Dielectric Relations of Nematic 4-n-Heptylamino benzoic Acid in Mixtures with 4-Cyano benzoic Acid and 4-Fluoro benzoic Acid

Dielectric constants and the dielectric loss in the frequency range from 0.1–12 MHz were measured in the binary systems of 4-n-heptylamino benzoic acid with 4-cyano benzoic acid and 4-fluoro benzoic acid in the nematic phase. Not only the strong increase of dielectric anisotropy, but also the appearance of a Debye relaxation in the MHz range in both the mixtures proves the existence of the mixed associates. This model was proved by the temperature dependence of relaxation times and on chemical structure of the mixed associates, as well as, by the comparison with the measurements of one more binary system of acids.     

Etching of Anthracene Cleavages in Sulphuric Acid — Formic Acid Solutions

Crystal etching, though a simple and widely adopted technique for the study of imperfections in a wide variety of materials, the process is not very well understood. The etch pit shapes are controlled by a number of factors, such as, the composition of etchant, the period of etching, the temperature of etching and the symmetry of plane under study. This communication reports observations of etching the (001) cleavage planes of anthracene in sulphuric acid — formic acid mixtures.     

Propeller-like Conformation of Diphenylacetic Acid

Abstract Crystal structure of diphenylacetic acid has been solved by X-ray diffraction. The crystals are monoclinic, space group P2₁/c, with a = 12.254(4) ?, b = 7.2260(8) ?, c = 17.521(4) ?, β = 133.38(1)°, Mr = 212.24, V = 1127.6(5) ?³, Z = 4 and R = 0.045. A strong hydrogen bond links the molecules in dimers. The dimers are connected by weaker C–H···π and π···π interactions. A calculation was performed for the isolated molecule and for the dimer within the Hartree-Fock (HF) level with a 6-311G(d) basis set. In both calculations, the minimum of the energy is achieved with the phenyl rings assuming a more symmetric arrangement around the central carboxylic plane than is experimentally observed. Graphical Abstract In diphenylacetic acid the molecules are coupled in dimers by a strong hydrogen bonds. Weaker intermolecular interactions involving the aromatic ring π systems join the dimers together. Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Crystal Structure of a Metallohybrid Acid of 1,3,5-Benzenetricarboxylic Acid of Copper(II)

Abstract The crystal structure of a metallohybrid carboxylic acid obtained from the reaction of 1,3,5-benzenetricarboxylic acid (TCAH3) with copper(II)acetate monohydrate in the presence of pyridine (py) having composition Cu(py)₂(TCAH2)₂(H₂O)₂ [1] is reported. It crystallizes in triclinic space group P-1 and with a = 7.0110(3)?, b = 8.9523(5)?, c = 11.5370(5) ?, α = 79.776(3) °, β = 82.881(3)°, γ = 83.628(3)°, and V = 704.18(6)?³. The hydrogen bond in 1 is compared with the hydrogen bond pattern in the structure of 1,3-dicarbomethoxy 4,6-benzenedicarboxylic acid, which crystallizes in mononclinic space group P21/c and has unit cell parameters of a = 6.9549(16)?, b = 8.7676(15)?, c = 20.111(4)?; β = 92.585(17) ° and V = 1225.1(4) ?³. Index Abstract Crystal structure of a metallohybrid carboxylic acid obtained from the reaction of 1,3,5-benzenetricarboxylic acid with copper(II)acetate monohydrate in the presence of pyridine is determined and compared with hydrogen bond pattern present in the structure of 1,3-dicarbomethoxy 4,6-benzenedicarboxylic acid. Crystal structure of a metallohybrid acid of 1,3,5-benzenetricarboxylic acid of copper(II). Kusum Bania, Nilotpal Barooah, Rupam Sarma, Jubaraj B. Baruah     

Unusual Substitution in Hydrazinobenzoic Acid upon Complexation. Crystal and Molecular Structure of Hydrazinobenzoic Acid Hydrochloride

Crystallography Reports - The crystal and molecular structure of 2-hydrazinobenzoic acid was determined. In solution in the presence of copper(II) chloride, 2-hydrazinobenzoic acid is transformed...     

Deformation Phenomena in n-Pentadecanoic Acid Crystals

The formation of heat induced fracture-like patterns, slip-twin promoted deformation, some epitaxial relations are discussed in case of n-pentadecanoic acid crystals, grown from solutions, by solvent evaporation methods.     

