共查询到20条相似文献,搜索用时 15 毫秒
1.
Arzu Özek Çiğdem Albayrak Mustafa Odabaşoğlu Orhan Büyükgüngör 《Journal of chemical crystallography》2009,39(5):353-357
Abstract The crystal structure of C14H12ClNO2 was determined by X-ray analysis. It crystallizes in the triclinic space group Pc with a = 12.5346(10) ?, b = 4.5101(3) ?, c = 12.0534(11) ?, α = 90.00o, β = 113.669(6)o, γ = 90.00o, Z = 2, Dx = 1.393 mg/m3, μ (MoKα) = 0.298 mm−1. The title compound is photochromic and molecule is non-planar. It adopts a phenol–imine tautomeric form with a strong intramolecular
O–H···N hydrogen bond and a strong intermolecular C–H···O hydrogen bond. Minimum energy conformations AM1 were calculated
as a function of the three torsion angles θ1(C10–C9–N1–C8), θ2(C9–N1–C8–C1) and θ3(N1–C8–C1–C6), varied every 10°. As in the X-ray experiment results, molecule has an angle that makes it non-planar between
two aromatic rings in AM1 optimized geometry.
Graphical Abstract Molecular and crystal structure of [(E)-2-[(3-chlorophenylimino)methy])-4-methoxyphenol], C14H12ClNO2, have been determined by single crystal X-ray diffraction study, and conformational analysis of the title molecule with respect
to the selected torsion angle has been achieved by AM1 semi-empirical calculations.
相似文献
2.
Hande Petek Çiğdem Albayrak Nazan Ocak İskeleli Erbil Ağar İsmet Şenel 《Journal of chemical crystallography》2007,37(4):285-290
The single crystal X-ray diffraction analysis of the title compound, C14H20N2O3, reveals that the structure is adapted to its zwitterionic form and centrosymmetric dimers are formed by N+–H···O− type ionic weak hydrogen bonds in the crystal structure. The title compound crystallizes in the triclinic space group P−1 with a = 5.9255(13) ?, b = 9.853(3) ?, c = 12.248(3) ?, α = 101.793(19)°, β = 94.941(17)°, γ = 104.36(2)°, Z = 2, Dx = 1.308 g/cm3, μ (Mo-Kα) = 0.092 mm−1. The structure was solved by direct methods and refined to a final R = 0.0371 for 2183 reflections with I > 2σ (I). The crystal structure is stabilized by N+–H···O− type intra-molecular hydrogen bonds and N+–H···O− type packing interactions referred to as weak hydrogen bonds. To elucidate conformational flexibility of the title molecule,
the selected torsion angle is varied from −180° to +180° in every 10° separately and then molecular energy profile is calculated
and construed. In addition, charge-population analysis of the crystallographically observed structure confirms its zwitterionic
form. 相似文献
3.
Qiu Li-Hua Zhou Wei-Qun Shen Zong-Xuan Zhang Ya-Wen 《Journal of chemical crystallography》2007,37(3):181-186
The title compound (C23H30N2O), a chiral ligand, has been successfully synthesized from a natural proline. FTIR spectrum has been discussed. DFT (B3LYP)
method has been used to determine the structure. With the basis set of the 6–311G* quality, the DFT calculated bond parameters and harmonic vibrations are predicted in very good agreement with experimental
data.
相似文献
Zhou Wei-QunEmail: |
4.
Vanessa Renee Little Valerio Bertolasi Keith Vaughan 《Journal of chemical crystallography》2010,40(10):807-811
Abstract
The crystal structure of methyl 1,4-di[(E)-2-(p-tolyl)-1-diazenyl]piperazine (4) has been determined by single crystal X-ray diffraction analysis. The bis-triazene (4) adopts a normal chair conformation in the piperazine ring, with puckering parameters : φ2 = −29(5)°, QT = 0.534(2) ? and θ2 = 177.0(2)°. The crystal structure of 4 is compared with the structure of the triazene (2a) and the closely related bis-triazenes (3 and 5a). The piperazine ring of 2a and 4 adopt a typical chair conformation, whereas the piperazine ring of 3 adopts an unusual pseudo-boat conformation. Crystal data: 4 C18H22N6, triclinic, space group P[`1] P\overline{1} , a = 6.8925(2) ?, b = 7.8574(3) ?, c = 16.8856(8) ?, α = 103.103(2)°, β = 90.528(2)°, γ = 101.776(2)° and V = 870.44 (6) ?3, for Z = 2. 相似文献5.
