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  • 1
    Electronic Resource
    Electronic Resource
    An analysis of the characteristics of rough bed turbulent shear stresses in an open channel (1997)
    Springer
    Stochastic environmental research and risk assessment 11 (1997), S. 193-210 
    Details
    ISSN: 1436-3259
    Keywords: Turbulence ; sediment ; fluvial ; river ; bursting process ; statistics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Architecture, Civil Engineering, Surveying , Energy, Environment Protection, Nuclear Power Engineering , Geography , Geosciences
    Notes: Abstract Entrainment of sediment particles from channel beds into the channel flow is influenced by the characteristics of the flow turbulence which produces stochastic shear stress fluctuations at the bed. Recent studies of the structure of turbulent flow has recognized the importance of bursting processes as important mechanisms for the transfer of momentum into the laminar boundary layer. Of these processes, the sweep event has been recognized as the most important bursting event for entrainment of sediment particles as it imposes forces in the direction of the flow resulting in movement of particles by rolling, sliding and occasionally saltating. Similarly, the ejection event has been recognized as important for sediment transport since these events maintain the sediment particles in suspension. In this study, the characteristics of bursting processes and, in particular, the sweep event were investigated in a flume with a rough bed. The instantaneous velocity fluctuations of the flow were measured in two-dimensions using a small electromagnetic velocity meter and the turbulent shear stresses were determined from these velocity fluctuations. It was found that the shear stress applied to the sediment particles on the bed resulting from sweep events depends on the magnitude of the turbulent shear stress and its probability distribution. A statistical analysis of the experimental data was undertaken and it was found necessary to apply a Box-Cox transformation to transform the data into a normally distributed sample. This enabled determination of the mean shear stress, angle of action and standard error of estimate for sweep and ejection events. These instantaneous shear stresses were found to be greater than the mean flow shear stress and for the sweep event to be approximately 40 percent greater near the channel bed. Results from this analysis suggest that the critical shear stress determined from Shield's diagram is not sufficient to predict the initiation of motion due to its use of the temporal mean shear stress. It is suggested that initiation of particle motion, but not continuous motion, can occur earlier than suggested by Shield's diagram due to the higher shear stresses imposed on the particles by the stochastic shear stresses resulting from turbulence within the flow.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02427915
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  • 2
    Electronic Resource
    Electronic Resource
    Crystal structure of tetrakisdiphenylammonium hexadecachlorotetrabismuthate(III) (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 841-844 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; bismuth chloride complexes ; diphenylammonium
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract [(C6H5)2NH2]4 +[Bi4Cl16]4− crystallizes in the triclinic space group $$P\bar 1$$ witha=11.835(2),b=12.393(2),c=12.625(3)Å, α=108.37(3), β=108.69(3), γ=96.00(3)° andD c=2.135 g cm−3 forZ=1. The [Bi4Cl16]4− anion is a centrosymmetric cluster of four distorted edge-sharing BiCl6 octahedra. The ranges of the Bi−Cl bonds are 2.484(4)–2.606(3)Å for Bi−Cl(terminal), 2.691(3)–2.956(4)Å for Bi-Cl(µ2), and 2.960(3)–3.120(4)Å for Bi-Cl(µ3). The cations and anions are held in place by weak hydrogen bonds.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01671080
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  • 3
    Electronic Resource
    Electronic Resource
    Crystal structure of a bulky cyclic sulfite (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 215-218 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; cyclic sulfite ; pentacycloundecane-8 ; 11-dione
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The structure of the cyclic sulfite derived from the reaction of thionyl chloride withendo-8-hydroxy-exo-8-(endo-8′-hydroxypentacyclo[5.4.0.0.2,6.03,10.05,9]undec-exo-8′-yl)pentacyclo-[5.4.0.0.2,6.03,10.05,9]undecane is reported. All bond lengths and angles are consistent with the strained cage geometry. A static disorder of the terminal oxygen was found to be present.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01665171
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  • 4
    Electronic Resource
    Electronic Resource
    Structure of the pinacol formed via sodium-promoted reductive dimerization of 12-methyleneheptacyclo-[6.6.02,6.03,13.04,11.05,9.010,14]tetradecan-7-one (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 417-420 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; pinacol ; reductive dimerization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The pinacol resulting from sodium promoted reductive coupling of a methyleneheptacyclo-[6.6.02,6.03,13.04,11.05,9.010,14]tetradecanone possesses a conformation in which equivalent groups on the pinacol carbon are virtually perpendicular to each other. This rotation minimizes steric interactions, thus the geometries of all the fragments in the molecule are within expected values.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01665280
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  • 5
    Electronic Resource
    Electronic Resource
    Crystal and molecular structure of 1-vinyl-3-methyl-imidazolium iodide, C6H9N2I (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 601-603 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; imidazolium ; vinyl
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound crystallizes with two independent molecules in the unit cell. The two molecules arecis-trans isomers. Crystal data: orthorhombic, P212121,a=7.0417(6),b=9.5341(9),c=25.411(2) Å,Z=8. The crystal structure has been solved by automated Patterson methods and refined toR=0.024 for 1843 observed reflections.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01667031
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  • 6
    Electronic Resource
    Electronic Resource
    Molecular structure of 3-(3-oxo-bicyclo[2.2.1]hept-5-en-2-yl)-oxirane-2-carboxylic acid methyl ester (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 81-84 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; epoxy ester
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal and molecular structure of an epoxy ester is described. The structure has been solved by vector search methods and refined by least squares methods toR 1=0.0372 [I〉2σ(I)]. The structure consists of two independent molecules in the asymmetric unit. These molecules are chemically the same. Crystal data: C11H12O4, triclinic, space group $$P\bar 1$$ ,a=10.324(3),b=10.553(7),c=10.869(5)Å, α=61.77(4), β=88.64(4), γ=88.16(6)°,V=1042.7(9)Å3,Z=4.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02018702
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  • 7
    Electronic Resource
    Electronic Resource
    Crystal structure of a highly hydrated tristrontium phosphate, Sr9(PO4)6·16H2O (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 341-346 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; hydrated phosphate ; layer-type structure ; strontium phosphate ; strontium phosphate hydrate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal structure of a highly hydrated tristrontium phosphate, nonastrontium hexakis(phosphate) hexadecahydrate, Sr9(PO4)6·16H2O, has been determined by single crystal X-ray diffraction. The crystals are monoclinic,a=15.203(2),b=6.488(1),c=18.984(7) Å, β=98.42(2)o, space groupP2/c (No. 13),Z=2,V=1852.3 Å3,d c =2.951 Mg·m−3. The structure was refined by full-matrix least-squares techniques toR=0.038,R w =0.051, for 2329 reflections with I≥3σ(I). The structure can be described in terms of a layer-type arrangement parallel to (100). One layer consists of a compact assembly of columns of Sr and PO4 ions in a pseudohexagonal arrangement resembling an apatitic structure. A second layer containing all the water molecules and one PO4 ion that occupies the interstitial space may be referred to as the hydrated layer. The structure has an overall similarity to that of octacalcium phosphate and can be considered as a model for amorphous calcium phosphate.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01677098
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  • 8
    Electronic Resource
    Electronic Resource
    Molecular structure of [(tBu)2Al(μ-NHtBu)]2 (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 563-567 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; aluminum ; amide
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal and molecular structure of [(tBu)2Al(μ-NHtBu)]2 has been determined. The unit cell contains two independent molecules with only slight variation in the orientation of thetert-butyl ligands. Crystal data: Triclinic, $$P\bar 1$$ ,a=9.0138(6),b=10.2944(8),c=15.791(1) Å, α=91.262(6), β=89.822(6), γ=106.141(6)°,V=1407.2(2) Å3,Z=2,R=0.039,R w=0.041.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01668416
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  • 9
    Electronic Resource
    Electronic Resource
    Crystal structure of 5-(p-methoxyphenylamino)indane and AM1 calculations on N-arylamines derivatives, precursors of phenothiazine drugs (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 735-739 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; diphenyl amines ; AM1 calculations ; phenothiazines