Polymorphism in Caffeine Citric Acid Cocrystals

Journal of Chemical Crystallography - A second polymorph of an anhydrous 1:1 caffeine citric acid cocrystal (C8H10N4O2, C6H8O7) is reported. Crystals were analyzed using single crystal X-ray...     

Smectic C-to-Nematic Transition in p-n-Heptyloxybenzylidene-p-aminobenzoic Acid

The results on the phase transitions in p-n-heptyloxybenzylidene-p-aminobenzoic acid are reported. The microscopic and X-ray studies show that the compound goes over from smectic C to nematic phase directly. The transition entropies and specific heat are determined using differential scanning calorimetry. The translational order parameter is determined using low angle X-ray intensity measurements. The tilt angle in smectic C phase is found to be 56° and is independent of temperature. The X-ray data also lead to the conclusion that the compound exists as a dimer.     

有机非线性倍频晶体间硝基苯甲酸*二乙醇胺的研究

本文报道了间硝基苯甲酸(m-NBA)*二乙醇胺(DEA)单晶体在不同环境下的生长习性以及对该晶体形貌的影响.测定了该晶体及两种原料的红外光谱,同时讨论了晶体的差热分析、透光波段以及初步测定了晶体的二次谐波强度.     

Crystal Forms of the Antiepileptic Lamotrigine: Molecular Salts and Solvates with Fluorobenzoic Acid,Nicotinic Acid, 2-Thiobarbituric Acid, 3-Picoline and Butyl Alcohol

Abstract  

The crystal structures of three salts and two solvated multicomponent crystals of lamotrigine with 4-fluorobenzoic acid, nicotinic acid, 2-thiobarbituric acid, 3-picoline and butyl alcohol are reported. Compound 1a crystallizes in monoclinc system, space group P2₁ with a = 13.3860(5) ?, b = 8.3420(3) ?, c = 15.5200(6) ?, β = 93.524(1)°, V = 1729.78(11) ?³, and Z = 2. Compound 1b crystallizes in monoclinic system, space group P2₁/c with a = 10.6625(7) ?, b = 16.2575(11) ?, c = 13.6346(9) ?, β = 100.904(1)°, V = 2320.8(3) ?³, and Z = 4. Compound 1c crystallizes in triclinic system, space group P[`1] \overline{1} , with a = 10.1309(7) ?, b = 12.0260(8) ?, c = 14.0826(10) ?, α = 71.783(1)°, β = 86.451(1)°, γ = 80.902(1)°, V = 1609.10(19) ?<sup>3</sup>, and Z = 1. Compound 1d crystallizes in monoclinic system, space group P2<sub>1</sub>/c with a = 14.9570(10) ?, b = 8.0230(6) ?, c = 13.8162(10) ?, β = 102.884(1)°, V = 1616.2(2) ?<sup>3</sup>, and Z = 4. Compound 1e crystallizes in triclinic system, space group P[`1] \overline{1} , with a = 7.5710(6) ?, b = 8.5721(7) ?, c = 13.5532(11) ?, α = 85.364(1)°, β = 79.632(1) (1)°, γ = 86.188(1)°, V = 861.19(12) ?³, and Z = 2. Characteristic R₂²(8) dimer is observed in all five structures. A complete hydrogen bonded motif analysis is described. Lamotrigine-lamotrigine base pair is observed in all the structures, except in (1b). In (1c), the R₂²(7) dimer is noticed while, in all other structures R₂²(8) dimer exist between the lamotrigine-lamotrigine base pair. In all the six structures, chlorine atoms of the lamotrigine molecules are not involved in any interactions.     

Optical Anisotropy of Dodecyl Benzene Sulfonic Acid

The order parameters of a number of novel 2-aryl-l,4-naphthoquinone dyes dissolved in a mixed cyanobiphenyl-terphenyl nematic liquid crystal system (Type E43, B.D.H. Chemicals Ltd.) have been determined. Observed values range from 0.80 to 0.09, and can be interpreted qualitatively by consideration of the w-dipole moment and transition moment directions of the dyes calculated by the PPP-SCF-CI MO method.     

