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1.
Aliakbar Dehno Khalaji Hossein Mighani Hamid Reza Bijanzadeh Kazuma Gotoh Hiroyuki Ishida 《Journal of chemical crystallography》2011,41(10):1515-1519
Abstract
New Schiff-base compound (E)-2-(2,5-dimethoxybenzylideneamino)phenol (1) was synthesized and characterized by elemental analyses, FT-IR and 1H-NMR spectroscopy and single crystal X-ray diffraction. Molecular orbital calculation has been carried out for 1 by using HF method at 6-31G basis set. The title compound 1 crystallizes in monoclinic system, space group C2/c, with a = 19.4581(13) ?, b = 9.5805(5) Ǻ, c = 13.8431(7) Ǻ, β = 93.471(2)°, V = 2575.9(3) Ǻ3 and Z = 8. In the crystal structure two molecules are stabilized by a pair of intermolecular O1–H1···N1i hydrogen bonds. The dimeric units are further linked via C6–H6···O3ii hydrogen bond. 相似文献2.
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3.
Zahid H. Chohan Hazoor A. Shad Loic Toupet Taibi Ben Hadda Mehmet Akkurt 《Journal of chemical crystallography》2011,41(2):159-162
Abstract
The title compound (3), C17H14BrN3O4S, is a Schiff base compound of 5-bromosalicylaldehyde (1) and sulfamethoxazole (2). The structure of (3) was determined by spectral (IR, 1H and 13C NMR), elemental analyses and X-ray diffraction data. Compound (3) crystallizes in the monoclinic space group C2/c, with a = 31.936(3), b = 6.2571(5), c = 16.903(1) ?, β = 94.867(8), V = 3365.5(5) ?3, Z = 8. In the molecule of compound (3), the molecule is bent at the S atom with a C–SO2–NH–C torsion angle of −86.3(3)°. Pairs of molecules, related by inversion centres, form intermolecular N–H···N hydrogen bonds to produce a dimer. An intramolecular phenolic O–H···N hydrogen bond is also formed. Intermolecular hydrogen bonding and π–π stacking hold the molecules together. The average distance between stacked benzene ring planes is 3.625(2) ?. 相似文献4.
Aran Kumar J. Dinesh Simerpal Kour M. S. Hundal Sushil K. Pandey 《Journal of chemical crystallography》2012,42(4):299-304
Abstract
Triethylammonium salts of O,O′-alkylene dithiophosphato like OGOPS2HNEt3, [where, G = –CH2CMe2CH2–(1), –CH2CEt2CH2–(2), –CMe2CH2CHMe–(3) and –CMe2CMe2–(4)] have been synthesized in quantitative yield by the direct reaction of P2S5 with 1,2- and 1,3-substituted glycols in presence of triethylamine, Et3N, in 1:2:2 molar stoichiometry in toluene. These have been mainly characterized by molecular weight, IR and NMR (1H, 13C and 31P) spectroscopic studies. Single crystal X-ray structure analysis of [OCH2CMe2CH2OPS2HNEt3] reveals that phosphorus atom is tetrahedrally bonded to two sulfur atoms and two oxygen atoms in the ring and the molecule exists as discrete cation and anion. The structure is stabilized by cation–anion N–H···S hydrogen bonded interactions. Antiparallel pattern of triethylammonium ion is sandwiched within the two-dimensional layers of the ring system. 相似文献5.
Two New 2-Benzoylbenzoate Metal Complexes with Bapen: Synthesis,Spectroscopic and Crystal Structures
Abstract
Coordination compounds of compositions [Ni(bba)2(bapen)] (1) and [Cu(bba)2(bapen)]0.5H2O (2), where bba = 2-benzoylbenzoate, bapen = N,N′-bis(3-aminopropyl)ethylenediamine, have been prepared. The crystal and molecular structure of (1) and (2) were determined by X-ray analysis. Nickel and copper atoms are six-coordinated by four N atoms of amine and O donor atoms of 2-benzoylbenzoate anions, whereas 0.5 water molecule is situated outside the coordination sphere in (2). The calculated ∆(OCO) values are consistent with presence of monodentate carboxylate. Thermal analysis show that the mass losses of 1 in the temperature ranges 240–343 °C correspond to the decomposition of bba ligands, while the mass losses of 2 in the temperature ranges 105–125 °C correspond to the decomposition of crystal lattice water molecule. 相似文献6.