Nermin Doğan Süheyla Özbey Mehmet Karakaplan Tarık Aral 《Journal of chemical crystallography》2008,38(12):943-947
Abstract The crystal and molecular structure of chiral crown ether, (S)-2-[(4-methoxyphenoxy)methyl]-15-crown-5 · NaClO4, has been determined by single-crystal X-ray diffraction. The complex crystallizes in the orthorombic space group Pbca with
Z = 8. Lattice parameters are a = 11.451(2), b = 12.842(3), c = 31.330(7) ?. The structure was refined to R factor of 0.0547.
The Na ion is heptacoordinated. The Na–Oether distances range from 2.363(4) to 2.433(4) ? and average 2.404(5) ?. Perchlorate anion is bounded to sodium ion asymmetrically;
the Na–O8 and Na–O9 distances are 2.444(5) ? and 2.607(5) ?. The C–O and C–C distances of the 15-membered ring average 1.419(9)
and 1.478(12) ? while the O–C–C and C–O–C angles average 108.2(6)˚ and 115.4(6)˚.
Index Abstract In the molecule, the sodium ion is seven coordinated by the five ring oxygen atoms and two oxygen atoms of the perchlorate
anion. The macrocyclic strand of the molecule displays ag-a, ag+a, ag−a, ag+a, ag−g-set of torsion angles.
相似文献
6.
Bidhan A. Shinkre Dwayaja H. Nadkarni Samuel B. OwensJr. Gary M. Gray Sadanandan E. Velu 《Journal of chemical crystallography》2008,38(3):205-209
Abstract Details of the synthesis of the E isomer of 3-(2,5-dimethoxyphenyl)-2-(4-methoxyphenyl)acrylonitrile, and the X-ray crystal structures of both the E and Z isomers of this compound are presented. The E isomer crystallizes in the P21/c space group with cell parameters, a = 8.5659(17) ?, b = 16.399(3) ?, c = 11.224(2) ?, α = 90°, β = 95.27(3)°, γ = 90°and Z = 4. The Z isomer crystallizes in the Pca21 space group with cell parameters, a = 4.1223(8) ?, b = 19.113(4) ?, c = 19.453(4) ?, α = 90°, β = 90°, γ = 90° and Z = 4.
Index Abstract Synthesis of E isomer and X-ray crystal structure determination of both E and Z isomers of 3-(2,5-dimethoxyphenyl)-2-(4-methoxyphenyl)acrylonitrile
are presented.
相似文献
7.
Kusum Bania Rupam J. Sarma Anirban Karmakar Jubaraj B. Baruah 《Journal of chemical crystallography》2007,37(12):859-864
Abstract The crystal structures of four bis-phenols are reported to substantiate the fact that the weak interactions play a major role
in the crystal packing of bis-phenols. The reaction of 2,4-dimethylphenol with aldehydes such as 2-naphthaldehyde, terephthaldehyde
in the presence of trifluoracetic acid gave 2-[bis(2-hydroxy 3,5-dimethylphenyl)methyl]naphthalene (1) and 4-[bis(2-hydroxy 3,5-dimethylphenyl) methyl]benzaldehyde (2), respectively. The 2-[bis-(2-hydroxy 3,5-dimethylphenyl)-methyl]naphthalene (1) crystallizes in orthorhombic, Pbca, a = 11.905(3) ?, b = 18.788(5) ?, c = 18.894(5) ?, 4-[bis(2-hydroxy 3,5-dimethylphenyl)methyl] benzaldehyde (2) in monoclinic, Cc, a = 8.880(3) ?, b = 16.394(7) ?, c = 13.700(5) ?, γ = 104.542(2)°. The reaction of 2-nitrobenzaldehyde with 2,4-dimethylphenol gave 2-benzo[c] isoxazo-3-yl
4,6-dimethylphenol (3) and its crystal parameters are orthorhombic, P212121, a = 7.737(6) ?, b = 11.885(9) ?, c = 13.336(8) ?. The reaction of 2,6-dimethylphenol with 4-nitrobenzaldehyde and 2-chlorobenzaldehyde gave bis(4-hydroxy 3,5-dimethylphenyl)(4-nitrophenyl)methane
