共查询到20条相似文献,搜索用时 678 毫秒
1.
Fernando Rascón-Cruz Sandra González-Gallardo Miguel A. Muñoz-Hernández Rubén A. Toscano Verónica García-Montalvo 《Journal of chemical crystallography》2009,39(7):530-534
Abstract Synthesis and X-ray structural determination of three phosphorus compounds are reported. (3b) is monoclinic P2(1)/c with a = 11.852(1), b = 12.825(1), c = 12.445(1) ?, β = 103.693(1)o; (4a) and (4b) are monoclinic P2(1)/n with a = 12.1422(16), b = 9.0860(12), c = 14.845(2) ?, β = 96.498(3)o for (4a), and a = 12.2714(16), b = 9.2812(12), c = 14.800(2) ?, β = 97.176(2)o for (4b). They all exhibit distorted tetrahedral geometry about the P atom. Ph2P(X)NHC7H7 (X=S (4a) and X=Se (4b)) show typical P–S and P–Se double bond distances and P–N single bonds, while P–S bond in 1-Ad2P(S)Cl (3b) is comparable to P–S single bonded probably due to the largeness of 1-adamantyl groups.
Graphical Abstract Synthesis and X-ray structural determination of 1-Ad2P(S)Cl (3b), Ph2P(S)NHC7H7 (4a) and Ph2P(Se)NHC7H7 (4b) are reported.
相似文献
2.
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
3.
Bala Chandra Chenna Bidhan A. Shinkre Shweta Patel Samuel B. OwensJr. Gary M. Gray Sadanandan E. Velu 《Journal of chemical crystallography》2008,38(3):189-194
Abstract Synthesis, separation and X-ray crystal structures of E and Z isomers of 3-(2,5-dimethoxyphenyl)-2-(4-methoxyphenyl)acrylic acid are reported. Separation of E and Z isomers from a 1:1 mixture has been carried out by selective acidification of their sodium salts carefully controlling the
pH of the solution. The structures of E and Z isomers were confirmed by determining crystal structures of these isomers using single crystal X-ray diffraction. The E isomer crystallizes in the P21/c space group with a = 11.493(2) ?, b = 5.5456(11) ?, c = 24.900(5) ?, α = 90°, β = 92.36(3)°, γ = 90°, Z = 4. The Z isomer crystallizes in the P21/c space group with a = 10.192(2) ?, b = 12.893(3) ?, c = 13.948(3) ?, α = 90°, β = 92.18(3)°, γ = 90°, Z = 4. Details of the synthesis and structural characterization and X-ray crystal structure determination of the title compounds
are presented.
Index Abstract
Synthesis, Separation and Crystal Structures of
E
and
Z
Isomers of 3-(2,5-Dimethoxyphenyl)-2-(4-Methoxyphenyl)Acrylic Acid
Balachandra Chenna, Bidhan A. Shinkre, Shweta Patel, Samuel B. Owens Jr., Gary M. Gray, Sadanandan E. Velu*
Separation of E and Z isomers of 3-(2,5-dimethoxyphenyl)-2-(4-methoxyphenyl)acrylic acid from a 1:1 mixture has been carried out by selective acidification
of their sodium salts and the structures of the individual isomers have been determined by X-ray single crystal diffraction.
相似文献
4.
Saroj K. S. Hazari Tapashi G. Roy Kanak K. Barua Edward R. T. Tiekink 《Journal of chemical crystallography》2008,38(1):1-8
Abstract In the crystal structure of the nitrate salt, columns of di-cationic macrocycles, each disposed about a center of inversion,
are interspersed by pairs of nitrate anions that form charged-assisted N–H···O hydrogen-bonding interactions, reinforced by
C–H···O contacts. The topology of the resulting supramolecular architecture is that of a linear chain and these associate
via further weak C–H···O contacts. In the structure of the acetate trihydrate, di-cationic macrocycles are circumscribed by
32-membered rings defined by O–H···O interactions, involving the acetate anions and solvent water molecules. Systematic variations
in the geometric parameters in the molecular structures are correlated with the influence of intermolecular interactions.
