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  • 1
    Digitale Medien
    Digitale Medien
    Springer
    Journal of chemical crystallography 29 (1999), S. 115-119 
    ISSN: 1572-8854
    Schlagwort(e): Aminosulphines ; thionicotinamide S-oxide ; thiobenzamid ; X-ray structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Thiobenzamide and thionicotnamide S-oxide were prepared as intermediates in the dimerization of corresponding thioamides to 1,2,4-thiadiazoles and the X-ray crystal structure of thionicotinamide S-oxide water solvate was determined. Crystals belong to orthorhombic Pbca space group with a = 14.129(3), b = 7.299(2), c = 15.277(3)Å, and Z = 8. The geometry of the molecule accords well with that found in similar compounds; an intramolecular N–H···O hydrogen bond is present, while the packing is mainly determined by the hydrogen bond system involving the water molecule and the side-chain of the organic molecule. The contacts between pyridine moieties, stacked along the [010] axis, complete the packing.
    Materialart: Digitale Medien
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  • 2
    Digitale Medien
    Digitale Medien
    Springer
    Journal of chemical crystallography 29 (1999), S. 667-670 
    ISSN: 1572-8854
    Schlagwort(e): 6′-butoxy-2,6-diamino-3,3′-azo-dipyridine ; X-ray structure ; hydrogen bonds
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Chemical preparation, X-ray single crystal, and calorimetric studies of C14H18N6O · H2O are described. The compound crystallizes in the triclinic space group, P $${\bar 1}$$ with unit cell dimensions: a = 6.2640(3), b = 10.9840(4), c = 12.2220(3) Å, α = 105.03(2), β = 96.96(2), γ = 101.6(2)°, V = 712.10(5) Å3, and Z = 2. The 6′-butoxy-2,6-diamino-3,3′-azo-dipyridine monohydrate structure is built up from organic layers parallel to the (120) plane linked via O—H···N bond.
    Materialart: Digitale Medien
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  • 3
    Digitale Medien
    Digitale Medien
    Springer
    Journal of chemical crystallography 29 (1999), S. 653-657 
    ISSN: 1572-8854
    Schlagwort(e): picoline derivative ; X-ray structure ; nonlinear optic
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Because of their strongly delocalized π electronic systems, polymeric and non-polymeric aromatic compounds show high nonlinear optical properties. The present work deals with the synthesis and structural characterization (including X-ray single crystal studies) of new picoline derivatives, 5-ethyl-2-(4-nitro-styryl)-pyridine, space group P $${\bar 1}$$ a = 6.9505(7), b = 7.418(1), c = 13.877(2) Å, α = 105.14(1), β = 93.88(1), γ = 105.89(1)°, and 5-ethyl-2-(4-nitro-7-ol-styryl)-pyridine, space group Pcab, a = 8.628(2), b = 10.405(2), and c = 31.604(5) Å.
    Materialart: Digitale Medien
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  • 4
    ISSN: 1572-8854
    Schlagwort(e): vinilic sulfides ; thioacetylenes ; tosylates ; X-ray structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The reaction between 1-phenylsulphenyl-2-phenylethyne and p-toluenesulfonic acid in methylene chloride gives (Z)-1-(phenylsulphenyl)-2-phenylethenyl p-toluenesulfonate (1) in good yields. This reaction is both a regio- and a stereospecific cis addition, confirmed by X-ray crystal structure analysis of the title compound. 1 crystallizes in the monoclinic space group P21/n with the lattice parameters a = 10.556(3), b = 9.730(3), c = 19.687(3) Å, β = 105.05(2)°, V = 1952.7(8) Å3, and Z = 4. The results of elemental analysis, IR and NMR spectroscopy are included.
    Materialart: Digitale Medien
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  • 5
    ISSN: 1572-8854
    Schlagwort(e): 4-iminecinnoline analogs of quinolones ; X-ray structure ; intramolecular hydrogen bond ; packing
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Crystal structures of hydrochlorides of 7-chloro- and 7-methyl-4-iminecinnoline analogs of antibacterial quinolones have been determined by X-ray diffraction methods. The cell parameters for the 7-chloro (1) analog in the space group P21/c are a = 9.061(1), b = 19.062(1), c = 7.310(1)Å, β = 104.92(1)°, Z = 4, and D calc = 1.569 g/cm3 and for the 7-methyl (2) analog in the space group P $${\bar 1}$$ are a = 7.277(5), b = 9.080(5), c = 10.058(5) Å, α = 106.10(1), β = 102.38(1), γ = 90.18(1)°, Z = 2, and D calc = 1.429 g/cm3. Despite geometrical equivalency of methyl and chlorine and some resemblance of their packings, the crystal structures are not isostructural. Each compound forms a strong intramolecular hydrogen bond between protonated 4-imine (a donor) and 3-carboxylic (an acceptor) groups. Compounds with a similar bond, but with reversed functionality and orientation of the 3-carboxylic group, form common quinolones, being mostly 4-oxoquinoline-3-carboxylic acids. The difference should exclude chemical affinity of 4-imine analogs to the guanine base of a bacterial DNA in DNA-gyrase complex, as proposed by Shen et al. 2 for 4-oxoquinoline-3-carboxylic acids showing antibacterial activity. Also the free acidic function of a carboxyl group may significantly lower permeability of 4-imine-3-carboxylic analogs of quinolones. Surprisingly, they have demonstrated antibacterial activity comparable with that of nalidixic acid.