(4) and bis(4-hydroxy 3,5-dimethylphenyl)(2-chlorophenyl)methane (5), respectively. The bis(4-hydroxy 3,5dimethylphenyl)(4-nitrophenyl)methane (4) crystallizes in monoclinic, C2/c, a = 25.921(1) ?, b = 12.202(4) ?, c = 15.6084(7) ?, β = 122.172(4)°, and bis(4-hydroxy 3,5-dimethylphenyl) (2-chlorophenyl)methane crystallizes as acetonitrile
solvate (5) in triclinic, P-1, a = 12.314(3) ?, b = 14.111(3) ?, c = 15.078(5) ?, α = 98.268(2)°, β = 111.268(2)°, γ = 114.304(1)˚. The unit cell of 5 contains two pairs of crystallographically unsymmetric molecules of bis-phenols.
Index abstract The crystal structures of four bis-phenols are reported to substantiate the fact that the weak interactions plays a major
role in crystal packing and can induce symmetry non-equivalence among bis-phenols in unit cell of bis-phenols.
相似文献
8.
(4E)-5-(3-Chlorophenyl)-N-(4-chlorophenyl)-2-diazo-3-oxopent-4-enoic acid amide (5) was synthesized from p-chloroaniline to N-(4-chlorophenyl)-2-diazo-3-oxo-butyramide (4) with 3-chlorobenzaldehyde. The yielded product 5 was investigated with X-ray crystallographic, NMR, MS, and IR techniques. Compound 5 (C17H11Cl2N3O2, Formula wt = 360.19), crystallizes in the monoclinic space group P21/c with unit cell parameters a = 10.516(2), b = 17.996(4), c = 8.902(2) Å, α = 90.00, β = 105.36(3), γ = 90.00°. V = 1624.5(6) Å3, Z = 4, D x = 1.473 Mg m?3. The final R was 0.0511. 相似文献
9.
4-(E)-2-[3-(3-[(E)-2-(4-cyanophenyl)-1-diazenyl]hexahydro-1-pyrimidinylmethyl)hexahydro-1-pyrimidinyl]-1-diazenylbenzonitrile (1) has been synthesized by reaction of p-cyanobenzene diazonium chloride with a mixture of formaldehyde and 1,3-propanediamine. The crystal structure has been determined by single crystal X-ray diffraction analysis. The bis-triazene (1) adopts a folded conformation, similar to previously studied ethylenediamine analogues, and there is evidence of -stacking in the crystal packing. The two planar phenyltriazenyl groups are almost parallel, forming an angle of 6.6(1), and display weak intermolecular s interactions between molecules. This result establishes the structure of the product of this diazonium coupling reaction as the 1-(1-hexahydropyimidinylmethyl)hexahydropyrimidine derivative and not the alternate tetraazabicyclo[5.5.1]tridecane derivative. Crystal data: 1C23H26N10, monoclinic, space group P21/c, a = 10.717(1) Å, b = 7.749(1) Å, c = 28.252(2) Å, = 97.223(2), V = 2327.5(5) Å3, for Z = 4. 相似文献
10.
Resul Sevinçek Muhittin Aygün Serap Alp Canan Kazak 《Journal of chemical crystallography》2011,41(8):1140-1144
Abstract
Molecular and crystal structure of 4-[(p-N,N-dimethylamino)benzylidene]-2-phenyloxazol-5-one, C18H16N2O2, have been determined by single crystal X-ray diffraction study. The title compound is monoclinic, with a = 12.1704(23) ?, b = 3.9810(5) ?, c = 30.9603(56) ?, β = 101.176(15)°, Z = 4, D x = 1.32 g/cm3, μ(Mo Kα) = 0.087 mm−1, and space group is P121/c1. The structure was solved by direct methods and refined to a final R = 0.047 for 3166 reflections with I > 2σ(I). The crystal structure is stabilized by C–H⋯O and C–H⋯N type intra-molecular, C–H⋯O type inter-molecular interactions. To enlighten the flexibility and the geometric isomerism (E or Z) of the title compound, the selected torsion angle is varied from −180 to 180° in every 10° separately and molecular energy profile is calculated and analyzed. 相似文献11.