Assembly of Dipicolinic Acid by Alkali-Metal Cations

Abstract  

Different types of structures of hydrogen-bond assemblies derived from partially deprotonated dipicolinic acid (LH2) molecules having alkali metal cation such as sodium, potassium and cesium are structurally characterised. These self assembled complexes have general formula [M(LH)(LH2)(H₂O) _m ] _n xH₂O {m = 2, 3, n = 1, 2, n, and x = 0, 0.5 M = Na (1); K (2) and Cs(3)}. Sodium complex is a hepta-coordinate mononuclear complex; potassium complex is octa-coordinate complex with dinuclear K₂O₂ type of carboxylate core; whereas the cesium complex is nona-coordinate polymeric complex. All these complexes crystallises in Triclinic, P-1 space group. Sodium complex has a = 6.9003(4) ?; b = 11.1440(6)?; c = 11.2059(5)?; α = 85.695(4)o; β = 82.103(3)o; γ = 87.432(4)o and volume = 850.60(8) ?³ Z = 2; Potassium complex has a = 7.0937(4)?; b = 11.0034(5)?; c = 11.2732(6)?; α = 91.603(3)o; β = 96.088(3)o; γ = 97.207(4)o; volume = 867.29(8) ?³; Z = 1 and cesium complex has a = 7.1410(6)?; b = 11.0625(8)?; c = 12.0667(9)?; α = 96.849(4)o; β = 93.850(4)o; γ = 105.495(4)o; volume = 907.14(12) ?³; Z = 2.     

Intermolecularly Associated Carboxylic Acid Dimers in the Supramolecular Assembly of (R)-1,4-Benzodioxane 2-Carboxylic Acid

Abstract  The title compound, C₉H₈O₄, (I), crystallizes in the monoclinic space group P 21/c with unit cell parameters a = 7.3380(5) ?, b = 9.3790(7) ?, c = 12.3172(9) ?, β = 90.687(7)°, Z = 4. The molecule consists of a benzene ring fused to a 1,4 dioxane ring in a half-chair conformation with a carboxylic acid group bonded at the dioxane 2-position. The carboxylic acid group forms a classic O–H···O hydrogen bonded dimer with an O···O distance of 2.6292(12) ? in a R₂² (8) graph-set motif which links the molecules into pairs around inversion centers in a supramolecular assembly in the unit cell. The dihedral angle between the mean planes of the R₂² (8) graph-set motif’s of two adjacent dimers in the unit cell is 75.7(5)°. The mean plane of an R₂² (8) graph-set motif makes an angle of 88.4(5)° with the mean plane of the benzene ring in the same dimer and 13.1(2)° or 13.4(7)° with the mean plane of a benzene ring from an adjacent dimer. Additional weak Cg π-ring intermolecular interactions significantly influence the bond distances, bond angles and torsion angles of the dioxane ring and attached carboxyl group. Comparison to a MOPAC AM1computational calculation provides support to these observations. Graphical Abstract  The association of carboxylic acid dimers in the supramolecular assembly of (R)-1,4-benzodioxane 2-carboxylic acid is investigated by examination of its crystal structure. Its geometric and packing parameters are described and compared to a MOPAC AM1 computational calculation. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Solid State Structures of Anhydrous 1-Aminoethylidenediphosphonic Acid

Abstract  

The 1-aminoethylidenediphosphonic acid (AEDPH₄) is anhydrous when it is synthesized according to the U.S. Patent 4239695. It crystallizes in water to form hydrous crystal AEDPH₃·H₃O (1). With the help of a simple low-temperature, low-pressure hydrothermal method and template 2,2′-bidpyridyl (2,2′-bipy), single crystals with the same structure of the anhydrous AEDPH₄ (2) is obtained. Compound 2 were characterized by elemental analysis (EA), infrared spectrometry (IR), thermogravimetric analysis (TGA) and X-ray single crystal diffraction. In compounds 2, the AEDPH₄ molecules are linked into 3D supramolecules by various hydrogen bonds.     

乙醇萃取酸性氧化石墨烯的研究

以改进的氧化还原法(Hummers法)制备的氧化石墨烯为原料,采用乙醇萃取法过滤酸性氧化石墨烯溶液使其恢复至中性.对比分析了与以往采用水剂法进行清洗的效果,并且进一步考察了乙醇浓度以及温度对萃取过程的影响.采用Zeta电位、场发射扫描电镜、X射线衍射仪以及pH值检测和重溶情况对萃取效果进行了表征和判断.试验结果表明:乙醇萃取法可以大大缩短酸性氧化石墨烯溶液恢复至中性的时间并且不改变其本身性能;当氧化石墨烯溶液浓度为1 mg·mL-1和0.5 mg·mL-1时,分别加入浓度为40; v/v和95; v/v乙醇,温度为60℃是最佳的萃取选择.