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The structural determination by X-ray crystallography of the titled N-arylamine 4a, as well as AM1 calculations on a series of derivatives (4b–c, 5a–c), are reported. The compound 4a is monoclinic P21/c with a = 7.656(3), b = 23.655(5), c = 7.686(9) Å, β = 112.59(6)°, V = 1285.2(2) Å3 and Z = 4. This structure has been used as a template for the building of some others derivatives used for AM1 calculations. The results show that the cyclization position on the aromatic rings, which can lead to two regioisomers, depends on the nature of the benzylic substituants.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1021860410863
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  • 10
    Electronic Resource
    Electronic Resource
    Synthesis, characterization, and X-ray crystal structure of di-(2,4-imidazolidinedione-5-ethyl)disulfide, C10H14N4O4S2 (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 761-765 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; noncentrosymmetric ; disulfide ; imidazolidinedione ; homocystine hydantoin
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Di-(2,4-imidazolidinedione-5-ethyl)disulfide or homocystine hydantoin, C10H14N4O4S2 (I), crystallizes in the non-centrosymmetric space group P21 (No. 4) with two molecules in the unit cell with a = 7.132(1), b = 9.282(2), c = 10.770(2) Å and β = 105.68(1)°. The two imidazolidinedione rings are planar with a dihedral angle of 46.9°. The rings are joined by a diethyl disulfide bridge at chiral centers on the rings. The C-S-S-C torsion angle is −80°(−sc). The absolute stereochemistry of the chiral centers was determined to be (5S, 5′S), η = + 0.92 (11). Important bond distances include: S-S = 2.022(4); S-C (mean) = 1.809(8); and C=O (mean) = 1.224(7) Å. The compound is stabilized by a network of intermolecular carbonyl-to-amine hydrogen bonding and van der Waals cohesive forces.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1021816628610
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  • 11
    Electronic Resource
    Electronic Resource
    Crystal structure of a macrocyclic tetraamine isocyanato zinc(II) complex (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 831-834 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; macrocyclic tetraamine ; isocyanato zinc(II) complex
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The complex, [Zn(L)(NCO)]Cl · 3H2O (1) (L = 3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,01.18,07.12]docosane), has been synthesized and structurally characterized. 1 crystallizes in the monoclinic system, space group P21/n with a = 10.530(3), b = 9.315(2), c = 27.188(3) Å, β = 92.58(1)°, V = 2664.1(9)Å3, and Z = 4. The zinc atom is in a distorted squarepyramidal environment with the four nitrogen atoms of the macrocycle and one nitrogen atom of the isocyanate ligand.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1021831921283
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  • 12
    Electronic Resource
    Electronic Resource
    Synthesis and crystal structure of [(PhenH)(PhenH2)][BiCl6]·2H2O with different o-phenanthroline protonations (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 791-796 
    Details
    ISSN: 1572-8854
    Keywords: Halobismuthate(III) ; phenanthroline ; synthesis ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The reaction between bismuthate oxide and phen (1,10-phenanthroline) in acid medium led to the isolation of the unusual [(PhenH)(PhenH2)][BiCl6]·2H2O derivative, which has been characterized by X-ray analysis and IR spectroscopy. The compound crystallizes in the triclinic space group $$[\text[P\bar 1]]$$ with a = 8.313(2), b = 9.349(2), c = 9.807(3) Å, α = 86.39(3), β = 110.27(3) and γ = 106.48(3)°. The crystal structure is made of [BiCl6]3− anions and [(PhenH)(PhenH2)]3+ cations. A network of hydrogen bond interactions involving the two clathrated water molecules, the phenanthroline moiety and the chlorines characterizes the entire structure.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1021871502627
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  • 13
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    Synthesis and crystal structure of macrocyclic nickel(II) complex bridged by chromate (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 867-870 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; macrocyclic nickel(II) complex ; chromate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract A novel compound catena-(μ-CrO4-O,O′)[Ni(L1)Ni(L2)] 3H2O (1) (L1 = 3,5,10,12-tetramethyl-1,4,8,11-tetraazacyclotetradecane and L2 = 2,5,9,12-tetramethyl-1,4,8,11-tetraazacyclotetradecane) has been synthesized for the first time and structurally characterized. 1 crystallizes in the triclinic space group Pī with a = 9.623(1), b = 10.084(1), c = 12.723 (3) Å, α = 66.74(2), β = 75.20(1), γ = 72.02(1)°, V = 1066.2(3) Å3, and Z = 2. The coordination environment around the Ni(II) ions is an axially elongated octahedron with the secondary amines of the isomeric ligands and two oxygen atoms of [CrO4]2−.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1022890217250
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  • 14
    Electronic Resource
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    Synthesis, characterization, peripheral studies, and structural analysis of E-4-(N-methylanilino)-3-pentene-2-one, C12H15NO (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 899-903 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; ir/nmr ; β-amino-α ; β-unsaturaled ketone ; noncentrosemmtric ; enamino ketones
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Crystallographic structural refinement of E-4-(N-methylanilino)-3-pentene-2-one (I) has been carried out by means of three-dimensional single-crystal X-ray diffractometry. The title compound crystallizes in space group C2 (No. 5,Z = 4). The lattice constants are a = 21.543(4), b = 6.433(1), c = 8.019(2) Å, and β = 97.82(3)°. Characterizations include physical property determinations and spectrometric identifications employing IR, 1H and 13C NMR, and X-ray powder analyses. The molecules in the crystal lattice are held together by van der Waals forces. Selected bond distances and angles are presented and discussed as well as synthesis and peripheral studies.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1022802619976
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  • 15
    Electronic Resource
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    The structure of N-(1H-benzo[d]imidazol-2-ylmethyl)-N-(2,6-dichlorophenyl)amine (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 145-147 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; benzimidazole ; antimicrobial activity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The N-(1H-benzo[d]imidazol-2-ylmethyl)-N-(2,6-dichlorophenyl)amine, C14H11N3Cl2, M r = 292.17, crystallizes in the orthorhombic space group Pbca with unit cell parameters a = 10.707(2), b = 9.615(2), c = 25.944(6) Å. The benzimidazole ring system is planar and makes a dihedral angle of 77.8(1)° with the phenyl ring. The structure is stabilized by an N–H···N hydrogen bond.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1022497931783
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  • 16
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    Synthesis and structural characterization of a novel polymeric praseodymium(III) complex with a new flexible double betaine (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 177-183 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; coordination polymer ; praseodymium(III) carboxylate complex ; double betaine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract A novel polymeric Pr(III) complex with a new double betaine, namely [{Pr(L1)1.5(H2O)2} n ][ClOli4]3 n ·nH2O (1) (L1 = 1,4-diazoniobicyclo[2,2,2]octane-1,4-dipropionate), has been synthesized and characterized by X-ray analysis. In the title complex, the Pr(III) atom is nine-coordinated by seven oxygen atoms from five L1 ligands and two aqua ligands. Each pair of adjacent praseodymium(III) atoms is linked by a pair of μ3 chelating and bridging carboxylate groups, thus forming an infinite metal···metal chain running parallel to the a direction, and such chains are cross-linked by flexible backbones of L1 ligands into a three-dimensional network with the perchlorate anions and lattice water molecules accommodated in the interstitial space. The title complex crystallizes in the monoclinic space group P21/n with a = 8.085(2), b = 14.316(3), c = 29.775(6) Å, β = 103.04(3)° and Z = 4.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1022414109261
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  • 17
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    Crystal structures of three substituted pentacyclo[5.4.0.02,6.03,10.05,9]undecanes (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 251-258 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; pentacycloundecane
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal structures of three compounds formed via ultimate nucleophilic attack of unsaturated hydrocarbon fragments are reported. Geometries of the bis(vinyl)-, mono(vinyl), and bis(ethynyl)-substituted PCU species are unexceptional. The crystal structures are dictated by the availability of intermolecular hydrogen bonding.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1021893001351
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  • 18
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    Molecular structure and absolute configuration of (+)-(1R, 2S, 6R, 7S, 1′R)-5-(1′-phenylethylamino)-endo-tricyclo[5.2.1.02,6]deca-4,8-dien-3-one (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 497-499 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; tricyclodecadienone ; enaminone ; resolution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal and molecular structure of (+)-(1R, 2S, 6R, 7S, 1′R)-5-(1′-phenylethylamino)-endo-tricyclo[5.2.1.02,6]deca-4,8-dien-3-one is described. Based on the known absolute configuration (R) of the α-phenylethylamine moiety the X-ray analysis revealed the absolute configuration of the title compound. The structure was refined to R 1 = 0.0298 for 1950 reflections (with I 〉 2σ(I)). Crystal data: C18H19NO, monoclinic, space group P21, a = 6.7406(4), b = 9.959(2), c = 11.3123(8)Å, β = 102.969(5), V = 740.0(2)Å3, and Z = 2.