Tuncay Tunç Musa Sarı Murat Sadıkoğlu Orhan Büyükgüngör 《Journal of chemical crystallography》2009,39(9):672-676
Abstract A new Schiff-base complex 2-{(E)-[2-hydroxyphenyl)imino]methyl}phenol has been synthesized and characterized by elemental analyses, UV–VIS and IR spectroscopy
and single crystal X-ray determination. The structure comprises two independent and similar molecules. The two independent
molecules in the asymmetric unit are hydrogen bonded and have different conformations. In each molecule, C13H11NO2, adopt an E configuration about the azomethine C–N double bond. The complex crystallized in the triclinic space group P-1.
Two benzene rings and azomethine group are practically coplanar, as a result of intramolecular hydrogen bonds involving the
hydroxy O atom and azomethine N atom. Also hydroxy group of the molecule is the presence intermolecular O–H···O hydrogen bonds
with the hydroxy group of the other molecule.
Index Abstract and Figure A new Schiff-base complex 2-{(E)-[2-hydroxyphenyl)imino]methyl}phenol has been synthesized and characterized by elemental analyses, UV–VIS and IR spectroscopy
and single crystal X-ray determination. The structure comprises two independent and similar molecules. The two independent
molecules in the asymmetric unit are hydrogen bonded and have different conformations. In each molecule, C13H11NO2, adopt
an E configuration about the azomethine C–N double bond. The complex crystallized in the triclinic space group P-1. Two benzene
rings and azomethine group are practically coplanar, as a result of intramolecular hydrogen bonds involving the hydroxy O
atom and azomethine N atom. Also hydroxy group of the molecule is the presence intermolecular O–H···O hydrogen bonds with
the hydroxy group of the other molecule.
相似文献
12.
Yelda Bingöl Alpaslan Nevin Süleymanoğlu Emin Öztekin Ferda Erşahin Erbil Ağar Şamil Işık 《Journal of chemical crystallography》2010,40(11):950-956
Abstract
The molecular and crystal structure of the title compound, C14H11Cl2NO, has been determined by X-ray single crystal diffraction technique. The compound crystallizes in the orthorhombic, space group Pbca with unit cell dimensions a = 7.5537(10) ?, b = 11.5518(13) ?, c = 29.760(4) ?, M r = 280.14, V = 2596.8(6) ?3, Z = 8, R 1 = 0.065 and wR 2 = 0.191. The title compound exists in the enol–imine tautomeric form with a strong intramolecular O–H···N hydrogen bond. The dihedral angle between the two benzene rings is 37.66(15)°. The asymmetric unit in the crystal structure contains only one neutral molecule. Calculational studies were performed by using AM1, PM3, PM6 semi-empirical and DFT methods. Geometry optimizations of compound have been carried out by using three semi-empirical methods and DFT method and bond lengths, bond and torsion angles of title compound have been determined. Dipole moments (Debye) and the energy parameters of compound (kcal/mol) were calculated by using above mentioned calculation methods. Atomic charge distribution has been obtained from AM1, PM3, PM6 and DFT. In order to determine conformational flexibility on the molecule, molecular energy profile of the title compound was obtained with respect to the selected torsion angle T(N1–C7–C1–C2), which is varied from −180° to +180° in every 10 via PM3 semi-empirical method. 相似文献13.