The nitrate crystallizes in the monoclinic space group P21/n with a = 8.3524(11) ?, b = 12.5497(16) ?, c = 11.1208(16) ?, β = 103.180(3)°, and Z = 2. The acetate trihydrate also crystallizes in the monoclinic space group P21/n with a = 9.6679(15) ?, b = 15.278(2) ?, c = 9.8376(18) ?, β = 106.068(5)°, and Z = 2.
Index Abstract
Supramolecular Association in the Structure of 2,9-
C-meso
-2,5,5,7,9,12,12,14-Octamethyl-1,8-diaza-4,11-
diazoniacyclotetradecane as its Bis(nitrate) and Bis(acetate) Trihydrate
Saroj K. S. Hazari,
(1)
Tapashi G. Roy,
(1)*
Kanak K. Barua
(1)
and Edward R. T. Tiekink
(2)*
A linear supramolecular chain stabilized by charge-assisted N–H···O hydrogen-bonding interactions is found in the nitrate
salt. In the acetate trihydrate, di-cationic macrocycles are circumscribed by 32-membered rings constructed by O–H···O hydrogen-bonds.
Supramolecular Association in the Structure of 2,9-
C-meso
-2,5,5,7,9,12,12,14-Octamethyl-1,8-diaza-4,11-
diazoniacyclotetradecane as its Bis(nitrate) and Bis(acetate) Trihydrate
Saroj K. S. Hazari,
(1)
Tapashi G. Roy,
(1)*
Kanak K. Barua
(1)
and Edward R. T. Tiekink
(2)*
(1)Department of Chemistry, University of Chittagong, Chittagong-4331, Bangladesh
(2)Department of Chemistry, The University of Texas at San Antonio, One UTSA Circle, San Antonio, Texas 78249-0698
Electronic supplementary material The online version of this article (doi: ) contains supplementary material, which is available to authorized users. 相似文献
5.
The crystal structure of 6,13-bis-(N,N-dimethylcarbamoyl)thioquinanthrene 3 has been determined as monoclinic, with space group P2(1)/c with lattice parameters a = 10.044(2) Å, b = 21.385(4) Å, c = 10.889(3) Å, = 102.92(3)°, Z = 4 and Dcalc = 1.342 Mg/m3. The middle 1,4-dithiin ring in the title compound 3, C24H20N4O2S2 is in a boat conformation with the dihedral angle between the planes of the aromatic rings 132.45(8)°. 相似文献
6.
Poonam Kaushik Dejan-Krešimir Bučar Leonard R. MacGillivray 《Journal of chemical crystallography》2007,37(10):713-715
Abstract The crystal and molecular structure of trans-1,2-bis(2-benzothiazolyl)ethene is reported. Crystal data for 1: monoclinic, space group C 2/c, a = 24.926(3) ?, b = 4.843(1) ?, c = 11.164(1) ?, β = 105.274(5) °, V = 1300.0(3) ?3, and D
c
= 1.50 g/cm3 for Z = 4 and R = 0.028. The molecule crystallizes in the form of a colorless plate and forms one-dimensional slipped π-stacks.
Graphical Abstract The title compound crystallizes to form 1D slipped π-stacks in the solid state.
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
7.
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8.
Amitabha Datta 《Journal of chemical crystallography》2009,39(9):619-622
Abstract The copper(II) complex [Cu(C5H4NCH2−N=CH–C6H3OCH3–O)Cl], (1) containing a new tridentate Schiff base ligand (LH), which is the 1:1 condensation product of 2-(aminomethyl)pyridine and o-vaniline, has been synthesised and characterized by IR and UV–Vis spectra. Structural investigation shows that 1 crystallizes to a monoclinic system, having space group P2(1)/c, a = 6.9634(7), b = 18.1209(19), c = 10.3448(11) ?, α = 90°, β = 103.97(2)°, γ = 90° and Z = 4. The coordination geometry around the copper atom is slightly distorted square planar, formed by the N2O donor set of the Schiff base and one Cl atom. The Cu–N(1), Cu–N(2), Cu–O(1) and Cu–Cl bond distances are 2.0114(14), 1.9414(14),
1.9147(12) and 2.2520(5) ?, respectively.