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    URL: http://dx.doi.org/10.1023/A:1021733108852
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  • 19
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    Synthesis and X-ray structure of N-phenyl phenylglyoxamide (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 555-560 
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    ISSN: 1572-8854
    Keywords: N-phenyl phenylglyoxamide ; phenylglyoxanilide ; synthesis ; x-ray structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound (C14H11NO2) is monoclinic with a = 13.579(2), b = 5.297(1), c = 16.455(2) Å, β = 98.11(2)°, Z = 4, and space group P21/n. The significant structural features lie in the two carbonyl groups of the glyoxamide which are oriented antiperiplanar to each other [−163.6(3)°]. The central bond C(1)–C(2) is 1.545(4) Å. The observed conformation is stabilized by intramolecular hydrogen bonds.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1023248223359
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  • 20
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    Molecular structure and absolute configuration of (−)-(1R, 2S, 6R, 7S, 2′S)-5-(2′-hydroxymethylpyrrolidin-1′-yl)-endo-tricyclo[5.2.1.02,6]deca-4,8-dien-3-one (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 493-495 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; tricyclodecadienone ; enaminone ; dynamic kinetic resolution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal and molecular structure of (−)-(1R, 2S, 6R, 7S, 2′S)-5-(2′-hydroxymethyl-pyrrolidin-1′-yl)-endo-tricyclo[5.2.1.02,6]deca-4,8-dien-3-one is described. Knowing the absolute configuration of the prolinol moiety (S) the X-ray diffraction study established the absolute configuration of the title compound. The structure was refined to R 1 = 0.0322 for 1237 reflections (with I 〉 2σ(I)). Crystal data: C15H19NO2, monoclinic, space group P21, a = 6.0757(4), b = 11.3473(5), c = 9.5114(7)Å, β = 104.686(6)°, V = 634.32(7)Å3, and Z = 2.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1021781024782
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    The crystal structure of 5α,9α-peroxyergosta-7,22-dien-6-one-3β-ol acetate (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 239-241 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; ergosterol peroxide
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Ergosterol acetate, in pyridine, reacts with hydrogen peroxide and catalytic amounts of FeCl3 to afford the unusual product 5α,9α-peroxyergosta-7,22-dien-6-one-3β-ol acetate. The peroxide, in the title structure, is seen to bridge the C5 and C9 positions of the sterol backbone. Crystal data: C30H44O5, orthorhombic, P212121, a = 6.552(2), b = 11.048(8), c = 37.60(2), V = 2772(3)Å3, Z = 4.
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    The crystal structure of hexabenzoylhexaazaisowurtzitane (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 593-596 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; cage compound ; hexabenzoylhexaazaisowurtzitane
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal and molecular structure of an interesting cage compound is described. Crystal data: C48H36N6O6·(CH3)2CO; monoclinic; space group: P2 1 /n; a = 14.948(3) Å, b = 15.079(3) Å, c = 19.539(4)Å, β = 93.93(3)°, V = 4394(2)Å3; and Z = 4.
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    URL: http://dx.doi.org/10.1023/A:1022452707772
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    Synthesis and crystal structure of the copper(II) complex with novel Schiff base ligand: Cu(C8H7O2N)2(OH2) (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 295-298 
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    ISSN: 1572-8854
    Keywords: Copper ; crystal structure ; synthesis ; Schiff base ligand
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title complex Cu(C8H7O2N)2(OH2) crystallized in the orthorhombic space group, Pbca with unit cell parameters: a = 15.242(2), b = 11.782(4), c = 17.946(4) Å, and Z = 8. Two nitrogen atoms, two phenolic oxygen atoms of the ligand, and one water molecule are coordinated with copper to form a distorted tetragonal pyramidal polyhedron.
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    URL: http://dx.doi.org/10.1023/A:1009569701034
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    Structural study of the molecular complex in crystals of brucine with pantolactone (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 121-125 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; brucine ; pantolactone ; molecular complex ; chiral resolution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract We have determined an X-ray crystal structure, a = 12.482(1), b = 14.349(1), c = 14.342(1) Å, orthorhombic, P212121 for a molecular complex of brucine with pantolactone. The crystal structure is composed of corrugated sheets of brucine molecules containing the guest pantolactone molecules. The conformational twist of the pyrrolidine ring in brucine may probably be important in projecting the amine N2 to provide a strong and specific binding site for a chiral complexation. The pseudo-equatorial orientation of the hydroxyl group of the pantolactone anchors itself for binding via hydrogen bonding. In the crystal packing, the pantolactone molecules form helices and the brucine molecules are attached to these helices by O=H···N hydrogen bonds.
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    Synthesis and crystal structure of the heterometallic square-chain polythiometalate: {[W4Ag5S16]2 · [La(DEF)2(DMF)6][La(DEF)4(DMF)4]}n (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 629-633 
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    ISSN: 1572-8854
    Keywords: heterometallic polymeric cluster ; polythiometalate ; synthesis ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The complex (NH4)2 WS4 reacts with AgNO3 and La(NO3)3 · 6H2O in a mixture of DEF/DMF (DEF—N,N′-diethylformamide), to give a new heterometallic square-chain polythiometalate {[W4Ag5S16]2 · [La(DEF)2(DMF)6] · [La(DEF)4(DMF)4]}n (1). 1 crystallizes in the monoclinic space group P2/c, a = 19.5534(8), b = 16.9552(6), c = 22.3479(9) Å, β = 106.053(1)°, V = 7120.1(5) Å3, and Z = 2. The anion polymeric chain of 1 can be regarded as an octanuclear cyclic cluster of [W4Ag4S16]4− fragments linked through Ag+ ions. The polymeric chain is extended through the parallel edges of the square unit. The mean W—Ag distance is 2.963(16) Å. The La3+ cations are coordinated by different solvent molecules, the average La—O bond of these large trivalent cations is 2.47(1) Å.