1-[(E)-2-(4-bromophenyl)-1-diazenyl]-3-({3-[(E)-2-(4-bromophenyl)-1-diazenyl]-6-ethylhexahydro-1-pyrimidinyl}methyl)-4-ethylhexahydropyrimidine (1) has been synthesized by reaction of a mixture of formaldehyde and 1,3-pentanediamine{DYTEK®EPdiamine} with p-bromobenzenediazonium chloride. This compound crystallizes in two polymorphic forms 1-α and 1-β whose crystal structures have been determined by single crystal X-ray diffraction analysis. Both polymorphs 1-α and 1-β display crystallographic disorder within the hexahydropyrimidine rings. The molecule of 1 is built up of two equivalent 3-(aryldiazenyl)-6-ethylhexahydro-1-pyrimidinyl groups in the s-trans orientation around the central methylene group (C13). In both structures the triazene moieties adopt the anti configuration around the N=N bonds, displaying significant π-conjugation. The crystal packings are determined only by van der Waals interactions. The crystal structures of 1-α and 1-β are compared with the previously reported structure of the 5,5-dimethylhexahydropyrimidine analogue 3. Compounds 1 and 3 are isomeric with respect to the hexahydropyrimidine moiety. The structures of 1 and 3 are very different in one respect; in 1 the aryldiazenyl-hexahydropyrimidinyl groups are in the s-trans orientation around the central methylene group, whereas in 3 the arrangement of the aryldiazenylhexahydropyrimidinyl groups is the s-cis orientation. Crystal data: 1-α C25H34N8Br2, monoclinic, space group P2(1)/c, a = 9.2150(3), b = 19.4059(6), c = 15.4324(5) Å, β = 98.738(1)°, V = 2727.7(2) Å3, for Z = 4; 1-β C25H34N8Br2, triclinic, space group P-1, a = 9.6009(3), b = 10.7509(4), c = 14.2169(5) Å, α = 99.830(2), β = 105.973(3), γ = 95.578(1)°, V = 1373.9(1) Å3, for Z = 2. 相似文献
14.
The crystal structure of (E)-2-[(2-Bromophenylimino)methyl]-5-methoxyphenol is determined by using X-ray diffraction and then the molecular structure
is investigated with density functional theory (DFT). X-Ray study shows that the title compound has a strong intramolecular
O-H…N hydrogen bond and three dimensional crystal structure is primarily determined by C-H…π and weak van der Waals interactions.
The strong O-H…N bond is an evidence of the preference for the phenol-imine tautomeric form in the solid state. Optimized
molecular geometry is calculated with DFT at the B3LYP/6-31G(d,p) level. The IR spectra of compound were recorded experimentally
and calculated to compare with each other. The results from both experiment and theoretical calculations are compared in this
study. 相似文献
15.
Hüseyin Ünver Mustafa Yıldız Aşkın Kiraz Özen Özgen 《Journal of chemical crystallography》2009,39(1):17-23
Abstract The Schiff base (Z)-6-[(2-hydroxyphenylamino)methylene]-2-methoxycyclohexa-2,4-dienone has been synthesized from the reaction of 2-aminophenol
with 2-hydroxy-3-methoxybenzaldehyde. The title compound has been characterized by elemental analysis, FT-IR, 1H-NMR, 13C-NMR and UV–Visible techniques. The structure of the title compound also was determined crystallographically. The crystal
structure has been solved by direct methods and refined by full-matrix least squares. The title compound crystallize in the
monoclinic space group P21/c with a = 10.438(1), b = 8.851(1), c = 12.746(1) ?, β = 95.72(1)°, V = 1171.7(2) ?3, D
x
= 1.379 g cm−3, respectively (R1 = 0.0522 and wR2 = 0.126 for 1442 reflections [I > 2σ(I)]).
Index Abstract
N-salicylideneaniline derivatives have been shown to exist as tautomeric forms due to intramolecular proton shifts between
the phenol-oxygen and the imine-nitrogen, via intramolecular hydrogen bonding O–H···N or O···H–N.
相似文献
16.
Nihal Kan Kaynar Erbil Ağar Hasan Tanak Songul Sahin Orhan Büyükgüngör Metin Yavuz 《Crystallography Reports》2018,63(3):372-374
The molecular structure of the title compound, C14H11ClN2O4, was determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic sp. gr. P21/c with Z = 4. The title compound, C14H11ClN2O4, is a Schiff base which adopts the phenol-imine tautomeric form in the solid state.The molecule is almost planar and the dihedral angle between the planes of two aromatic ring is 2.2(1)°. The molecular structure is stabilized by intramolecular O–H···N hydrogen bond which generates a six-membered ring. In the crystal structure, the molecules are linked together by intermolecular C–H···O interactions. 相似文献
17.
