Electronic Properties,Reactivity, Flexibility,Polarity, Thermodynamic Properties,and Dynamic Simulation of a Series of Hybrid Organic–Inorganic Polyoxoselenomolybdate Compounds

Crystallography Reports - A large theoretical study of three hybrid inorganic-organic polyoxoselenomolybdate-based systems (C7H10N)4[Se2Mo5O21]⋅5H2O (1), (C6H8N)4[Se2Mo5O21]⋅7H2O (2)...     

Growth from Solutions,Structure, and Spectral–Luminescent Properties of Crystalline Films of Di-n-hexyl-para-quaterphenyl

Crystallography Reports - The results of studying the growth and structure of crystalline films of para-quaterphenyl derivative with terminal n-hexyl...     

Inclusion compounds of N,N,N′,N′-tetracyclohexylfumaride with isomers of cresol and water

The crystal structures and thermal analyses of the host compound, N,N,N,N-tetracyclohexylfumaride, witho-cresol,p-cresol and water are reported and compared to that of them-cresol complex previously reported in an attempt to elucidate the reasons for host selectivity.     

Synthesis,structure, spectroscopic investigations,and computational studies of optically pure β-ketoamide

Chemical preparation, X-ray single crystal diffraction, IR and NMR spectroscopic investigations of a novel nonlinear optical organic compound (C₁₇H₂₂NO₂Cl) are described. The compound crystallizes in the orthorhombic system with the non-centrosymmetric sp. gr. P2₁2₁2₁. In the crystal structure, molecules are interconnected by N–H…O hydrogen bonds forming infinite chains along a axis. The Hirshfeld surface and associated fingerprint plots of the compound are presented to explore the nature of intermolecular interactions and their relative contributions in building the solid-state architecture. The molecular HOMO–LUMO compositions and their respective energy gaps are also drawn to explain the activity of the compound. The first hyperpolarizability β_tot of the title compound is determined using DFT calculations. The optical properties are also investigated by UV–Vis absorption spectrum.     

Inclusion compounds of N,N,N′,N′-tetraisopropylfumaride with isomers of methyl phenol and water

The crystal structures and thermal analyses of the host compound, N,N,N,N-tetraisopropylfumaride, witho-cresol,m-cresol and water are reported and compared to that of thep-cresol complex previously reported in an attempt to elucidate the reasons for host selectivity.     

Structure of azadirachtin-I, 11 β-H epimer

The 11 -H epimer of Azadirachtin-I, isolated from the seed kernels of Azadirachta indica A. Juss (Neem), was characterized by both NMR and X-ray crystallographic techniques. NMR data reveals that the H11 proton is in -orientation and the X-ray studies confirm this observation. The compound crystallized in space group P2₁ with the cell parameters a = 11.933(2) Å, b = 7.752(5) Å, c = 17.241(9) Å, = 106.80(3). Though the structural features are similar to the 11 -H epimer of Azadirachtin-H, the orientation of the acetoxy group at C3 is different. The dihedral angle C9–C8–C14–O13, which describes the relative orientation of the modified decalin and modified furan moities of the molecule, is 23.3(8).     

Crystal structure of 14, α-hydroxy,sandarocopimar-7, 15-diene-19-oic acid

C₂₀H₃₀O₃, M _r =318.46, Monoclinic,P2₁,a=12.232(2) ,b=11.491(2) ,c=14.160(3) , =115.2°(3),V=1800.3(7) ³,Z=4,D _x =1.18 Mg m^–3, (CuK)=1.5418 , =5.3 cm^–1,F(000)=696,T=298 K. FinalR=0.044 for 2645 reflections withI>2. The two crystallographically independent molecules in the unit cell adopt essentially similar conformations. The structure reveals atrans relationship between the hydrogen at C(9) and the methyl group at C(20). The stereochemistry at C(13) is S. Apart from van der Waals forces the structure is stabilized by hydrogen bonds.     

Synthesis,Crystal Structure,Antioxidant, and α-Glucosidase Inhibitory Activities of Methoxy-substituted Benzohydrazide Derivatives

Eight methoxy substituted at the benzylidene moiety benzohydrazide derivatives [R = 2-OCH₃ (1), 3-OCH₃ (2), 4-OCH₃ (3), 2,3-(OCH₃)₂ (4), 3,4-(OCH₃)₂ (5), 2,4,5-(OCH₃)₃ (6), 2,4,6-(OCH₃)₃ (7), and 3,4,5-(OCH₃)₃ (8)] were synthesized and characterized by ¹H NMR, FT-IR and UV-Vis spectroscopy. The crystal structure of 4 was determined by single crystal X-ray diffraction (sp. gr. Pbca, Z = 8). The molecule is slightly twisted with the dihedral angle between the two phenyl rings being 9.33(14)°. The methoxy group at the ortho position is twisted [C–O–C–C angle is–109.2(3)°] whereas the other at meta position is co-planar with the attached benzene ring. In the crystal packing, the molecules are linked into two-dimensional network parallel to the (001) plane by O–H···O, O–H···N, and N–H···O hydrogen bonds. Compounds 1–8 were evaluated for an antioxidant and α-glucosidase inhibitory activities and the results suggested that the ?OCH₃ substituent was ineffective for bioactivity enhancement.     