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    Synthesis and crystal structure of 4,5-(cis-cyclohexylenedithio)-1,3-dithiole-2-one (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 719-723 
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    ISSN: 1572-8854
    Keywords: synthesis ; crystal structure ; independent molecules
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The x-ray crystal structure of 4,5-(cis-cyclohexylenedithio)-1,3-dithiole-2-one has been determined. Yellow block shaped crystals of C9H10OS4 crystallize in the space group P $${\bar 1}$$ with cell dimensions a = 8.872(4), b = 9.330(8), c = 14.333(12) Å, α = 95.23(7), β = 91.09(5), γ = 107.60(5)°, V = 1124.8(14) Å3, and Z = 4. This compound has two S---S contacts [3.574, 3.610 Å] shorter than 3.70 Å and the usual disordered ethylene moiety [C(3)—C(8)] of the six-membered ring is fixed by the cis-cyclohexylene subsitituent. This means that it may be a new precursor for conducting and strong near-IR absorbing nickel-dithiolenes. Also, it provides the first example of polymorphism of the dmit derivatives and contains two independent molecules I and II in the asymmetric unit.
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  • 27
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    Crystal structure and emission study of [(PPh3)2Cu(dmp)-O-(dmp)Cu(PPh3)2]2+ (dmp = 2,9-dimethyl-1,10-phenanthroline) (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 797-802 
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    ISSN: 1572-8854
    Keywords: synthesis ; crystal structure ; Cu(I) complex ; μ-oxo-bis(2,9-dimethyl-1,10-phenanthroline) ; luminescence
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The synthesis and crystal structure of a luminescent dinuclear Cu(I) complex as the BF− 4 salt from toluene and methanol containing triphenylphosphine and μ-oxo-bis(2,9-dimethyl-1,10-phenanthroline) is described. The coordination geometry about the Cu(I) center is distorted tetrahedral. An unusual feature of the structure is a pseudo-inversion center located near the oxygen atom at approximately 0.51, 0.26, 0.25, such that all of the atoms except for the oxygen are related by a pseudo-inversion center to another atom in the same molecule, as well as by crystallographic inversion to the other molecule in the unit cell. The complex displays luminescence from an MLCT band in fluid solution and emission from both a metal-centered charge-transfer and intraligand (phenanthroline) state at 77K in a chloroform snow. Crystal data: triclinic, P $$\bar 1$$ , a = 15.163(2), b = 16.985(2), c = 18.731(2) Å, α = 106.458(9), β = 91.416(8), γ = 102.557(9)°, V = 4496(1) Å3, and Z = 2.
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    Synthesis and crystal structure of hexakis(N-methylimidazole) iron(II) pyridine-2-sulfonate (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 23-26 
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    ISSN: 1572-8854
    Keywords: iron ; crystal structure ; synthesis ; N-methylimidazole
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The compound [Fe(C4H6N2)6][C5H4NSO3]2 crystallized in the monoclinic space group, P21/n with unit cell parameters: a = 13.676(3), b = 8.345(2), c = 18.663(4) Å, β = 106.40(3)° and Z = 2. The title compound consists of a [Fe(C4H6N2)6]+2 hexacoordinated iron(II) cation and two C5H4NSO− 3 anions. In the cation the iron atom is coordinated to six N-methylimidazole imine nitrogen atoms in a distorted octahedral arrangement. The N1,N5,N1i,N5i atoms are coplanar and the iron lies in this plane.
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  • 29
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    Heterometallic cuboidal complexes as derivatives of the [MO3S4(H2O)9]4+ cluster (1995)
    Springer
    Journal of cluster science 6 (1995), S. 449-461 
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    ISSN: 1572-8862
    Keywords: Molybdenum ; heterometallic ; cuboidal clusters ; synthesis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract Heterometallic atoms can be incorporated into the Mo 3 IV trinuclear ion [Mo3S4(H2O)9]4+ to give cuboidal complexes of the kind Mo3MS4, or related edge-linked species {Mo3MS4}2, or corner-shared Mo3S4MS4Mo3 double cubes, depending on the heteroatom used. All of the products formed can be obtained as aqua ions. With four recent additions there are now 15 different heterometal atoms participating in this chemistry from Cr in Group 6 to Bi in Group 15. Preparative procedures, X-ray crystal structures, and distinctive properties including UV-Vis spectra, elution characteristics using Dowexcation exchange chromatography, ICP metal analyses, and the stoichiometries of reactions in which the heterometallic product is oxidized back to [Mo3S4(H2O)9]4+ (with release of the heterometal in an ionic form) are considered.
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    Synthetic Methodologies and Structures of Metal-[C60]Fullerene Complexes (1998)
    Springer
    Journal of cluster science 9 (1998), S. 393-415 
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    ISSN: 1572-8862
    Keywords: Fullerene ; transition-metal ; complex ; synthesis ; structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract A review of the chemistry of transition metal-[C60]fullerene complexes is presented. The main focus is directed toward the different methodologies for obtaining both metal bound and ligand bound complexes of C60, and the different types of structures which have been so far identified for metal-C60 complexes.
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    Organometallic and coordination chemistry on phosphazenes. III. Synthesis, characterization, and electrochemical behavior of transition metal-cinnamonitrile cyclophosphazene derivatives (1996)
    Springer
    Journal of inorganic and organometallic polymers and materials 6 (1996), S. 145-170 
    Details
    ISSN: 1572-8870
    Keywords: Phosphazenes ; coordination chemistry ; synthesis ; electrochemical behavior ; transition metal ; cinnamonitrile cyclophosphazene
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Hexakist 4-formylphenoxy cyclophosphazene (1) reacts with six equivalents of cyanomethylenetriphenylphosphorane to give hexakist 4-cinnamonitrile cyclotriphosphazene bearing 12 functional groups tsix nitriles and six olefins' able to coordinate up to 12 metals. In this way a series of polynuclear phosphazene metal derivatives (8–12) was prepared with different transition metals and in different oxidation states. Pt(0), Pt(II) and Rh(I). The analogous cinnamonitrile derivatives (3–7) were prepared and used as models for the characterization of corresponding phosphazene compounds. The redox properties of the complexes3–5 and8–10 as well as of the free cinnamonitrile2 and the free substituted cyclophosphazene1 have been investigated by cyclic voltammetry (CV) and controlled potential electrolysis (CPE) in aprotic media (THF, CH2Cl2, or NCMe 0.2M [NBu4][BF4]), at Pt electrodes. Cathodic processes have been detected only when the unsaturated C=C bond of the cinnamonitrile group is uncoordinated: hence, for compounds1. 4. and9. they are irreversible occur at potentialsE p red ca. −1.3 to ca. −1.9V vs SCE which are less cathodic than that exhibited by the free cinnamonitrile (2:E p red ca. −2.0 V vs SCE), and are believed to be centered at the electron-acceptor emptyπ * (C=C) orbital of each of the cinnamonitrile groups present in the molecule. Anodic processes are displayed only by complexes3. 5. 8. and10 with at least one Pt(0) site: they are irreversible, conceivably centered at such a metal center, and occur at potentials (E p bv ca. 0.7 1.2 V vs SCE) which are dependent on the electronic effects of the ligands, in particular the strong electron-withdrawing ability of the cyclophosphazene group. Complex10 undergoes dissociation in NCMe to form9 and possibly solvated [Pt(PPh3)2] species which adsorb at the electrode surface. No evidence for any redox process centered at the phosphazene ring has been found.
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    Highly stereoselective sodium borohydride promoted reduction ofendo-5-acetyl-1,2,3,4-tetrachloro-7,7-dimethoxynorborn-2-ene (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 657-660 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; norbornene ; stereoselective reduction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Racemicendo-5-acetyl-1,2,3,4-tetrachloro-7,7-dimethoxynorborn-2-ene was stereoselectively reduced by sodium borohydride to give only theS,S orR,R diastereomers. The crystal structure of the product displays no unusual features.
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    Structure of 2-acetoxy-1,2-di(1-adamantyl)ethanone (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 291-294 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; 1,2-di(1-adamantyl)ethene
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The structure of 2-acetoxy-1,2-di(1-adamantyl)ethanone is reported. The steric requirements of the two adamantyl groups affect the structure in three ways—a slight elongation of the central bond, a small expansion of the angles about the central bond, and a conformation in which the C(sp2)-connected adamantyl group virtually bisects the large substituents attached to the sp3 carbon.