Index Abstract The copper(II) complex [Cu(C5H4NCH2−N=CH–C6H3OCH3–O)Cl], (1) containing a tridentate Schiff base ligand (LH), synthesised and characterized by IR and UV–Vis spectra. The central copper
ion possesses a distorted square-planar geometry.
相似文献
9.
R. Alan Howie Marcus V. N. de Souza Camilo H. da Silva Lima James L. Wardell Solange M. S. V. Wardell 《Journal of chemical crystallography》2012,42(4):394-400
Abstract
The molecule of (E)-3-(3-MeOC6H4CH=CHCO)-benzotriazole 1-oxide, 2, has a very near planar structure, while the 2-nitrophenyl ring is rotated out of the plane of the remaining atoms in (E)-3-(2-O2NC6H4CH=CHCO)-benzotriazole 1-oxide, 1. The nitrogen oxide bond lengths in 1 and 2 are 1.258 (6) and 1.2683 (15) ?, respectively, and are in the region found for related compounds. There are no strong intermolecular hydrogen-bonds in either compound, instead there are weak C–H···O intermolecular hydrogen-bonds and π···π stacking interactions in 1, and C–H···O, C–H···π, and π···π stacking interactions in 2. Different three-dimensional arrays are generated in each case. Compound 1 crystallises in the orthorhombic space group Pna21, with a = 25.061 (2) ?, b = 3.6997 (2) ?, c = 14.2623 (12) ? and Z = 4. Compound 2 crystallises in the triclinic space group P-1, with a = 5.7297 (3) ?, b = 10.8440 (6) ?, c = 11.4965 (6) ?, α = 89.689 (3)°, β = 76.019 (3)°, γ = 75.047 (3)°, Z = 2. 相似文献10.
The crystal structures of the new compounds 2,6-bis-hydrazinopyridine dihydrate (2), its tosylate salt (3) and 2,6-bis-(3,5-di-tert-butylpyrazolyl)pyridine (4) were obtained by single-crystal X-ray diffraction. Crystallization of 2 occurs in the centrosymmetric monoclinic space group P21/c (No. 14) with a = 9.6218(18), b = 6.7331(12), c = 13.489(3); and β = 109.292(8)∘ and Z = 4. Crystallization of 3 occurs in the centrosymmetric monoclinic space group P21/c (No. 14) with a = 26.530(3), b = 16.6456(18), c = 9.9458(10) and β = 96.828(5) and Z = 8, while 4 crystallizes in P21/n (No. 14) with a = 15.0555(10), b = 10.4496(7), c = 16.9599(12) and β = 101.480(4) and Z = 4. These are the only structures for any bis-hydrazinopyridines reported to date. Details of the synthesis, structures
and spectroscopic results are presented and discussed. 相似文献
11.
The crystal structure of trans-[((bis)triethylphosphine)(bis(phenylselenato))platinum (II)] has been determined by single crystal X-ray diffraction. Crystallization
occurs in the triclinic space group P-1 (No. 2) with a = 8.9964(2) ?, b = 11.5103(2) ?, c = 14.9335(3) ?; α = 85.8750(10)°, β = 72.5350(10)°, γ = 68.4450(10)°. Details of the structure and spectroscopic results are presented and discussed and comparisons are made with
related square planar platinum (II) structures. 相似文献
12.
Eric W. Reinheimer Hanhua Zhao Kim R. Dunbar 《Journal of chemical crystallography》2010,40(6):514-519
Abstract
The synthesis and crystal structure of the 1:1 complex o-Me2TTF-TCNB is reported. The complex crystallizes in the triclinic space group P-1 with a = 6.920(1) ?, b = 7.928(2) ?, c = 17.453(4) ?, α = 100.53(3)°, β = 99.66(3)°, and γ = 97.32(3)°. The bond length of the central C=C bond in o-Me2TTF is 1.342(2) ?, indicating a neutral state for the o-Me2TTF donor. 相似文献13.
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14.