Synthesis of Sulfonated Cholesterol Derivatives—Electrical,Thermal, and Optical Properties

Poly(cholesterylacrylatesulfone) (PCHAS) and poly(cholesterylacrylatesulfone-co-1-hexene)s (PCHASHs) at different ratios are synthesized from the monomer cholesteryl acrylate. The liquid crystalline phases are observed under a hot stage fitted with a polarizing optical microscope. The polysulfone and copolysulfones are characterized by FT-IR, ¹H-NMR, DSC, and TGA techniques. From SEM (EDX) the qualitative amounts of elemental sulfur found in PCHAS and PCHASH11 are 2.90 weights (%) and 4.39 weights (%), respectively. The GPC data using THF as the solvent shows that the number average molecular weight of the PCHAS is 5268 g/mol and the molecular weights of the PCHASHs are higher than the PCHAS.     

Synthesis,NMR, and X-ray crystallographic determination of the absolute configuration of 4,6-O-ethylidene-2,3-di-O-methanesulfonyl-α-d-glucopyranosyl chloride

The synthesis, NMR spectra and crystal structure of 4,6-O-ethylidene-2,3-di-O-methanesulfonyl--d-glucopyranosyl chloride are reported. The chloro substituted carbohydrate, C₁₀H₁₇ClO₉S₂, crystallizes in the monoclinic space group.,P2₁, witha=10.124(4),b=9.517(4),c=18.058(8) Å and =105.18(1)°. FinalR=0.0434. There are two independent molecules in the asymmetric unit with conformations that differ around the mesyl (–S(O)₂CH₃) groups.     

Preparation of New Inorganic—Organic Layered Compounds,Hydroxy Double Salts,and Preferential Intercalation of Organic Carboxylic Acids into Them

Abstract

New inorganic—organic layered compounds were prepared by ion-exchange reactions of zinc-nitrate and copper-nitrate HDSs with organic carboxylic acids whose interlayer spacings increased depending on the sizes of carboxylic acids. The amounts of ion-exchanged 2-naphthoic acid and 2,6-naphthalene dicarboxylic acid were larger than those of 1-naphthoic acid and 2, 7-naphthalene dicarboxylic acid, respectively, indicating the molecule recognition ability of the HDSs.     

Experimental determination of the solid–liquid equilibrium,metastable zone,and nucleation parameters of the flunixin meglumine–ethanol system

Measurements of the metastable zone and solubility for flunixin meglumine–ethanol system were obtained. The solubility was measured within the temperature range from 288.15 to 328.15 K. The mole fraction solubility was correlated satisfactorily with the temperature by the equation: x_eq=2.35×10^?12e^0.07121T. The value of enthalpy of dissolution, enthalpy of fusion and enthalpy of mixing were determined to be 49.04, 64.03 and ?14.99 kJ mol^?1 respectively. The metastable zone width of flunixin meglumine was measured by an electric conductivity method. A comparison of the nucleation temperatures from electric conductivity measurement and from focused beam reflectance measurement (FBRM) shows that both detection techniques give almost the same results for flunixin meglumine. The nucleation parameters of flunixin meglumine in ethanol were determined from the metastable zone data. Over the equilibrium temperature range from 312.28 to 325.55 K, the nucleation rate constant was varied from 0.00001 to 0.00120 #/m² min, whereas the nucleation order was varied from 2.23022 to 3.39299. The obtained high values of nucleation order indicated a high rate of nucleation.     

Preparation,structural, and spectroscopic study of tetrakis(4-methylpyridinium) β-octamolybdate

The title compound, (C₆H₈N)₄[Mo₈O₂₆], has been prepared and its crystal structure determined by X-ray crystallography. The compound is triclinic,P¯1,Z=1 witha=10.167(1),b=10.745(1),c=10.027(8) Å,=85.05(1),=106.73(3), =107.75(1)°,V=999.1(7) ų,F(000)=748,D _x=2.59 andD _o=2.61(1) Mg/m³. The [Mo₈O₂₆]^4– anion shows slight differences in several bond lengths and angles when compared with other related octamolybdates. The planar cations are connected to the polyanions through bifurcated hydrogen bonds. The MoO₆ octahedra are distorted and the distortion has been evaluated using three different equations. The spectroscopic study shows that the cations are protonated and the polyanion presents the well-known infrared spectrum for octamolybdates.     