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    Structure of a PCU-derived pinacol formed via sodiumpromoted reductive dimerization of pentacyclo[5.4.0.02,6.03,10.05,9]undecane-8,11-dione monoethylene ketal (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 517-520 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; pinacol ; reductive dimerization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The pinacol resulting from sodium promoted reductive coupling of pentacyclo[5.4.0.02,6.-03,10.05,9]undecane-8,11-dione monoethylene ketal possesses a conformation, dictated by intramolecular hydrogen bonding, that lies midway between eclipsed and staggered. The C−C and C−O distances in the pinacol unit are, respectively, longer and shorter than usual, and all parameters are as expected.
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    Crystal and molecular structure determination, TGA-DTA, and infrared and Raman spectra of rubidium nitroprusside, Rb2[Fe(CN)5NO] (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 325-330 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; rubidium nitroprusside ; IR ; Raman ; thermal analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound, Rb2[Fe(CN)5NO], crystallizes in the space group P212121, witha=5.687(1),b=15.956(2),c=12.645(3) Å, andZ=4. Anions are in equivalent C1 sites (one per asymmetric unit) and are slightly distorted octahedra (C4v ideal symmetry). TGA and DTA curves and vibrational (infrared and Raman) spectra of Rb2[Fe(CN)5NO] were obtained. Results are interpreted in view of the crystal structure of the compound and the behavior of related substances.
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    Thermodynamic vs. kinetic control in the Diels-Alder cycloaddition of cyclopentadiene to 2,3-dicyano-p-benzoquinone (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 281-286 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; cyclopentadiene ; 2,3-dicyano-p-benzoquinone ; Diels-Alder reaction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Diels-Alder cycloaddition of cyclopentadiene (1a) to 2,3-dicyano-p-benzoquinone (2a), when performed in methanol solvent at ambient temperature, proceeds with kinetic control to afford 1α,4α,4aβ,8aβ-tetrahydro-5,8-dioxo-1,4-methanonaphthalene-4a,8a-dicarbonitrile (7, 77% yield). However, when this cycloaddition is performed by refluxing an equimolar solution of1a and2a in benzene for 3 h, the product of thermodynamic control, i.e., 1α,4α,4aα,8aα-tetrahydro-5,8-dioxo-1,4-methanonaphthalene-6,7-dicarbonitrile (3a) is obtained in 64% yield. The structure of3a was confirmed by an analysis of the reduced intramolecular photocyclization product,9.
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    Crystal and molecular structure of (2E,4S,10R)-4-hydroxy-2-undecen-10-olide (nor-patulolide C), C11H18O3 (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 305-308 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; undecen-olid ; nor-patulolide
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The stereogeometry and absolute configuration of the title compound has been proved by an X-ray diffraction analysis. Crystal data: monoclinic, P21,a=7.7976(2),b=7.8288(2),c=8.9791(4) Å, β=90.331(4)o, Z=2. The crystal structure has been solved by vector search methods and refined toR=0.042 for 1798 observed reflections.
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    Crystal and molecular structure of diphenylphosphinylacetic acid (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 361-364 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; carboxylic acid ; phosphine oxide ; hydrogen bonding
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Diphenylphosphinylacetic acid crystallizes in the monoclinic space groupP2l/n with unit cell dimensionsa=5.6875(7),b=17.049(4),c=13.471(2) Å, β=93.36(1)° and Z=4. The molecular packing consists of hydrogen bonded chains arising from intermolecular interactions between a carboxylic acid hydroxyl group and an oxygen of an adjacent phosphine oxide moiety.
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  • 39
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    Tetracyclo[6.3.0.04,11.05,9]undecane-2,7-dione (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 425-428 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; tetracyclo[6.3.0.04,11.05,9]undecane-2,7-dione
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The compound crystallizes in the triclinic space group, $$P\bar 1$$ , witha=6.7702(4),b=7.0180(4),c=9.1960(7) Å, α=92.457(6), β=96.150(6), γ=93.444(5)°, andZ=2. The structure contains a rather short intramolecular H...H contact of 2.26(4) Å.
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    Structure of a binuclear silver(I) complex [Ph3PAg(O2CCH2Ph)]2 (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 553-557 
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    ISSN: 1572-8854
    Keywords: Silver(I) complex ; synthesis ; crystal structure ; spectroscopic properties
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The reaction of [Ph3PAgI]4 with sodium phenylacetate in MeOH and CH2Cl2 at room temperature gave rise to a binuclear silver complex with triphenylphosphine and phenylacetate mixed ligands, [Ph3PAg(O2CCH2Ph)]2. The crystal and molecular structure of the complex has been determined by single crystal X-ray diffraction analysis. The space group is $$P\bar 1$$ witha=9.198(2),b=9.516(2),c=13.842(3) Å, α=102.00(3), β=108.34(3), γ=93.58(3)°,Z=1, andDc=1.506 g cm−3. The silver atoms are each coordinated by one phosphorus atom from triphenylphosphine and two oxygen atoms from the carboxylate groups in a T-shape. The complex is further characterized by its IR,1H, and31P NMR spectra.
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    Crystal structure of strontium potassium arsenate octahydrate (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 741-746 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; hydrated ions ; ionic hydration ; strontium arsenate ; struvites ; struvite-type structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal structure of strontium potassium arsenate octahydrate, SrKAsO4·8H2O, has been determined by single crystal X-ray diffraction. The crystals are tetragonal, a = 7.144(1), c = 23.613(2) Å, space group I41md (No. 109), Z = 4, V = 1205.1(1) Å3, and d c = 2.258 g cm−3. All cations and anions in this compound are completely surrounded by water molecules. Sr2+ and K+ ions are each coordinated to eight water molecules arranged in an approximately square antiprism. The [Sr(H2O)8]2+ polyhedron shares one face of four water molecules with a [K(H2O)8]+ polyhedron forming O4-Sr-O4-K-O4 polyhedra. The O4-Sr-O4-K-O4 units are linked together through a pair of edge-sharing linkages of the outer water molecules, alternating along the a-axis and b-axis. The hydrated cation polyhedra appear to define the host lattice, which accommodates the AsO 4 3- ion in the interstitial space. The environment of the AsO 4 3- ion consists of 16 water molecules; each oxygen atom is the acceptor in hydrogen bonds from four water molecules. The pair distances associated with this environment may be used in investigations of the structure of hydrated 4 n- ions in solutions. Each water molecule is coordinated to one Sr and one K, and hydrogen bonded to two O atoms of two different AsO 4 3- ions. There is no hydrogen bonding between water molecules.
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    Crystal structures of a series of 3,7-bis-(arylazo)-1,3,5,7-tetraazabicyclo[3.3.1]nonanes (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 797-809 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; bicyclononane ; triazene ; bis-triazene ; nitrile substituent ; nitro substituent ; trifluoromethyl substituent ; hydrogen bonding
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal and molecular structure of a series of 3,7-bis(arylazo)-1,3,5,7-tetraazabicyclo[3.3.1] nonanes (1a–d) have been determined by single crystal X-ray diffraction analysis. All four compounds have the same feature, that the tetraazabicyclononane unit assumes a cage-like structure with the aryltriazene moieties lying parallel to one another so that the aryl rings are held together by π – π stacking. Crystal data: 1a C17H18N10O4, triclinic, space group P − 1, a = 9.8899(10), b = 13.0845(13), c = 16.458(2) Å, α = 94.095(2)°, β = 107.004(2)°, γ = 111.027(2)°, V = 1863.5(3) Å3 and Z = 4; 1b, C19H18F6N8, orthorhombic, space group Pbca, a = 15.3210(8), b = 10.9512(6), c = 24.5698(13) Å, V = 4122.4(4) Å3 and Z = 8; 1c C19H18N10, monoclinic, space group P21/n a = 6.3742(6), b = 13.7343(13), c = 21.542(2)Å, β = 97.738(2)°, V = 1868.8(3) Å3, and Z = 4; 1d, C19H18N10, monoclinic, space group P21/c, a = 18.205(2), b = 17.398(2), c = 12.784(12) Å, β = 109.480(2)°, V = 3818.0(6) Å3, and Z = 8.