Annamária Krajníková Róbert Gyepes Katarína Győryová 《Journal of chemical crystallography》2010,40(8):650-655
Abstract
The syntheses and structural characterizations of two novel 2-bromobenzoatozinc(II) complexes—[Zn(2-BrC6H4COO)2] n (I) and [Zn(2-BrC6H4COO)2(mnad)]2 (II), where mnad is N-methylnicotinamide are reported. Compound (I) crystallized with a monoclinic lattice (space group P21/c) and is polymeric in solid state. Its cell parameters are: a = 7.37220(10) Å, b = 19.9639(3) Å, c = 30.2756(5) Å, β = 94.7510(7)°, V = 4440.59(12) Å3, Z = 4. The coordination environments of all zinc atoms are distorted tetrahedra built from four carboxylate oxygen atoms coming from four 2-bromobenzoato ligands. Compound (II) crystallized with a monoclinic lattice (space group P21/c) with a = 11.7488(2) Å, b = 20.3683(3) Å, c = 9.30130(10) Å, β = 100.3941(11)°, V = 2189.30(5) Å3, Z = 2. This dimeric molecule features a paddle-wheel [Zn2O8] cage in solid state; the coordination environment of the central atom is square pyramidal consisting of four carboxylate oxygen atoms and the pyridine N atom of the mnad ligand. 相似文献15.
Abstract The synthesis, characterization, and molecular structure of the title compound, [(1-benzylpyrazole)[N,N-bis(2-aminoethyl)-1,2-ethanediamine]copper(II)] diperchlorate, [(nbp)(tren)Cu(II)](ClO4)2, 2 · 2ClO4, is reported. The salt crystallized in the monoclinic space group P21/n with a = 10.1453(5) ?, b = 17.5250(8) ?, c = 13.6021(6) ?, β = 100.737(19)° and V = 2376.06(19) ?3 with Z = 4. The structure contains copper(II) (nbp)(tren) cations, each with a distorted-trigonal-bipyramidal CuN5 coordination geometry, separated by perchlorate anions. The cations exhibit steric strain associated primarily with close
contacts between the methylene protons of the nbp ligand and one of the amine groups of the tren ligand. The strain has a
noticeable effect on the coordination geometry and certain physical properties of the complex.
Graphical Abstract In the title structure, steric strain in the (nbp)(tren)Cu(II) cations, associated with close contacts between protons of
the nbp ligand and two of the amine groups of the tren ligand (dashed lines in the figure below) affects certain physical
properties of the cation and is consistent with an anomalously long Cu(II)–N(pyrazole) distance (Cu–N41) and an unusually
large axial–equatorial angle, N41–Cu–N12.
相似文献
16.
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17.
Jian Li Zu-Pei Liang Cheng-Yun Wang Xi-Shi Tai 《Journal of chemical crystallography》2009,39(9):638-641
Abstract The title compound N-(2,3,4-trimethoxy-6-methylbenzylidene)-2-methyl-benzenamine (C18H21NO3, M
r = 299.36) was synthesized and characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. The crystal
belongs to monoclinic, space group P21/n, with a = 7.2804(5), b = 8.5909(9), c = 26.117(3) ?, β = 92.056(2)°, V = 1,632.4(3) ?3, Z = 4, D
c = 1.218 g cm−3, λ = 0.71073 ?, μ(Mo Kα) = 0.083 mm−1, F(000) = 640. The final refinement gave R = 0.0497, wR(F
2) = 0.1157 for 2,879 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the dihedral angle between the two phenyl rings is 25.9 (2)°. The molecule adopts
a trans configuration about the central C=N functional bond. The crystal structure is stabilized by C–H…O hydrogen bonds and π–π stacking interactions. The title compound possesses moderate antibacterial activity.
Graphical Abstract The title compound N-(2,3,4-trimethoxy-6-methylbenzylidene)-2-methyl-benzenamine (C18H21NO3, M
r = 299.36) was synthesized and characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. The crystal
belongs to monoclinic, space group P21/n, with a = 7.2804(5), b = 8.5909(9), c = 26.117(3) ?, β = 92.056(2)°, V = 1,632.4(3) ?3, Z = 4, D
c = 1.218 g cm−3, λ = 0.71073 ?, μ(Mo Kα) = 0.083 mm−1, F(000) = 640. The final refinement gave R = 0.0497, wR(F
2) = 0.1157 for 2,879 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the dihedral angle between the two phenyl rings is 25.9 (2)°. The molecule adopts
a trans configuration about the central C=N functional bond. The crystal structure is stabilized by C–H…O hydrogen bonds and π–π stacking interactions. The title compound possesses moderate antibacterial activity.
