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1.
Molecular and crystal structure of N-(6-methoxybenzothiazol-2-yl)-1-(4-fluorophenyl)-O,O-dipropyl-α-aminophosphonate, C21H26FN2O4PS, have been determined by single-crystal X-ray diffraction study. The title compound is tetragonal, with a = 21.35(3) Å, c = 20.16(5) Å, Z = 16, D x = 1.308 Mg/m3, μ(MoKα) = 0.247 mm?1, and space group is I41/a. The structure was solved by direct method and refined to a final R = 0.0687 for 2370 reflections with I > 2σ(I). The compound shows a fully delocalized benzothiazole system with a sp2 hybridization of the N(2). There is a strong intermolecular hydrogen bond between P=O and NH. The crystal structure is stabilized by a strong intermolecular N–H?sO hydrogen bond. 相似文献
2.
Abstract
The synthesis and Crystal structure are given for the bis (N,N,N′,N′-tetramethylethylendiammonium) octaiodo pentachloroantimonate (III) salt. An X-ray investigation has shown that the title compound crystallizes in a monoclinic system, space group P21/m with the following lattice parameters a = 9.786(2) Ǻ, b = 14.024(5) Ǻ, c = 14.336(3) Ǻ, β = 91.35(2)° and Z = 2. The structure was solved from 3085 independent reflections with R 1 = 0.0402 and wR 2 = 0.0952 and refined with 152 parameters. The structure shows a layer arrangement perpendicular to the [(b)\vec] \vec{b} -axis: planes of [SbCl5]2−, I3 − and I5 − anions alternate with planes of [(CH2)2(NH(CH3)2)2]2+ cations. The [SbCl5]2− square pyramids present an active lone electron pair (LEP) on the Sb atoms and they are interconnected by means of N–H···Cl hydrogen bond originating from [(CH2)2(NH(CH3)2)2]2+ entities. The polyiodides (I3 − and I5 −) anions form a planer zigzag polymeric chains via I···I linking interactions. These chains are linked to the [SbCl5]2− anions by a long range contact. 相似文献3.
Abstract The salt tris-(N–N dimethyl benzylammonium)-hexachlorobismuthate(III) crystallizes in the triclinic system P1 with unit cell parameters: a = 9.0300(12), b = 9.9220(3), c = 19.575(2) ?, α = 79.955(5), β = 89.952(2), γ = 88.108(6)°, V = 1726.0(3) ?3, Z = 2. The examination of the structure shows an alternate stacking of inorganic layers of hexachlorobismuthate(III) anions
and organic layers of [C6H5CH2NH(CH3)2]+ cations parallel to the a-axis. The cohesion forces of the packing of N–N dimethyl benzylammonium units in the layer and between two adjacent layers are provided by hydrogen bonds (N–H⋯Cl) and van
der Waals contacts.
Index Abstract The examination of the structure shows a layer arrangement parallel to the a-axis: planes of octahedral anions [BiCl6]3− alternate with planes of [C6H5CH2NH(CH3)2]+ cations (Fig. 3). The cohesion forces of the packing of the N–N dimethyl benzylammonium units in the layer and between two adjacent layers are provided by hydrogen bonds (N–H⋯Cl) and van
der Waals contacts.
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
4.
Liang Xian Jing Zhao Ming Cheng Lianhua Zou Guangliang Wang 《Journal of chemical crystallography》2009,39(8):612-614
Abstract
N-p-bromophenyl-N′-phenylacetylthiourea was characterized by elemental analysis, IR and 1H NMR etc. Single crystal structure of the title compound was determined on X-ray diffraction instrument. The title compound
crystallizes in monoclinic space group c2/c, with a = 21.442(5) ?, b = 12.208(2) ?, c = 11.955(2) ?, β = 109.375(4)°, and D
calc = 1.571 g/cm3 for Z = 8. An intermolecular hydrogen bond N–H···S which links two thiourea molecules as a dimer and an offset face-to-face π–π
stacking interaction were observed in the title compound. The strong non-covalent interaction influences the conformation
and property of thiourea derivatives.
Index Abstract The title compound, N-p-bromophenyl-N′-phenylacetylthiourea, was synthesized by the treatment of phenylacetyl chloride with 4-bromoaniline and its crystal structure
determined. Single crystal X-ray diffraction analysis reveals that hydrogen bonds and face-to-face π–π stacking interactions
have strong influence on the conformation and molecular stacking of the title compound.