Synthesis and X-ray structural investigations have been carried out for the two title compounds C14H10N2O (3a) and C22H26N2O (3b). Compound 3a crystallizes in the monoclinic space group P21/c, with a = 3.843(1) Å, b = 24.618(5) Å, c = 11.318(2) Å, = 92.61(3), V = 1069.7(4) Å,3 and Z = 4. Compound 3b crystallizes in the triclinic space group P-1, with a = 9.004(2) Å, b = 9.447(2) Å, c = 11.713(2) Å, = 76.70(3), = 83.12(3), = 82.16(3), V = 956.5(3) Å,3 and Z = 2. Both stilbazole derivatives have Z-geometry about the ethylene bridge which links the heterocyclic and aromatic rings. The molecular skeleton of 3a is slightly non-planar: the dihedral angles between the acrylonitrile linkage and the pyridine ring, and between this linkage and the p-hydroxyphenyl ring are 7.2(2) and 4.1(2), respectively. The molecular skeleton of 3b is less planar: the values of similar dihedral angles are 17.0(2) and 20.8(2), respectively. In the crystal of 3a, the molecules are packed in stacks along the a axis with head-to-head orientation. Intermolecular hydrogen bonds O=H s N and C=H s N link molecules into sheets parallel to (100) plane. In the crystals of 3b, the molecules have a head-to-tail orientation and intermolecular hydrogen bonds O=H s N link the molecules into infinite chains along [01-1] direction. 相似文献
18.
Waseeq Ahmad Siddiqui Saeed Ahmad Hamid Latif Siddiqui Tanvir Hussain Masood Parvez 《Journal of chemical crystallography》2010,40(2):116-121
Abstract
o-[(Phenyl/p-methoxyphenyl)carbamoyl]benzene sulfonamides were synthesized in a straightforward manner utilizing directly saccharin and aniline/p-anisidine as starting material and their crystal structures have been determined. (C13H12N2O3S): Mr = 276.31, monoclinic, P21/c, a = 10.277(6), b = 7.501(2), c = 16.261(10) ?, β = 96.37(2)°, V = 1,245.8(11) ?3, Z = 4. (C14 H14 N2 O4 S): Mr = 306.33, monoclinic, P21/c, a = 10.381(5), b = 7.861(2), c = 16.837(9) ?, β = 93.43(2)°, V = 1,371.5(10) ?3, Z = 4. In both structures the phenyl rings are inclined at 47.09(7) and 39.88(5)° with respect to each other and the structures are characterized by extensive inter and intramolecular hydrogen bonds. 相似文献19.
Nihal Kan Kaynar Hasan Tanak Songul Şahin Necmi Dege Erbil Ağar Metin Yavuz 《Crystallography Reports》2016,61(2):239-242
The crystal structure of the title compound, C14H12N2O3, was recently determined as a mixture of its neutral (OH containing) and zwitterionic (NH containing) forms, in a 0.60 (4): 0.40 (4) ratio using the X-ray determination. In this study, the title compound has been characterized by FT-IR and X-ray diffraction. The redetermination showed that the title compound has only enol (OH) form because of lack of the NH stretching vibration in FT-IR spectrum. In addition, the molecular structure and tautomerism of the title compound have been discussed. 相似文献
20.
The X-ray crystal structure of 2-amino-3-cyano-4-(4-methylphenyl)-6-methoxyl-1,4,9,10-tetrahydrobenzo [f]chromene 1, C22H20N2O2, is determined. The crystals of compound 1 are triclinic, space group P-1, a = 10.120(1), b = 13.127(1), c = 15.203(2) Å, = 67.841(9), = 80.81(1), = 77.58(1), Z = 4, V = 1819.7(4) Å3. It is interesting that all the atoms of the pyran ring are coplanar, which is different from other similar compounds. The structure is stabilized by intermolecular hydrogen bonds. 相似文献