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    Characterization and structural analyses of trimethoxy and triethoxybenzo[b]thiophene (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 289-295 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; centrosymmetric ; methoxybenzo [b] thiophene ; estrogen receptor ; tubulin
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal and molecular structures of two methoxybenzo [b] thiophenes have been determined by three-dimensional, single-crystal X-ray diffractometry. Both 3-(3′,4′,5′-trimethoxybenzoyl)-2-(4′-methoxyphenyl)-6-methoxybenzo[b]thiophene and 3-(3′,4′,5′-triethoxybenzoyl)-2-(4′-methoxyphenyl)-6-methoxybenzo[b]thiophene (hereafter referred to as I and II, respectively) crystallize in the triclinic centrosymmetric space group $$P \bar 1$$ (No. 2, C1) with two formula units per cell with a = 6.842(1) Å, b = 12.602(2) Å, c = 13.815(2) Å, α = 94.80(1)°, β = 98.27(2)°, and γ = 100.59(2)° and a = 10.600(1), b = 11.415(2), c = 12.137(2) Å, α = 94.57(1)°, β = 101.18(1)°, and γ = 110.45(1)°, respectively. The phase problems were solved by direct methods and the respective final full-matrix least-squares refinements converged to R = 0.039 and 0.068. The structures differ in the orientation of the trimethoxy and triethoxy groups of the benzoyl ligands. The molecules in the crystal lattice are held together by van der Waals forces. Selected bond distances, angles, and torsion angles are tabularized as well as reference to the synthesis of the title compounds and peripheral studies.
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  • 44
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    Synthesis and crystal structure of a polymeric erbium(III)–sodium(I) coordination complex of picolinic acid N-oxide (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 413-418 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; coordination polymer ; erbium(III)–sodium(I) carboxylate complex ; picolinic acid N-oxide
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract A new Er(III)–Na(I) coordination polymer of stoichiometry [NaEr2L5(H2O)6(NO3)](NO3)·3.5H2O (HL = picolinic acid N-oxide) has been synthesized and characterized by single-crystal X-ray analysis. Crystals are triclinic, PĪ with a = 9.823(2), b = 12.453(2), c = 20.643(4) Å; α = 98.49(3), (β = 101.40(3), γ = 108.69(3)°; V = 2284(1) Å3; Z = 2. Of the two independent eight-coordinate erbium(III) ions in this complex, one is surrounded by four bidentate chelating L ligands, and the other by one bidentate chelating L ligand, four aqua ligands and two anti-carboxylate oxygen atoms from two neighboring [ErL4] units. The sodium(I) ion is in a distorted octahedral environment, being coordinated by a unidentate nitrate anion, three aqua ligands and two anti-carboxylate oxygen atoms from two adjacent [ErL4] units. The complex is built from zigzag chains of syn-anti carboxylate-bridged erbium(III) moieties directed in the a direction, which are cross-linked pairwise by aqua-bridgeddimericsodium(I) units. The resulting composite polymeric chains are further connected by hydrogen bonds to form a three-dimensional network.
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  • 45
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    Crystal structure and two-stage hydrolysis of dimethoxo (meso-tetra(4-methoxyphenylporphyrinato))tin(IV), Sn(tmpp)(OMe)2 (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 481-486 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; tin porphyrin ; two-stage hydrolysis ; methanolate ; trans equivalent axial ligand
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract In this work, we determine the crystal structure of dimethoxo(meso-tetra(4-methoxyphenylporphyrinato))tin(IV), Sn(tmpp)(OMe)2 (1). Experimental results indicate that the tin atom has an octahedral geometry. The geometry around the tin center has Sn(1)–O(5) = 2.020(6), Sn(1)–O(6) = 2.003(7) Å and an average Sn(1)–N = 2.10(1) Å. The two methoxo groups are unidentately coordinated to the tin(IV) atom. Two-stage hydrolysis of Sn(tmpp)(OMe)2 in CDCl3 was observed by 1H and 13C NMR spectroscopy. Compound (1) crystallizes in the space group P21/n with a = 14.7492(1), b = 19.2022(3), c = 16.0806(2) Å, β = 94.104(1)°, and Z = 4.
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    Synthesis and structural characterization of a novel polymeric gadolinium(III)–copper(II) complex of iminodiacetic acid (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 475-479 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; coordination polymer ; gadolinium(III)-copper(II) complex ; iminodiacetic acid
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract A novel polymeric Gd2Cu3 complex of iminodiacetic acid (H2L1=NH{CH2COOH}2), namely, Gd2Cu3(L1)6, 1, has been synthesized and structurally characterized. In the title complex, the Gd3+ ion is nine-coordinated by six O atoms from three bidentate chelating carboxylate groups and three O atoms from three anti-anti bridging carboxylic groups of six L1 ligands; the Cu2+ ion is six-coordinated by four O and two N atoms from two chelating L1 ligands. Each pair of Gd(III) atoms is bridged by three L1 ligands, each of which also chelates with one copper(II) ion, thus forming a Gd2Cu3 cluster unit. Such cluster units are cross-linked by flexible L1 ligands into a three-dimensional coordination framework. The title complex crystallizes in the trigonal space group P-3c1 (No. 165) with a = b = 13.433(4), c = 14.770(6) Å; V = 2308(1) Å3; Dcalca = 1.859 g cm−3; Z = 2.
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    Structure of a deaza dimer of 4-methyl-3H-1,2,4-triazole-3,5(4H)-dione (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 15-18 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; dimer ; triazole
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound crystallizes in the monoclinic space group, P21/n; a = 9.0024(5), b = 5.8135(3), c = 15.2232(8) Å, β = 91.153(4)° Z = 4; and R = 0.050 based on 853 observed, unique reflections. The structure consists of two fused five-membered triazole rings, oriented relative to each other at 152°.
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    Crystal structures of two substituted biphenyl derivatives: 5,5′-di t-butyl-2-2′-biphenyldiol and 5,5′-dimethyl-2,2′-biphenyldiol (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 157-161 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; biphenyl ; mutual orientation ; strong H-bonds
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract 5,5′-Di t-butyl-2,2′-biphenyldiol (I), C20H26O2, crystallizes in the orthorhombic space group P212121 with a = 18.243(2), b = 9.947(2), c = 9.685(3) Å, and Z = 4; 5,5′-dimethyl-2,2′-biphenyldiol (II), C14H14O2, crystallizes in the monoclinic space group P21/c with a = 9.959(2), b = 7.932(3), c = 15.392(2) Å, β = 105.43(2)°, and Z = 4. The aromatic rings are tilted by 52.7(1) and 43.8(1)° to each other in compounds (I) and (II), respectively. Strong intra- and inter-molecular H-bonds connect the molecules in the crystals.