相似文献
5.
K. Padayachy M. A. Fernandes H. M. Marques A. S. de Sousa 《Journal of chemical crystallography》2008,38(8):577-582
Abstract The title compound N,N′-bis(p-tolylsulfonyl)diethylenetriamine (1) was synthesized and its crystal structure determined by X-ray diffraction. Adjacent molecules of 1, symmetrically related through a c-glide, are linked by alternating hydrogen bonds that form molecular chains along [0 0 1]. Two molecular chains occur in each
unit cell and pack to form alternating layers in a three-dimensional supramolecular structure. The compound crystallizes in
the Pca21 space group stabilized by the inclusion of solvent dichloromethane molecules in structural voids between molecules of 1. The dichloromethane molecules are related through a twofold screw rotation axis and are not disordered.
Index Abstract Intermolecular hydrogen bonds involving sulfonamide moieties of title compound afford a supramoleular structure that accommodates
the inclusion of dichloromethane in alternating layers.
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6.
Sodium borohydride reduction of E-3-benzylidenechromanone epoxides in dry methanol has afforded 3(S*), 4(S*)-dihydroxy-3-[α(R*)-methoxybenzyl]chromans as an interesting class of products, the structures of which have been assigned mainly from spectral data and consideration of the mechanistic aspects. X-ray diffraction study of one of them, 3-[4-bromo-α(R*)-methoxybenzyl]-6-chloro-3(S*),4(S*)- dihydroxychroman, is performed. The title compound crystallizes in the monoclinic sp. gr. P21/n, with a = 13.336(6) Å, b = 10.866(5) Å, c = 27.166(11) Å, β = 95.193(6)°, V = 3920(3) Å3, and Z = 8. Supramolecular construction of the compound involves O–H···O intermolecular hydrogen bonds as well as three other types of non-covalent interactions which are responsible for crystal packing. Density functional theory was applied for geometry optimization, molecular orbital calculations, and prediction of UV spectral features. The geometric parameters (bond lengths, bond angles, and dihedral angles) for the representative compound obtained from density functional theory with B3LY6-31G basis set were in good agreement with experimental values. 相似文献
7.
Miyako Hisamoto Swarup Chattopadhyay Juergen Eckert Guang Wu Susannah L. Scott 《Journal of chemical crystallography》2009,39(3):173-177
Abstract The structure of cis-(CH3)2Au(O,O′-acac) was investigated by single-crystal X-ray diffraction. It crystallizes in the orthorhombic space group Cmca with unit cell dimensions a = 6.7831(13) ?, b = 15.080(3) ?, c = 18.073(3) ? and α = β = γ = 90°. The molecule is planar but lacks a C2 axis in the solid-state, with two Au–C bond lengths that differ by 0.078(21) ? due to crystal packing effects. The inequivalence
of the crystallographic carbon positions is evident in the solid-state 13C CP-MAS NMR spectrum, which was recorded at low temperature due to the thermal sensitivity of the compound during magic-angle
spinning. Head-to-tail stacking, which creates short intermolecular paths, was reproduced computationally in a dimer model.
Graphical Abstract
Solid-state Spectroscopic and Structural Investigation of
cis
-(CH
3
)
Au
2
(
O
,
O
′-acac)
Miyako Hisamoto • Swarup Chattopadhyay • Juergen Eckert • Guang Wu • Susannah L. Scott
In the solid state, cis-(CH3)2Au(O,O′-acac) has no C2 axis, two different Au–C bond lengths (1.960, 2.038 ?; Δd = 0.078(21) ?) and a close Au–C…C–Au contact; these features give rise to additional features in the 13C CP-MAS NMR spectrum. 相似文献
8.
Fiona N.-F. How Karen A. Crouse M. Ibrahim M. Tahir David J. Watkin 《Journal of chemical crystallography》2009,39(12):894-897
Abstract
S,S′-(Naphthalen-2-ylmethyl sulfanyl (1-p-tolyl-ethylidene) hydrazine (SNM4MA) was prepared by the condensation of S-napthalen-2-ylmethyldithiocarbazate (SNMDTC) and 4-methylacetophenone. Yellow needles of SNM4MA were obtained upon slow evaporation of a 50:50 mixture of acetonitrile and DMSO over a period of weeks. The compound crystallizes in the monoclinic system with the space group C 2/c and Z = 4. The unit cell parameters are a = 7.0221(2) ?, b = 22.8428(6) ?, c = 23.5127(6) ? with β = 94.0222(13)°. Single crystal X-ray analysis shows that the molecule has crystallographic two-fold rotational symmetry coincident with the S–S bond. The title compound exists as a trans–cis conformer in which the naphthalene group is trans with respect to the thione sulfur while the benzyl group adopts a cis geometry. 13C and 1H spectra confirm that the dimeric nature is retained in DMSO solution. 相似文献9.