Abstract
A mononuclear copper(II) complex, [Cu(pydca)(2-Etlm)(H2O)] (1) (H2pydca = pyridine-2,6-dicarboxylic acid, 2-Etlm = 2-ethylimidazole), has been synthesized and characterized by elemental analyses, IR, UV–Vis, TG-DTA and single crystal X-ray diffraction. The complex 1 is in the orthorhombic crystal system, space group Pbca and Z = 8. The structural analysis indicated that Cu(II) center is five coordinated in a slightly distorted square pyramidal geometry by one N and two O atoms from a 2,6-pyridine dicarboxylate dianion, one N atom from a 2-ethylimidazole ligand, and one O atom from a aqua molecule. This mononuclear motif of 1 is further assembled to 3D supramolecular framework through strong O–H···O and N–H···O hydrogen bonding interactions. 相似文献7.
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
8.
Abstract
The unstable crystals of triammonium fac-trichloridotrioxidorhenate(VII) chloride have been obtained from ammonium rhenate(VII) solution in concentrated hydrochloric acid. The crystal structure consists of fac-trichloridotrioxidorhenate(VII) anions, chloride anions and ammonium cations. Each fac-trichloridotrioxidorhenate(VII) anion and each chloride anion lies in special position of 3m site symmetry (cell parameters: a = 9.026(3) Å; c = 7.690(4) Å; space group: P63 mc). The ammonium cation lies in special position of m site symmetry. The following anion geometrical parameters of the fac-trichloridotrioxidorhenate(VII) anion have been obtained: Re–O bond length of 1.720(2) Å, Re–Cl bond length of 2.5428(9) Å, the bond angles: O–Re–O of 103.5(1)° and Cl–Re–Cl of 79.8(1)°. 相似文献9.
Abstract
A new nickel(II) complex formulated as, trans-[Ni(amp)2(SCN)2(H2O)2]·2H2O (1), (amp = 2-aminopyrimidine) has been synthesized and characterized by elemental analysis, IR spectroscopy, its molecular and crystal structures were determined by X-ray crystal structure analysis and its thermal stability by TGA/DTA methods. 1 is a neutral complex and the central atom sits on an inversion center and is coordinated by two endocyclic nitrogen atoms of two 2-aminopyrimidine heterocycles, two oxygen atoms of two water molecules and two nitrogen atoms of SCN− ions. 2-aminopyrimidine molecules, thiocyanate ions and water molecules are in trans position. Thermal methods confirm two co-crystallized water molecules in 1. π–π stacking interactions and extensive O–H···O, O–H···N, O–H···S and N–H···N hydrogen bonds contribute to the formation of a three-dimensional supramolecular structure. Crystal data for complex at 120 K: triclinic, space group P-1, a = 7.2026(14), b = 7.8332(15), c = 9.0270(17) ?, α = 67.694(3), β = 72.732(4), γ = 77.012(4), Z = 1, R 1 = 0.0323. 相似文献10.