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    Synthesis, spectroscopic studies, and crystal structure of tris(tetra-n-butylammonium) hexakisisothiocyanatoindate(III) (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 317-321 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; indium complexes ; isothiocyanate complexes ; octahedral coordination
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The reaction of a 1:10 molar ratio between indium chloride and tetra-n-butylammonium thiocyanate in ethanol affords the complex [(n-C4H9)4N]3[In(NCS)6] (1), the structure of which has been established by X-ray diffraction. This compound crystallizes in the cubic space group Pa3¯ with eight formula units in the unit cell. The formula unit consists of three separate cationic tetra-n-butylammonium groups and an independent hexakisisothiocyanatoindium anionic group. The six near linear thiocyanate ligands coordinate octahedrally through the nitrogen atom to the indium metal center. The coordination of the n-butyl groups to the ammonium-nitrogen atom is tetrahedral. The complex has also been characterized by IR, 1H and 13C NMR, physical properties, and X-ray powder analysis.
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    Crystal structures of a series of 3,8-di[-2-aryl-1-azenyl]-1,3,6,8-tetraazabicyclo[4.4.1]undecanes (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 145-156 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; bicycloundecane ; triazene ; bis-triazene ; nitro substituent ; carboalkoxy substituent ; π–π stacking
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal and molecular structure of a series of 3,8-di[-2-aryl-1-azenyl]-1,3,6,8-tetraazabicyclo[4.4.1]undecanes (1–5) have been determined by single crystal X-ray diffraction analysis. In all five compounds, the tetraazabicycloundecane portion of the molecule assumes a cage-like, folded structure with the aryltriazene moieties aligned approximately parallel; the structure is held in the folded configuration by either intramolecular or intermolecular π–π stacking forces. Crystal data: 1 C19H22N10O4, monoclinic space group P21/c, a = 10.1846(7), b = 9.9556(7), c = 20.819(2) Å, β = 98.725(1)°, V = 2086.5 (3) Å3, Z = 4; 2 C23H28N8O4, triclinic, space group Pī, a = 6.7064(7), b = 12.9662(14), c = 14.054(2) Å, α = 94.796(2), β = 91.621(2), γ = 104.836(2)°, V = 1175.7(2) Å3, Z = 2; 3 C19H22N10O4, monoclinic, space group P21/c, a = 14.237(2), b = 13.520(2), c = 11.5805(12) Å, β = 113.514(2)°, V = 2044.0(4) Å3, Z = 4; 4 C21H22N10, monoclinic, space group C2/c, a = 54.247(3), b = 11.5531(7), c = 12.9670(7) Å, β = 95.710(1)°, V = 8086.4(8) Å3, Z = 16; 5 C25H32N8 04, monoclinic, space group P21/c, a = 10.2908(7), b = 16.5687(12), c = 15.1662(10) Å, β = 94,188(1)°, V = 2579.0(3) Å3, Z = 4.
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    Synthesis and crystal structure of 4,5-dibromo[2.1.1]triblattene (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 351-354 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; dibromotriblattene
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Reaction of 4-bromopentacyclo[7.3.0.02,7.03,11.06,10]dodec-11-ene (1) with Br2—CCl4 afforded 4,4,5-tribromopentacyclo[7.3.0.02,7.03,11.06,10]dodecane (2) in 89–94% yield. Subsequent treatment of 2 with KOt-Bu-t-BuOH resulted in competitive elimination of the elements of HBr and of Br2 with concomitant formation of 4,5-dibromopentacyclo[7.3.0.02,7.03,11.06,10]dodec-11-ene (3, 76%) and 1 (17%), respectively. The structure of 3 was established unequivocally via application of X-ray crystallographic methods. Crystal data for 3: monoclinic, C2/c, a = 9.895(1), b = 9.0963(7), c = 12.471(1) Å, β = 106.875(8)°, z = 4.
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    Synthesis and structural characterization of [VS4(CuPPh3)4Br]·CH2Cl2 (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 375-381 
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    ISSN: 1572-8854
    Keywords: synthesis ; molecular structure ; tetrathiovanadate ; copper ; cluster
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Heating a solid mixture of (NH4)3VS4, CuCl, PPh3, and NEt4Br at 100°C for 10 h and extraction with CH2Cl2 yielded [VS4(CuPPh3)4Br]·CH2Cl2. Crystallographic data: Triclinic, P1¯, a = 15.189(3), b = 20.093(6), c = 12.031(3) Å, α = 102.39(2), β = 100.05(2), γ = 82.86(2)°, V = 3517(3) Å3, and Z = 2. The configuration of the VS4Cu4Br core can be described as a distorted cubane with an additional face. The V atom has retained the tetrahedral geometry of the free [VS4]3− moiety. The four Cu atoms have three different coordination environments, strongly distorted tetrahedral, nearly trigonal planar, and strictly trigonal planar. The infrared, electronic, and 51V NMR spectra have also been reported.
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    Synthesis, crystal structure, and molecular modeling (AM1) of Methyl 6-chloro-4-(2-chlorophenyl)-5-formyl-2-methyl-1, 4-dihydropyridine-3-carboxylate (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 237-243 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; AM1 ; x-ray diffraction ; dihydropiridines
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The synthesis and structural characterization of Methyl 6-chloro-4-(2-chlorophenyl)-5-formyl-2-methyl-1,4-dihydropyridine-3-carboxylate is described. The structure was refined to R1 = 0.0470 for 2665 reflections (with I 〉 2σ(I)). Crystal data: C15H13C12NO3, monoclinic,space group P21/c, a = 11.163(9), b = 14.484(8), c = 9.422(7) Å, V = 1512.9(19) Å3, Z = 4. The results of crystallographic and molecular modeling (AM1) were compared. The Cl atom attached to the phenyl group has two possible orientations, having 75% (sp) and 25% (ap) occupancy, respectively. The molecules in the crystal are held together by means of intermolecular hydrogen bonds of the type N=H...O and by C=H...O interactions.
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    Synthesis and crystal structure of a tetranuclear manganese(IV) cluster [L4Mn4O6](ClO4)4·2H2O (L = 1,4,7-triazacyclononane) (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 251-254 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; manganese(IV) cluster ; adamantane-shaped complex ; tetranuclear complex
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract A tetranuclear manganese (IV) complex, [L4Mn4O6](ClO4)4·2H2O (1), with 1,4,7-triazacyclononane (L) as the capping ligands, has been synthesized and characterized by X-ray diffraction; monoclinic, space group P21/n with a = 21.335(6) Å, b = 11.387(3) Å, c = 21.788 (6) Å, β = 111.410 (6)°, V = 4928 (2) Å, Z = 4. Each manganese atom has a distorted octahedral environment comprised of three facially coordinated amine nitrogen atoms and three oxygen atoms, and the cation is an idealized tetrahedron. The Mn4O6 4+ cation corresponds to an adamantane skeleton.
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    Multifunctional carbochain organosilicon polymers. I. A new approach to the synthesis of high molecular weight cyclolinear polycarbosiloxane (1995)
    Springer
    Journal of inorganic and organometallic polymers and materials 5 (1995), S. 123-133 
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    ISSN: 1572-8870
    Keywords: Multifunctional polymer ; cyclolinear polycarbosiloxane ; polyvinyldimethylphenylsilane ; polyvinyldimethylchlorosilane ; replacement ; hydrolytic condensation ; synthesis ; characterization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Controlled synthesis of high molecular weight cyclolinear polycarbosiloxanes (PCCS) is considered, using the following reactions sequence: (1) anionic polymerization of vinyldimethylphenylsilane, (2) replacement of the Ph group in polyvinyldimethylphenylsilane (M n=83.900,M w/M n=1.48) by a Cl group to prepare polyvinyldimethylchlorosilane (PVMCS), and (3) hydrolytic intramolecular condensation of PVMCS. The formation of carbochain polymer with predominantly six-membered carbosiloxane rings is demonstrated (M n=81.400,M w/M n=1.54).
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    Structure of a C2-symmetric bis(benzyloxy)trishomocubanone (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 747-750 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; trishomocubanone
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The structure of a bis(benzyloxy)trishomocubanone with molecular C2 symmetry reveals that substitution of benzyloxy groups has little effect on the trishomocubane cage.