Intermetallic Compounds KnMm (М = Ag,Au, As,Sb, Bi,Ge, Sn,Pb): Geometrical and Topological Analysis,Cluster Precursors,and Self-Assembly of Crystal Structures

Crystallography Reports - A geometrical and topological analysis and simulation of the self-assembly of the crystal structures of intermetallic compounds formed in the K–M (M = Ag, Au, As,...     

Synthesis,characterization, and mesomorphic investigation of vinyl ester-substituted chalcones and effect of lateral ‒NO2 and ‒OCH3 group

A novel homologous series of α-4-(4′-n-alkoxy cinnamoyloxy) phenyl β-2″-nitro, 3″–4″ di methoxy benzoyl ethylenes, H_2n+1CnO?C₆H₄?CH?CH?COO?C₆H₄?CO?CH?CH?C₆H₂(NO₂) (OCH₃)₂ (n = 1–8, 10, 12, 14, 16, 18) has been synthesized. All these compounds have been characterized by suitable spectroscopic techniques. C₁ homologue is nonmesogenic, while C₂ homologue shows enantiotropic nematogenic property and the rest of the homologous (C₃?C₁₈) displayed enantiotropically smectogenic plus nematogenic phase. Phase transition temperatures and textures of the LC phase were determined by an optical polarizing microscopy (POM) equipped with a heating stage. The mesomorphic properties of these compounds were confirmed by differential scanning calorimetry (DSC) analysis.     

Crystal structure of bis-N,N′-p-chlorosalicylideneamine-1,2-diaminobenzene

The crystal structure of the title compound, C₂₀H₁₄N₂O₂Cl₂, has been determined by single crystal X-ray diffraction techniques. It crystallizes in the orthorhombic system witha=7.532(3)Å,b=18.563(2)Å,c=25.089(3)Å, space groupPbca,V=3507.9(3)ų,Z=8,F(000)=1584.D _x =1.459 g cm^–3,M=385.3 a. m. u., (MoK)=0.7107 Å, =3.35 cm^–1,T=297°K,R=0.086,R _w =0.049 for 2119 unique diffractometer data. The molecules are linked by van der Waals forces.     

Relationship of the crystal structure of γ-N,N-dimethylaminopropyl 2,2-diphenylpropionate hydrochloride to antimuscarinic activity

The title compound was synthesized, characterized by¹H nmr, and crystallized for x-ray crystallography. The antimuscarinic potency of the title compound was about equipotent to aprophen or atropine in inhibiting acetylcholine-induced contraction of guinea pig ileum (K _B =4.5 nM) and in inhibiting carbachol-stimulated release of-amylase from rat pancreatic acinar cells (K _i =1.4nM), and in inhibiting the binding of [N-methyl-³H]scopolamine to cerebral cortex (K _i =6.6nM). In the crystal, the O-C-C-C-N⁺ segment adopted a gauche-gauche configuration resulting in an N⁺O (carbonyl) distance of 5.001(9)Å, a distance comparable to that in aprophen. The ether oxygen atom is buried rendering it inaccessible for interaction with the muscarinic receptor. The carbonyl oxygen atom is exposed to the surface of the molecule and is readily accessible for intermolecular interactions. The similarity in biological activities of the title compound and aprophen is congruous with their similar N⁺O (carbonyl) distances.National Research Council Senior Associate, on leave from the Department of Organic Chemistry, Israel Institute for Biological Research, Ness Ziona, Israel.National Research Council Senior Associate, on leave from the Department of Pharmaceutical Chemistry, Hebrew University of Jerusalem, Jerusalem, Israel.     

Nepetanudone, a dimer of the α-pyrone 5,9-dehydronepetalactone

The title compound C₂₀H₂₄O₄ crystallizes in the orthorhombic space group P2₁2₁2, with a = 10.245(3), b = 17.103(3), c = 9.879(3) Å, D _c = 1.260 g cm ^–3, and Z = 4. Nepetanudone is postulated to be formed by a [4+4] cycloaddition of two 5,9-dehydronepetalactone moieties to give an asymmetric dimer in which each pair of atoms is magnetically nonequivalent. The compound was recovered from extracts of Nepeta nuda ssp. albiflora.