Mohd Abdul Fatah Abdul Manan M. Ibrahim M. Tahir Karen A. Crouse David J. Watkin 《Journal of chemical crystallography》2011,41(2):230-235
Abstract
S-methyl 2-(5-chloro-2-oxoindolin-3-ylidene)hydrazinecarbodithioate (SM5ClISA) has been prepared from S-methyldithiocarbazate and 5-chloroisatin. The compound crystallized in monoclinic crystal system with space group P 21/n, Z = 4, V = 1201.85(7) ?3 and unit cell parameters a = 6.5466(2) ?, b = 7.5056(3) ?, c = 24.6509(8) ?, α = γ = 90° and β = 97.1434(18)°. The crystal structure reveals that the compound exists in the thione form with the chlorine occupies the fifth position in the isatin ring with the bond length of 1.739(2) ?. The 5-chloroisatin moiety is trans with respect to the C3–N2 and C3–S4 bonds whereas the methyl group of the dithiocarbazate moiety is cis with respect to the C3–N2 and C3–S5 bonds. 相似文献11.
Abstract
A series of novel 1,3-disubstituted-2-propyleno-1-one derivatives containing pyrazole ring were synthesized and characterized by IR, MS, H1NMR and elemental analysis. The structure of C25H20N2O2 (3a) was determined by single crystal X-ray crystallography. C25H20N2O2 is monoclinic with space group P21/c and cell constans: a = 9.863(2)?, b = 20.054(4)?, c = 10.274(2)? V = 2028.0(7)?3 and Z = 4. In addition, the crystal structure was solved by direct methods and refined by full-matrix least-squares on F 2 to final values of R1 = 0.0657 and wR2 = 0.1806, and it shows that the complex units are linked by non-classical hydrogen-bonding. The molecule adopts a trans configuration about the central C = C double bond. The crystal structure is stabilized by C–O···π intermolecular hydrogen bonds and π–π stacking interactions. 相似文献12.
Abstract
The tetrafluoroborate salt of 4-methoxybenzyl N-2-(dimethylamino)ethyl-N-nitrosocarbamate was prepared in two steps, via the corresponding carbamate. Its crystal structure is monoclinic, space group P21/c. The unit cell dimensions are: a = 19.499(8) ?, b = 5.877(3) ?, c = 15.757(7) ?, α = 90°, β = 110.019(7)°, γ = 90°, V = 1696.5(12) ?3, Z = 4. The structure exhibits an unexpected, pseudo-gauche conformation with respect to the C2–C3 bond, due to a stabilizing hydrogen bond between the carbonyl oxygen (O1) and the hydrogen atom at the trialkylammonium center (H3n), with a distance between them of 2.37 ?. DFT calculations on the cation (B3LYP/6-31 + G(d)) confirm that the hydrogen bond stabilized gauche conformation is the global minimum structure. 相似文献13.
Yu Yu Xiao-Wen Li Lu-Yan Jiang Yan-Tuan Li Zhi-Yong Wu Cui-Wei Yan 《Journal of chemical crystallography》2011,41(7):959-965
Abstract
A new μ-oxamido-bridged copper(II)–copper(II) binuclear complex with formula of [Cu2(heap)](bipy)(ClO4)2, where H2heap and bipy are N,N′-bis(N-hydroxyethylaminopropyl)-oxamide and 4,4′-bipyridine, respectively, has been synthesized and characterized by elemental analyses, molar conductivity measurement, IR and electronic spectra studies, and single-crystal X-ray diffraction. The single-crystal X-ray analysis reveals that the complex has two embedded inversion centers at the mid-points of the C6–C6i bond of the oxamido group and the C7–C7ii bond of the 4,4′-bipyridine, respectively [symmetry code: (i) 2−x, 1−y, 1−z; (ii) =2−x, −y, 1−z]. Copper(II) atom is in a square-planar coordination geometry. The Cu···Cu separation through the oxamido birdge is 5.1430(8) ?. The bridging ligand (heap2−) adopts a bis-tetradentate trans conformation. A one-dimensional hydrogen bonding supramolecular structure parallel to the [2 1 0] direction is found in the crystal. The interaction of the binuclear copper(II) complex with herring sperm DNA (HS-DNA) was investigated by using absorption and emission spectra, electrochemical techniques and viscometry. The results suggest that the binuclear copper(II) complex interacts with HS-DNA by electrostatic interaction with intrinsic binding constant of 1.54 × 104 M−1. 相似文献14.