Abstract The crystal structure of N′-(6-chloropyridin-3-formyl)-N-t-butyl urea, C11H14ClN3O2, has been established, and which belongs to monoclinic crystal system, space group Pn with unit cell dimensions a = 9.335(3) ?, b = 12.715(3) ?, c = 21.813(6) ?, β = 95.417(6)°, V = 2577.6(12) ?3 and Z = 8. An intramolecular N–H···O hydrogen bond forms a six-membered ring in the central part of the molecule. Both two N–H
atoms of single unit participate in intermolecular hydrogen bonds and an intramolecular hydrogen bond, respectively.
Index Abstract The crystal structure ofN′-(6-chloropyridin-3-formyl)-N-t-butyl urea, C11H14ClN3O2, has been established, and which belongs to monoclinic crystal system withZ = 8, space group Pn.
相似文献
10.
N. Raouafi M. Freytag P. G. Jones M. L. BenKhoud 《Journal of chemical crystallography》2007,37(6):381-386
N-(1H-Benzimidazol-2-yl) propionimidic acid ethyl ester (1) reacts with benzylamine to yield the corresponding N-(1H-Benzimidazol-2-yl)-N′-benzyl proponamidine (2). The structure and conformation of the amidine 2 were determined by 1H and 13C NMR and X-ray diffraction. The product crystallizes in monoclinic system with space group P21/c, a = 10.7913 ?, b = 15.5164 ?, c = 9.1130 ?, β = 108.378° and Z = 4. In the crystal there are two N–HN hydrogen bonds, the first is intramolecular H-Bond links H4 to N1; the second one is intermolecular and it links H2 to N3
of a second molecule leading to inversion-related dimers. The X-ray results were compared with those obtained by semi-empirical and ab-initio calculations. 相似文献
11.
Xiao-Ping Rao Yong Wu Zhan-Qian Song Shi-Bin Shang 《Journal of chemical crystallography》2010,40(4):328-331
Abstract
The title compound (C46H72N4O2, M r = 713.08) [systematic name: 1-isopropyl-3-((1R,4aS,10aR)-7-isopropyl-1, 4a-dimethyl-1,2,3,4,4a,9,10,10a-octahydrophenanthren-1-yl)urea] is a new derivative of dehydroabietic acid. It crystallized in the orthorhombic system, space group P2121 21 with cell dimensions of a = 9.5950(19) ?, b = 18.740(4) ?, c = 24.654(5) ?, V = 4,433.0(16) ?3, Z = 4, D c = 1.068 g/cm3, λ = 0.71073 ?, μ = 0.07 mm−1, F(000) = 1,568, final R = 0.0777 and wR = 0.1731 for 2,048 observed reflections with I > 2σ(I). Two crystallorgraphically independent molecules with different conformations co-exist in the structure. Each molecule exhibit classic tricyclic hydrophenanthrene structure, the two cyclohexane rings form a trans ring junction with chair and half-chair conformations, respectively. The crystal is stabilized by intermolecule hydrogen bonds and the molecules are in a head–tail zigzag arrangement. 相似文献12.
Methyl E(Z)-4,7 anhydro-5-benzamido-6,8-di-O-benzoyl-2,3,5-trideoxy-d-allo-oct-2-enoate have been synthesized like intermediates and isolated as single crystals during the synthesis of pyrazole-related C nucleosides as synthetic product with cytotoxic activity.1 Crystal structures of E(Z) isomers were determined by X-ray analysis. E isomer crystallizes in the triclinic crystal system, space group P1, a = 5.319(1) Å, b = 10.758(2) Å, c = 12.229(2) Å, α = 72.38(2)∘, β = 89.97(2)∘, γ = 87.07(2)∘, Dx = 1.320 Mgm−3 and Z isomer in the orthorhombic crystal system, space group P212121, a = 5.1297(13) Å, b = 19.667(5) Å, c = 25.871(6) Å, Dx = 1.348 Mgm−3. The molecular structure was solved by direct method on the basis of 2609 and 2727 unique reflections recorded at the temperature 293 K (E-isomer) and 173 K (Z-isomer) up to the final R-factor 0.0378 and 0.0435, respectively. C–H⋅sO contact networks were analyzed and the correlation established between the existence of the weak C–H⋅sO hydrogen bonds and the melting point of the single crystals. 相似文献
13.