相似文献
18.
Vanessa Renee Little Hilary Jenkins Keith Vaughan 《Journal of chemical crystallography》2008,38(6):447-452
Abstract The crystal structures of methyl 4-{(E)-2-(4-methylpiperazino)-1-diazenyl}benzoate (2a) and 1,4-di[(E)-2-(2-nitrophenyl)-1-diazenyl]piperazine (3a) have been determined by single crystal X-ray diffraction analysis. The bis-triazene (3a) adopts an unusual pseudo-boat conformation in the piperazine ring, with a dihedral angle of 52.20(0.06)° between the two
planes defined within the piperazine ring. The crystal structures of 2a and 3a are compared with the structure of the triazene (4) and the closely related bis-triazene (5). The piperazine ring of 2a adopts a typical chair conformation, whereas the piperazine ring of 3a adopts an unusual boat conformation. Crystal data: 2a C13H18N4O2, monoclinic, space group P21
/n, a = 13.849(3) ?, b = 6.577(1) ?, c = 14.904(3) ?, α = 90°, β = 96.098(3)°, γ = 90° and V = 1,349.8(4) ?3, for Z = 4. 3a C16H16N8O4, triclinic, space group P-1, a = 7.6066(6) ?, b = 8.3741(7) ?, c = 14.507(1) ?, α = 78.673(1)°, β = 81.877(1)°, γ = 73.445(1)° and V = 865.0(1) ?3, for Z = 2.
Index abstract
The crystal structures of methyl 4-{(E)-2-(4-methylpiperazino)-1-diazenyl}benzoate (2a) and 1,4-di[(E)-2-(2-nitrophenyl)-1-diazenyl]piperazine (3a) have been determined by single crystal X-ray diffraction analysis. 相似文献
19.
Angela Tuzi Anna Andolfi Alessio Cimmino Antonio Evidente 《Journal of chemical crystallography》2010,40(1):15-18
Abstract
The X-ray crystal structure of phyllostin (8-hydroxy-3-methyl-2-oxo-2,3,4a,5,8,8a-hexahydro-benzo[1,4]dioxine-6-carboxylic acid methyl ester) is reported. Phyllostin was recently and for the first time isolated, together with phytotoxin phyllostoxin and the phyllostictines A–D, from the culture filtrates of Phyllosticta cirsii, a fungal pathogen isolated from diseased Cirsium arvense leaves and evaluated as biocontrol agent of this noxious perennial weed. Phyllostin crystallizes in the monoclinic space group P21 with unit cell parameters: a = 8.371(2), b = 7.026(1), c = 9.918(1) ?, β = 92.013(8)°, Z = 2. The final refinement converged to R1 = 0.0530 for 1026 observed reflections having I > 2σ(I). In the molecule two trans joined six-membered rings are present. The cyclohexene ring adopts a half-chair conformation. The 2-oxo-1,4-dioxan ring adopts a distorted half-chair conformation. The relative stereochemistry of the four chiral centers turns out to be 3R,4aS,8R,8aS. In the crystal packing molecules form infinite chains through O–H···O intermolecular hydrogen bonds. Chains run along the crystallographic a axis forming layers of molecules stacking in the [0 1 0] direction. 相似文献20.
The co-crystal structure of 2-t-butylphenol with 3-t-butylsalicylaldehyde (1) was obtained by single-crystal X-ray diffraction. 2-t-Butylphenol was co-crystallized with 1 equivalent of 3-t-butylsalicylaldehyde. The phase crystallizes in the monoclinic system with P21/c space group. The unit cell dimensions are a = 12.351(3) Å, b = 15.253(3) Å, c = 10.377(2) Å, β = 97.58(3)∘, V = 1937.8(7) Å3 and Z = 4. The structure of the crystal layered by nonpolar group includes strong intramolecular and weak intermolecular hydrogen bonds. The aldehyde oxygen O2 accepts a three-centered bond through intramolecular O1–H1A⋅sO2 and intermolecular O3–H3A⋅sO2 interactions. In addition, the crystal consists of right-handed helical (P) and left-handed helical (M) chains linked by hydrogen bonding. 相似文献