Abstract
The unique dinuclear Ir(III) complex (Cp*IrCl)(μ-H)[μ-(η1:η3-C6H6S)](IrCp*) (1) has been synthesized and characterized by NMR spectroscopy (1H and 13C), elemental analysis, and single crystal X-ray diffraction. It is the first structurally determined complex in which an activated thiophene ligand displays an η3-allylic interaction. 1 appears to form from successive C-H bond activations of 2,5-dimethylthiophene, resulting in its bridging the two iridium centers. The η3-allylic interaction occurs with one of the Ir centers and has Ir–Cthio bond lengths ranging from 2.133(5)-2.207(5) ?; the C–C double bond involved in the interaction has a bond length of 1.438(7) ? compared to 1.348(8) ? for the uncoordinated C–C double bond. The 3-carbon of the thiophene ring bridges both iridium centers with bond lengths of 2.036(5) ? and 2.208(5) ?. 1 crystallizes in space group P−1 with cell constants a = 8.6303(6) ?, b = 9.0153(6) ?, c = 18.1089(12) ?, α = 84.728(1)°, β = 87.534(1)°, γ = 64.373(1)°, and Z = 2. The structure was solved by direct methods and refined to R = 0.0363 (F 2 > 2σ(F 2)) and wR = 0.0851 (F 2). The NMR data indicate the solution state structure is consistent with the solid state structure. 相似文献15.
Mukhtiar Hussain Muhammad Hanif Muhammad Altaf Saqib Ali Helen Stoeckli-Evans 《Journal of chemical crystallography》2011,41(1):30-33
Abstract
In the solid-state structure of the title compound, C16H10FNO6, the configuration about the C=C double bond is E. The compound crystallized in the triclinic system, having space group P-1 with unit cell dimensions a = 5.829(10) ?, b = 8.801(16) ?, c = 13.543(3) ?, α = 87.753(15)°, β = 81.945(15)°, γ = 86.342(14)°. The structure of the molecule is V-shaped and in the crystal the molecules are linked to form inversion dimers connected by pairs of C–H···O hydrogen bonds. 相似文献16.
Fiona A. M. Rudolph Amy L. Fuller Alexandra M. Z. Slawin Michael Bühl R. Alan Aitken J. Derek Woollins 《Journal of chemical crystallography》2010,40(3):253-265
Abstract
The X-rays structures of diphenyl sulfone 1, bis(3-aminophenyl) sulfone 2, bis(4-nitrophenyl) sulfone 3, 2-nitrophenylphenyl sulfone 4, benzylphenzyl sulfone 5, 4-nitrobenzylphenyl sulfone 6, 4-methylphenylbenzyl sulfone 7, dibenzyl sulfone 8, benzylisopropyl sulfone 9, and methylacetate,ethyl sulfone 10, are reported. B3PW91 DFT calculations were performed on selected sulfones for comparison. The S = O distances in these compounds range from 1.392(5) to 1.463(3) Å and S–C bond distances range from 1.743(7) to 1.790(3) Å. The C–S–C bond angles vary from 101.1(3)° to 106.80(14)° and the O–S–O bond angles vary from 116.7(2)° to 120.61(8)°. Using data obtained here and comparison with published structural data no evidence was found for para substituents on aryl groups influencing S–O bond distances, however, small changes on S–C bond distances were noted. Additionally, if the sulfur is flanked by an alkyl group the S–C distance is slightly larger than when it is flanked by an aryl group. Most of the sulfone compounds studied here display intermolecular soft hydrogen bonding interactions which influence their solid state packing. Furthermore, in dialkyl sulfone compounds these interactions appear to be strong enough to overcome conformational barriers calculated to be ca. 6 kJ mol−1. 相似文献17.