    Materialart: Digitale Medien
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  • 6
    ISSN: 1572-8854
    Schlagwort(e): ruthenium cluster ; bis(diphenylphosphino)methane ; hydride ; chloride ; X-ray structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The reaction of [Ru3(CO)10(μ-dppm)] 1 with PPhCl2 in refluxing CHCl3 results in the isolation of [(μ-H)Ru3(CO)8(μ-Cl)(μ-dppm)] 3 in 10% yield. Compound 3, which has been structurally characterized by crystallographic methods, is also formed from the reaction of 1 with H2 in refluxing CCl4. The compound crystallizes in the monoclinic space group P21/c with a = 16.814(2), b = 18.7590(12), c = 11.486(2) Å, β = 97.745(11)°, V = 3589.8(8) Å3, and Z = 4. The hydride and chloride ligands bridge the same edge of the triruthenium cluster as the dppm ligand.
    Materialart: Digitale Medien
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  • 7
    Digitale Medien
    Digitale Medien
    Springer
    Journal of chemical crystallography 29 (1999), S. 45-55 
    ISSN: 1572-8854
    Schlagwort(e): Melaminium dinitramide and melaminium nitrate ; melaminium salts ; dinitramide salt ; hydrogen bonding ; X-ray structure ; energetic materials
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Two energetic salts of the melaminium cation have been prepared and structurally characterized from room temperature X-ray single crystal diffraction data. Melaminium dinitramide (I), triclinic, P1¯, a = 6.6861(11), b = 6.9638(16), c = 10.447(2) Å , α = 99.07(3), β = 98.30(3), γ = 108.50(3)°, V = 445.6(2) Å3, and Z = 2. Melaminium nitrate (II), monoclinic, P21/c, a = 3.5789(7), b = 20.466(4), c = 10.060(2) Å, β = 94.01(2)°, V = 735.0(3) Å3, and Z = 4. The crystal structures of both salts show distinct monoprotonated melaminium cations and dinitramide- or nitrate anions, respectively. Efficient packing in the solid state is achieved by extensive hydrogen bonding between two-dimensional zigzag ribbons of the melaminium cations and the respective anions resulting in high densities of the solid state structures of 1.74 (I) and 1.71 g/cm3 (II).
    Materialart: Digitale Medien
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  • 8
    ISSN: 1572-8854
    Schlagwort(e): X-ray structure ; dtc ; cadmium complex
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The cadmium complex of bis(dipropyldithiocarbamate), [Cd2(n-Pr2dtc)4] (dtc = dithiocarbamate) was crystallized from ethylether. It crystallizes in the monoclinic system, space group P 2I/c, with lattice parameters, a = 8.2532(1), b = 19.4519(1), c = 13.4163(2) Å, β = 99.243(1)°, and Z = 4. The X-ray single-crystal structure of [Cd2(n-Pr2dtc)4] reveals that the complex is binuclear in the solid state and the Cd atom has a distorted square-pyramidal coordination environment and four equatorial donors are the two bidentate chelate sulfur atoms from two dtc ligands, of which the sulfur atom from the bridging dtc ligand occupies the apical position of the symmetry-related Cd atom in the dimer structure.
