolidin-2-yl)Phenol]Cerium (IV) 1,4-Dioxane Monosolvate

The metal complex, bis [2-(3-(2-((2-hydroxybenzylidene)amino)ethyl) oxazolidin-2-yl)phenol]cerium(IV) 1,4-dioxane monosolvate was synthesized and characterized by infrared, ¹H NMR, elemental analysis, single-crystal, and powder X-ray diffraction. The coordination polyhedra of cerium shows a distorted square-antiprismatic geometry. No classical hydrogen bonds were observed. The crystal packing was influenced by weak C-H···O (intermolecular) and van der Waals interactions.     

Synthesis,Crystal Structure,and DNA Binding Studies of the 3-(2-(2-Hydroxybenzylidene)Hydrazinyl)Quinoxalin-2(1H)-One

Crystallography Reports - The Schiff base, 3-(2-(2-hydroxybenzylidene)hydrazinyl)quinoxalin-2(1H)-one has been synthesized by condensation of 3-hydrazinyl quinoxalin-2(1H)-one and salicylaldehyde...     

Molecular and crystal structures of 2-amino-5-benzoyl-4-(2-nitrophenyl)-3-cyano-4,5-dihydrothiophene

The crystal structure of 2-amino-5-benzoyl-4-(2-nitrophenyl)-3-cyano-4,5-dihydrothiophene is determined by X-ray diffraction analysis. The unit cell parameters are as follows: a = 10.878(2) Å, b = 12.890(3) Å, c = 13.539(4) Å, α = 108.15(2)°, β = 99.26(2)°, γ = 107.13(2)°, V = 1656(2) ų, d _calcd = 1.410 g/cm³, Z = 4, and space group P1ˉ. The molecules occupy two systems of independent positions in the crystal. Similar to the compounds studied earlier in this series, the o-nitrophenyl substituent has a synperiplanar orientation relative to the hydrogen atom at the C(4) atom of the heterocycle. __________ Translated from Kristallografiya, Vol. 45, No. 2, 2000, pp. 282–285. Original Russian Text Copyright ? 2000 by Nesterov, Kuleshova, Samet, Shestopalov.