共查询到20条相似文献,搜索用时 31 毫秒
1.
Julie F. Glister Keith Vaughan Valerio Bertolasi 《Journal of chemical crystallography》2004,34(3):175-180
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) Å3, for Z = 8. 相似文献
2.
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) Å3, for Z = 4. 相似文献
3.
Kumar Biradha Hilary Jenkins M. Brad Peori Keith Vaughan Michael J. Zaworotko 《Journal of chemical crystallography》1999,29(9):1037-1041
The crystal and molecular structure of 1,3-di-2-[(4-methoxyphenyl)-1-diazenyl]imidazolidine (1) has been determined by single crystal X-ray diffraction analysis. This novel bis-triazene assumes a close-to planar structure with the aryltriazene moieties aligned in diametrically opposed directions, unlike many other previously reported bis-triazenes, which assume a folded structure. The structure of 1 is compared with the closely related, non-cyclic bis-triazene analogue (2), and also compared with the structure of the simple mono-triazene (3). Crystal data: 1 C17H20N6O2, monoclinic, space group C2/c, a = 34.948(3), b = 5.925(5), c = 8.1225(6) Å, = 100.8420(10)°, and V = 1652.0(2) Å3, for Z = 4. 相似文献
4.
Colin Hester Russell G. Baughman Harvest Collier 《Journal of chemical crystallography》1996,26(10):695-699
The reaction between cadmium(II) chloride and 2,2'-bi-1H-imidazole (H2biim) in an acidic solution affords [Cd(H3biim)2Cl4] (H3biim=2-(2-1H-imidazolyl)-1H-imidazolium) in 63% yield. The compound crystallizes in the triclinic space groupP1, wherea=8.072(2),b=8.100(2),c=8.593(2) Å, =75.89(2), =62.94(2), =63.29(1)°,V=446.4(2) Å3, andZ=1. The central Cd atom exhibits an octahedral geometry composed of a Cl4N2 core. The Cd-N bond distance is 2.392(2) Å. Cd–Cl distances are 2.5919(9) and 2.671(1) Å. 相似文献
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I. N. Polyakova O. A. Egorova V. S. Sergienko L. Yu. Tarasova V. V. Davydov 《Crystallography Reports》2011,56(2):270-273
The crystal structure of 2-[(4-nitrophenyl)carbonyl]cyclohex-1-ene-1-yl 4-nitrobenzoate is studied (T = 173 K, R1 = 0.0354 for 2713 observed reflections). This crystal is orthorhombic, a = 7.8367(8) Å, b = 9.6082(10) Å, c = 23.856(3) Å, V = 1796.3(3) Å3, space group P212121, and Z = 4. The molecule has a folded configuration, which is stabilized by π-π interactions between its two parts. A system of intermolecular C-H...O hydrogen bonds (H...O, 2.44–2.67 Å; CHO angles 122°–169°) and intramolecular C-H...O contacts closing five-membered cycles (H...O, 2.42–2.59 Å; CHO angles 96°–102°) are formed in the structure. 相似文献
10.
Yu. M. Chumakov V. I. Tsapkov B. Ya. Antosyak L. G. Popovschi G. Bocelli A. P. Guly S. A. Palomares-Sanchez 《Crystallography Reports》2012,57(2):235-240
Nitrato-4-bromo-2-[(2-hydroxyethylimino)methyl]phenolatoimidazolecopper and nitrato-4-chloro-2-[(2-hydroxyethylimino)methyl]phenolatoimidazolecopper
were synthesized and studied by X-ray diffraction. The crystals are isostructural. The coordination polyhedron of the copper
atom can be described as a distorted square pyramid whose basal plane is formed by the phenolic and alcoholic oxygen atoms
and the nitrogen atom of the monodeprotonated tridentate azomethine molecule and the imidazole nitrogen atom. The apex of
the copper polyhedron is occupied by the oxygen atom of the nitrato group. The complexes are linked together by hydrogen bonds
with the participation of the nitrato groups to form a three-dimensional framework. 相似文献
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Luo Mei Zhang Jia Hai Yin Hao Pang Wei Min Hu Ke Liang 《Crystallography Reports》2010,55(7):1217-1219
Two oxazolines compound 1a and 1b, 2-[4(S)-4,5-dihydro-4-phenyl-2-ozazolinyl-benzenamine, and (C15H14N2O), 2-[4(S)-4,5-dihydro-4-benzyl-2-ozazolinyl-benzenamine (C16H16N2O) were obtained in moderate yield from the reactions of 2-aminobenzonitrile with optically active L-(+)-Phenylglycinol and L-(+)-Phenylalaninol, respectively, in chlorobenzene under dry, anaerobic conditions. ZnCl2 was dried under vacuum and acted as a Lewis acid catalyst in this reaction. The structures of 1a and 1b were determined by
X-ray diffraction and NMR. There exist intra- and intermolecular N-H…N hydrogen bonds in the crystal structure. 相似文献
13.