The structure of the title compound bis-(1-tert-butyl-1,2-dibenzoylhydrazine)-N,N- sulfide was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic, space group P2(1)/c with the following crystallographic parameters: a = 14.681(7) Å, b = 14.501(7) Å, c = 16.535(8) Å, = 90°, = 109.173(9)°, = 90°, V = 3325(3) Å 3, z = 4, Dx = 1.244 mg/m3, F(000) = 1320, T = 293(2) K, 1.47° 25.00°, the final R factor: R1 = 0.0584, wR2 = 0.1111. The bond distances and angles in the tert-butyl groups are different, that can interpret its 1H NMR spectra, which are very unusual for the absorption of –CMe3 being multiple. 相似文献
14.
Abstract 20-O-β-d-glucopyranosyl-20(S)-protopanaxadiol (I) has been isolated as a metabolite of ginseng saponins by Paecilomyces
bainier. The crystal structure of (I) was also investigated by single crystal X-ray diffraction analysis. It crystallizes in the monoclinic space group P21, with a = 15.99 2 (3) ?, b = 11.960 (19) ?, c = 20.127 (3) ?, β = 101.85 (4)°, and V = 3767.5 (11) ?3, Z = 4, R
int = 0.1129, ωR(F
2) = 0.1749, F(000) = 1,448. The title compound is a dammarane-type triterpenoid, and the four rings of this compound connect with each
other in trans characteristics,with the three-six-membered rings in chair conformation and the five-membered ring adopting envelope one. A β-d-glucopyranosyl group and a 2-methyl-2-pentenyl group connect to C20 of S configuration. The space symmetrical motif is adopted and each packing unit-cell contains two symmetrical compound (I) molecules and four H2O molecules. The hydrogen-bonding (both intra- and inter-molecular) interactions play a major role in this structural association.
Index Abstract In the present paper, the single-crystal structure of 20-O-β-d-glucopyranosyl-20(S)-protopanaxadiol was determined by X-ray analysis 相似文献
15.
The processes of oxygen diffusion in La2 ? x Sr x CuO4 ? δ phases have been simulated for the first time by the molecular-dynamics method. Calculations were performed for the temperature range 300–2500 K. The behavior of the radial pair correlation functions, which characterize the degree of order of O1 ions in CuO2 layers, indicates that O2? anions form a weakly correlated subsystem within a CuO2 layer. To quantitatively confirm the conclusions about the predominantly two-dimensional character of ion transport and different mobilities of O1 and O2 particles in the cuprates under study, the pair oxygen diffusion coefficients in the La2 ? x Sr x CuO4 ? δ lattice were calculated. It is shown that oxygen diffusion occurs through the conventional hopping mechanism mainly in CuO2 layers; correspondingly, the diffusion coefficient for equatorial ions (O1) exceeds that for apical oxygen anions (O2) by an order of magnitude. The motion of oxygen anions was traced at the microscopic level through analysis of the particle transport trajectories. It has been proven for the first time that diffusion of O1 ions in the ab plane in a nonstoichiometric LaSrCuO3.61 sample occurs through jumps to the nearest position or along CuO2 layers; in a more complicated way, it may occur through unoccupied O2 lattice sites. 相似文献
16.
Dmitri V. Sevenard Olesya Kazakova Ralf-Matthias Schoth Enno Lork Gerd-Volker Röschenthaler 《Journal of chemical crystallography》2011,41(12):1795-1799
Abstract
The crystal structures of 2,5-bis(trifluoroacetyl)cyclohexane-1,4-dione (1) and o,o′-bis(trifluoroacetyl)-p-cresol (2) is reported. The first compound crystallizes in monoclinic space group P21/n with a = 6.5040(10), b = 10.1610(10), c = 8.2420(10) ?, β = 91.690(10)° and V = 0.54445(12) nm3. Double enolization (U-structure) with a considerable electron density delocalization in the enolone backbone was established in this case. Phenol 2 crystallizes in triclinic space group P-1 with a = 7.0690(10), b = 9.4890(10), c = 9.8190(10) ?, α = 103.720(10), β = 110.760(10), γ = 102.150(10)° and V = 0.56598(12) nm3. In contrast to CDCl3 solution, a “bifurcate” structure of 2 with jumping OH proton is quenched: only one of both trifluoroacetyl moieties is bonded by intramolecular hydrogen bond. 相似文献17.