    Materialart: Digitale Medien
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  • 9
    ISSN: 1572-8854
    Schlagwort(e): host–guest complexes ; antimony trifluoride ; azacrown ethers ; X-ray structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Synthesis and single-crystal X-ray structures are recorded for three adducts of SbF3 with different azacrown ethers. [SbF3·H2O·L1], 1, (L1 = 12,13-benz-1,10-di(azamethyl)-4,7-dioxacyclotetradecane-1,14-dione), triclinic, $$P\bar 1$$ , a = 11.234(2), b = 11.691(2), c = 8.869(2) Å, α = 94.66(3), β = 113.12(3), γ = 67.82(3)°, Z = 2. [SbF3Cl·H2O·(HL2)], 2, (L2 = monoaza-18-crown-6), orthorhombic, P212121, a = 8.763(2), b = 13.003(3), a = 16.836(3) Å, Z = 4. [(SbF3)2Cl2·(H2L3)], 3, (L3 = 1,10-diaza-18-crown-6), triclinic, $$P\bar 1$$ , a = 8.284(2), b = 9.016(2), c = 9.134(2) Å, α = 82.92(3), β = 65.24(3), γ = 63.38(3)°, Z = 1. All three structures include SbF3 neutral molecules in the pyramidal mode and the antimony second coordination sphere is completed up to six in different fashions. In 1 the dimeric (SbF3)2 adducts are made up due to the involvement of the symmetry-related fluorine atom in coordination. The distorted octahedron is then completed by water molecule and carbonyl oxygen of L1. The neutral molecules are joined by coordination and hydrogen bonds in the infinite ribbons. 2 and 3 are both comprised of neutral and charged species also bounded via coordination and hydrogen bonds. L2 and L3 in the complexes adopt the form of single and double-charged cations, respectively. The inorganic backbone unites the neutral SbF3 molecules and chloride anions in the alternative mode. The sixth coordination site in the antimony polyhedron is completed by the water molecule in 2 and the ethereal oxygen atom in 3. Alignment of the inorganic entities within the structures of 2 and 3 is strikingly similar. Hydrogen bonding patterns are discussed.
    Materialart: Digitale Medien
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  • 10
    Digitale Medien
    Digitale Medien
    Springer
    Journal of chemical crystallography 29 (1999), S. 383-389 
    ISSN: 1572-8854
    Schlagwort(e): chiral auxiliary ; π-stacking ; asymmetric synthesis ; X-ray structure ; chromium complexes
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract (—)-8-Phenylmenthol was prepared and converted to the corresponding tricarbonyl (η6-arene) chromium(0) complex. Derivitization as the acrylate ester (1) and subsequent X-ray analysis revealed a 1:1 mix of s-cis and s-trans acrylate in the unit cell, and geometric proximity to support a through-space π stacking interaction in the case of the s-trans isomer. The dihedral angle between the best planes through the chromium-bound aryl ring and the acrylate group is 19.9° for the s-trans isomer and 34.4° for the s-cis isomer. Crystal data for (1): C22H26O5Cr, monoclinic, P21 (No. 4), a = 10.269(1), b = 10.482(1), c = 19.787(2), β = 95.85(1), Z = 4, and D calc = 1.32 g cm−3.
    Materialart: Digitale Medien
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  • 11
    ISSN: 1572-8854
    Schlagwort(e): X-ray structure ; pentacoordinated copper(II) ; square-pyramid ; acetonitrile coordination
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The syntheses and structures of two square-pyramidal acetonitrile coordinated copper(II) complexes, [Cu(HbhsNO2)(CH3CN)2]ClO4 (1) and [Cu(HahsNO2)(CH3CN)(ClO4)] (2), are described. The mononegative ligands are obtained by deprotonation of the phenolic-OH of N-(benzoyl)-N′-(5-nitrosalicylidene)hydrazine (H2bhsNO2) and of N-(anisoyl)-N′-(5-nitrosalicylidene)hydrazine (H2ahsNO2). Crystal data for 1: monoclinic, P21/c (#14), a = 9.7245(14), b = 20.23(4), c = 11.042(3) Å, β = 91.86(2)°, V = 2171.0(7) Å3, and Z = 4 and for 2: triclinic, P1¯ (#2), a = 9.7710(19), b = 9.9687(15), c = 11.062(5) Å, α = 73.10(3), β = 88.77(3), γ = 88.379(14)°, V = 1030.4(5) Å3, and Z = 2. In each complex the planar ligand binds the metal ion via phenolate-O, imine-N, and amide-O. The nitrogen of an acetonitrile molecule satisfies the fourth site of the square-plane containing the metal ion. In 1 the axial coordination is provided by the nitrogen of a second acetonitrile molecule, whereas in 2 one of the oxygen atoms of the perchlorate occupies the fifth axial site. The axial acetonitrile molecule of 1 is bound to the metal center in a bent mode. The other noticeable difference between the two structures is in the geometry at the metal center. A large displacement (0.23 Å) of the metal ion from the ONON basal plane towards the axial coordinating atom is observed in 1. On the other hand, there is no displacement of the metal center from the same ONON basal plane in 2. The EPR and electronic spectral features in acetonitrile solutions are consistent with the solid state structures.
    Materialart: Digitale Medien
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