Ladd M. F. C. Larkworthy L. F. Leonard G. A. Povey D. C. Tandon S. S. 《Journal of chemical crystallography》1985,15(1):19-27
A single crystal X-ray investigation of the purple nickel (II) complex Ni[L(en)](NO3)2, produced by condensation of 1,2-diaminoethane (en) with the thiodiketone S(CH2COCH3)2 in the presence of nickel (II) nitrate (L is NH2(CH2)2N=C(CH3)CH2SCH2COCH3), shows that the metal ions are six coordinate. The new ligand L is tetradentate, with the N,N and S donor atoms arranged meridionally, and the coordination shell completed by the carbonyl oxygen atom of L and the nitrogen atoms of 1,2-diaminoethane. Metal-ligand bond distances are Ni-N: 2.08 av. (en), 2.10 and 2.05 (NH2 and N=C respectively of L); Ni-O, 2.16; Ni-S, 2.45 Å. There is considerable angular distortion from regular octahedral values of the bond angles at nickel. The crystals are monoclinic,P21/c (No. 14),a=12.433(2),b=11.709(1),c=13.150(2) Å,=103.93(1)°,V
c=1858.2(4) Å3. The structure was solved by the heavy-atom method and refined by full-matrix least squares to anR value of 0.055 for 3633 reflections. 相似文献
14.
The Crystal Structure of 1-[2-(furan-2-yl)-6-methyl-1,2,3,4-tetrahydroquinolin-4-yl]Pyrrolidin-2-one
Luis A. Vizcaya Asiloé J. Mora Gerzon E. Delgado Ali Bahsas Uriel Mora Vladimir V. Kouznetsov 《Journal of chemical crystallography》2012,42(3):267-270
Abstract
The title compound, C18H20N2O2, a potential pharmaceutical agent, crystallizes in the monoclinic P21/n space group with unit cell parameters a = 11.157 (7) ?, b = 8.776 (6) ?, c = 16.460 (11) ?, β = 103.08 (3)°. The tetrahydroquinoline ring system formed by the fusion of the benzene ring and the piperidine ring via two carbon atoms is coplanar, with the later adopting a sofa conformation. The pyrrolidine group in position 4 adopts an envelope conformation. Dimers related by inversion centers and linked by hydrogen bonds of the type N–H···O form cycles described by the graph set R22(16). Additionally, the dimers connect through weak hydrogen bonds of the type C–H···O with graph set C(10) to form chains extending along [001]. 相似文献15.
Xue-Mei Li Cheng-Chu Zeng Yi-sheng Xu Hong Yan Da-wei Zheng Ru-Gang Zhong 《Journal of chemical crystallography》2006,36(6):357-363
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. 相似文献
16.
Crystallography Reports - Crystal structure of brivanib ((R)-1-(4-(4-fluoro-2-methyl-1H-indol-5-yloxy)-5-methylpyrrolo[2,1-f][1,2,4]triazin-6-yloxy)propan-2-ol) is reported for the first time.... 相似文献
17.
Doris Pfeiffer Rolf-Günter Kretschmer Siegfried Hoffmann 《Crystal Research and Technology》1986,21(10):1321-1325
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. 相似文献
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Julie F. Glister Hilary Jenkins Keith Vaughan 《Journal of chemical crystallography》2006,36(7):445-452
1-[2-(p-Tolyl)-1-diazenyl]-3-({3-[2-(p-tolyl)-1-diazenyl]perhydrobenzo[d]imidazol-1-yl}methyl)perhydrobenzo[d]imidazole(1) has been synthesized by reactionof a mixture of 1,2-diaminocyclohexane and formaldehyde withp-toluene diazonium chloride inaqueous solution. The product has been characterized by IR and NMRspectroscopy and elemental analysis. A crystal grown from solution ina mixed solvent system of ethyl acetate and hexanes was analyzed byX-ray crystallography. The solution of the crystal structure of(1) is important in establishing theconnectivity of this molecule and other compounds of similarstructure. The crystal structure of (1) is compared with the previously reportedstructure of the p-cyano analogue(2). Compounds (1) and (2)differ principally in the relative orientation of the heterocyclicrings; in (1), the molecule has adistinct V-shape, whereas compound (2) adopts a more extended conformation.Significant conjugation within the triazene moieties is evident inboth (1) and (2), as manifested in the N465=N andN–N bond lengths. The conjugation is greater in (2) due to the extended conjugation through tothe nitrile group. The title compound (1){C29H40N8}crystallizes in the monoclinic, space group C2/c, with lattice constants: a = 30.532(6) ?,b =5.9050(12) ?, c= 15.463(3) ?, α = 90°,β = 99.94(3)°, γ = 90°,V =2746.0(10) ?3, Z = 4, D
c =1.209 mg m−3,F(000) = 1076, R
1 = 0.0785,wR
2= 0.1877. 相似文献
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