Zedong?Dong William?W.?Brennessel Brian?E.?Padden Steve?A.?Schroeder Indra?Prakash Ihab?Bishay Victor?G.?YoungJr. Eric?J.?MunsonJr. David?J.?W.?Grant
The hydrolysis product of neotame, N-(3,3-dimethylbutyl)-l--aspartyl-l-phenylalanine (DMBAP), was crystallized from water as an anhydrate with a melting point at 197C with decomposition. Its crystal structure was determined by single crystal X-ray diffractometry. The crystal is orthorhombic with space group P212_121 with Z=4 and one molecule per asymmetric unit. The cell constants are a=5.520 (2) Å, $b=10.608$ (5) Å and c= 31.92 (2) Å. The 13C solid-state nuclear magnetic resonance spectrum of DMBAP is compared with those of neotame monohydrate and neotame methanol solvate. 相似文献
18.
Heng-Shan Dong Yan-Fei Wang Hong-Ru Dong Bin Wang Bin Quan 《Journal of chemical crystallography》2009,39(2):91-94
Abstract The N,N′-bis[1-(4-methoxyphenyl)-5-methyl-1H-1,2,3-triazole-4-carbonyl]hydrazide 6 was synthesized from aryl triazole acids and its structure is established by MS, IR, and 1H NMR spectral data. Compound 6, C22H22N8O4, Mr = 462.48, crystallizes in the monoclinic space group P2(1)/c with unit cell parameters a = 15.3451(8), b = 8.6486(4),
c = 16.8502(9) ?, α = 90.00, β = 95.731(2), γ = 90.00o, V = 2225.1(2) ?3, Z = 4, and Dx = 1.381 mg m−3. The final R was 0.0450. The four aromatic rings are close to linear because of N···H–N hydrogen bonds.
Index Abstract Synthesis and crystal structures of N,N′-bis[1-(4-methoxyphenyl)-5-methyl-1H-1,2,3-triazole-4-carbonyl]hydrazide
Heng-Shan Dong, Yan-Fei, Wang, Hong-Ru Dong, Bin, Wang, Bin Quan
N,N′-Bis[1-(4-methoxyphenyl)-5-methyl-1H-1,2,3-triazole-4-carbonyl]hydrazide was synthesized.
相似文献
19.
The structural and transport characteristics of an Ag1 ? x Cu x I(0 < x < 0.25) solid solution have been simulated by the molecular-dynamics method. It is found that the cation diffusion coefficient decreases with increasing copper concentration; this correlation is in agreement with the experimentally observed decrease in ionic conductivity. It is shown that the cationic transport in disordered Ag1 ? x Cu x I phases is mainly due to the migration of silver cations, whereas the mobility of copper cations is much lower. Cu+ cations are found to reside in the 8c positions in a bcc cell; this finding suggests the existence of nanoscale α-CuI regions. 相似文献
20.
I. R. Amiraslanov N. A. Alieva G. G. Guseinov G. M. Agamirzoeva 《Crystallography Reports》2017,62(2):210-214
The Сu2Te compound has been synthesized by alloying Сu and Te taken in stoichiometric ratios. A Сu2Te sample has been homogenized by annealing at 773 K for 100 h. A pure copper phase in the form of thin filaments is found to segregate from the synthesized product (4 g) by the end of annealing. It is established by X-ray diffraction analysis that the copper-deficient sample is crystallized into the trigonal system with lattice parameters а = 8.328(1) Å, с = 7.196(1) Å, V = 432.2(1) Å3, sp. gr. \(P\overline 3 m1\), Z = 8. The crystal structure is determined and the sample composition Сu2–m Te (m = 0.25) is refined by the Rietveld method. The three independent copper atoms in the lattice are found to have different coordination numbers: 3, 4, and 5. 相似文献