Gang Chen Ying Tang Qun-Zheng Zhang Ya Wu Shun-Zhen Mu 《Journal of chemical crystallography》2010,40(4):369-372
Abstract
3-Hydroxy-3-nitromethyl-1,3-dihydro-indol-2-one was synthesized from isatin by Henry reaction using an eco-friendly method and characterized by NMR and MS. The crystal structure was determined from single-crystal X-ray diffraction data. It crystallizes in the orthorhombic space group, Pbca, with unit cell dimensions a = 10.515 (2) Å, b = 7.3736 (14) Å, and c = 23.261 (4) Å. The two rings are coplanar and the angle between hydroxyl group and nitromethyl group is 109.07(9)°. In the crystal structure, intermolecular N–H···O and O–H···O hydrogen bonds are responsible for the formation of a 3-dimensional network. No intramolecular hydrogen bond exists. 相似文献18.
Miguel Guerrero Josefina Pons Mercè Font-Bardia Teresa Calvet Josep Ros 《Journal of chemical crystallography》2011,41(5):721-726
Abstract
The crystal structure of the title compound C22H30N4O2·H2O (L), has been determined using X-ray diffraction at 293 K. The crystal of 1,2-bis[4-(3,5-dimethyl-1H-pyrazol-1-yl)-2-oxobutyl]benzene is in triclinic crystal system with space group P(−1) (Z = 2), lattice parameters a = 8.225(6) ?, b = 10.967(6) ?, c = 12.903(6) ?, V = 1119.1(11) ?3. Analyses of single crystals of L, crystallized from dichloromethane/diethyl ether (1:1), revealed that the molecules are arranged in couples, which adopt a pseudo chair conformation, by means of intermolecular O–H···N hydrogen bonding interactions. Moreover, the extended structure revealed a 1D chain caused by several C–H···N intermolecular interactions. 相似文献19.
Oscar F. Vázquez-Vuelvas David Morales-Morales Juan M. Germán-Acacio Mikhail Tlenkopatchev Armando Pineda-Contreras 《Journal of chemical crystallography》2011,41(3):419-424
Abstract
Two new 1,3,3-trimethyl-2-methylene-2,3-dyhidro-1H-indole derivatives, (E)-2,3-dihydro-2-(4-cyanophenylacylidene)-1,3,3-trimethyl-1H-indole, (I), and (E)-2,3-dihydro-2-(4-chlorophenylacylidene)-1,3,3-trimethyl-1H-indole, (II), have been synthesized and their crystal structure determined by single crystal X-ray diffraction. (I), C20H18N2O, crystallizes in a monoclinic space group, P21/c, with unit cell parameters a = 9.882 (3), b = 15.614(4), c = 11.181(3) ?, β = 106.691(4)°, Z = 4. (II), C19H18Cl N O, crystallizes in a monoclinic space group, P21/n, with unit cell parameters a = 14.6722(19), b = 7.2597(9), c = 16.304(2) ?, β = 111.249 (2)°, Z = 4. The molecules consist of a enaminoketone group formed by a Fischer base 1,3,3-trimethyl-2-methylene-2,3-dihydro-1H-indole bonded, at the exocyclic electron-rich β-carbon atom of the indole moiety, with the benzoyl chloride derivatives substituted at para-positions with cyano and chloro groups. The molecules adopt a s-cis conformation with respect to the C=O bond towards the C=C bond, and a E configuration about the latter indole exocyclic alkene C–C bond. Intermolecular arrangement of the crystals show, for (I) an antiparallel stacking mode favored by the formation of weak C–H···π interactions involving the phenyl ring attached to the carbonyl group and the phenyl of the indole fragment in a head-to-tail mode, whereas, (II) present an weak C–H···Hal interaction. 相似文献20.
Mustafa Yıldız Hava Özay Hüseyin Ünver Nazan Ocak İskeleli D. Mehmet Zengin Tahsin Nuri Durlu 《Journal of chemical crystallography》2010,40(11):909-913