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    Crystal structure of ethyl 4-methylthio-3-phenyl-2-thioxo-2,3-dihydro-1,3-oxazole-5-carboxylate (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 237-240 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; 1,3-oxazoline-2-thione ; resonance structures
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound C13H13NO3S2 crystallizes in the triclinic space group $$P\bar 1$$ (Z=2) with lattice constantsa=8.382(2),b=10.042(2),c=10.134(2) Å, α=119.35(1)°, β=101.40(1)° and γ=90.54(1)°. The interplanar angle between the least squares planes of the 1,3-oxazoline ring and the phenyl ring amounts to 90.2°, thus hindering conjugation between the benzene and heterocyclic system. The observed bond parameters of the five-membered heterocycle suggest a significant contribution from a zwitterionic dipolar limiting structure [38.7(5)%] to the description of this ring system. The particular contributions of the resonance structures were estimated by calculations using the HOSE model on the base of the observed bond lengths.
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    Synthesis and structure ofexo-11-cyano-endo-11-(trimethylsilyloxy)pentacyclo[5.4.0.02,6.03,10.05,9]undecan-8-one (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 267-271 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; pentacycloundecan-8-one ; pentacycloundecane-8,11-dione
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal structure of an asymmetric pentacyclo[5.4.0.02,6.03,10.05,9]undecan-8,11-dione derivative is reported, in which Me3SiCN has been added across one of the keto groups. The cage structure demonstrates the expected effects of this addition.
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    Structure of the product formed via Cu(I)-promoted oxidative dimerization ofexo-8-ethynylpentacyclo[5.4.0.02,6.03,10.05.9]undecan-endo-8-ol (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 543-547 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; diyne ; oxidative dimerization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The structure consists of two acetyl-substituted PCU cages linked by a diyne fragment. The conformation about the linker is midway between staggered and eclipsed, and the acetyl groups are somewhat distorted due to the proximity to the bulky cage units.
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    Crystal structure oftrans-tetrachlorobis[2-(2-1H-imidazolyl)-1H-imidazolium]cadmium(II), [Cd(H3biim)2Cl4] (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 695-699 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; 2,2'-bi-1H-imidazole ; cadmium chloride
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The reaction between cadmium(II) chloride and 2,2'-bi-1H-imidazole (H2biim) in an acidic solution affords [Cd(H3biim)2Cl4] (H3biim=2-(2-1H-imidazolyl)-1H-imidazolium) in 63% yield. The compound crystallizes in the triclinic space groupP1, wherea=8.072(2),b=8.100(2),c=8.593(2) Å, α=75.89(2), β=62.94(2), γ=63.29(1)°,V=446.4(2) Å3, andZ=1. The central Cd atom exhibits an octahedral geometry composed of a Cl4N2 core. The Cd-N bond distance is 2.392(2) Å. Cd−Cl distances are 2.5919(9) and 2.671(1) Å.
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    X-ray structures of two methoxybenzo[b]thiophenes (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 801-806 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; centrosymmetric ; methoxybenzo[b]thiophene ; estrogen receptor ; tubulin
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal and molecular structures of two methoxybenzo[b]thiophenes have been determined by three-dimensional, single-crystal X-ray diffractometry. Both 3-(4′-hydroxy-3′, 5′-dimethoxybenzoyl)-2-(4′-methoxyphenyl)-6-methoxybenzo[b]thiophene and 3-(2′,6′-dimethoxybenzoyl)-2-(4′-methoxyphenyl)-6-methoxybenzo[b]thiophene (hereafter referred to asI andII, respectively) crystallize in the monoclinic centrosymmetric space groupP21/n (No. 14, C 2h 5 ) with four formula units-per cell witha=6.866(1),b=28.638(2),c=11.830(2) Å, and β=105.52(1)° anda=9.328(1),b=7.977(1),c=29.650(4) Å, and β=97.87(1)°, respectively. The phase problems were solved by direct methods and the respective final full-matrix least-squares refinements converged toR=0.046 and 0.031. The structures differ in the positioning of the dimethoxy groups of the benzoyl ligands and the addition of a hydroxyl group inI. The molecules in the crystal lattice are held together by van der Waals forces plus the addition of hydrogen bonding in compoundI. Selected bond distances and angles and torsion angles are tabularized.
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    Crystal and molecular structure of β-resorcylidene aminoguanidine copper(II) complex (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 841-846 
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    ISSN: 1572-8854
    Keywords: Cu(II) resorcylidene aminoguanidine ; synthesis ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The tridentate Schiff base, β-resorcylidene aminoguanidine (RAG)1 was synthesized from 2,4-dihydroxybenzaldehyde and aminoguanidine and complexed with copper(II) to form a copper(II)-β-resorcylidene aminoguanidine (Cu-RAG)2 complex. X-ray diffraction analysis of compound2 (orthorhombic, Pnma,a=11.674(1);b=6.7198(7);c=17.836(2) Å) revealed a square-planar copper(II) cation with a tridentate·ligand bound through two nitrogen atoms (N1 and N3) of the aminoguanidine moiety and an oxygen (O1) of the monodeprotonated dihydroxybenzaldehyde function. The remaining coordination site was occupied by chloride and the structure was rigidly planar as demanded by the restrictions of the crystallographic space group. The unit cell contents exhibited an extended sheet-like structure constructed via hydrogen bonds both intermolecularly and involving two water molecules (O3 and O4) also restricted by the same mirror symmetry. The remaining water (O5) provided for interlayer hydrogen bonding.
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    Reaction of vinylmagnesium bromide with hexacyclo[10.2.1.02,11.04,9.04,14.09,13]pentadeca-5,7-diene-3,10-dione: Transannular hemiketal formation (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 429-433 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; hexacyclopentadeca-5,7-diene-3,10-dione
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Reaction between vinylmagnesium bromide and the cage dione leads to attack of only one equivalent of Grignard and intramolecular nucleophilic attack on the second ketone. The product compound crystallizes in the monoclinic space group, P21/a, witha=9.509(1),b=11.071(2),c=12.492(4) Å, β=104.32(2)°, andZ=4.
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    The crystal and molecular structure of 6,8,15,16b,16c,17-hexahydro-16b,16c-diphenyl-7H,16H-6a,7a,15a,16a-tetraazanaphtho[5,6]azulano[2,1,8-ij]naptho[f]azulene-7,16-dione (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 365-368 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; receptor ; clip shaped molecule
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal and molecular structure of a clip containing molecule is described. The structure was solved by vector search methods and refined by least squares methods toR l=0.0768 [I〉2σ(I)]. Crystal data: C40H30N4O2·HCCl3, triclinic, space group $$P\bar 1$$ ,a=9.302(2),b=12.981(2),c=15.765(2)Å, α=65.91(2)°, β=76.40(2)°, γ=80.15(1)°,V=1682.9(4)Å3, Z=2.
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    Synthesis and X-ray analysis of 1-((1S)-phenylethyl)-azetidine-(2R)-piperidinamide (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 639-642 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; chiral auxiliaries
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal and molecular structure of a new azetidine-2-carboxylic amide derivative is described. The structure was solved by direct methods and refined by least squares methods toR1=0.0393 for 4264 reflections (withI〉2σ(I)) The structure consists of two independent molecules which are chemically the same with slight differences in geometry. Crystal data: C17H24N2O, monoclinic, space groupP21,a=8.3782(4),b=20.0342(13),c=9.7769(8) Å, β=109.687(6)°,V=1545.1(2)Å3,Z=4.
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    Crystal structures of two 1,2-bis-(1-aryl-3-methyltriazene-3-yl-)ethanes with aryl substituents of opposite polarity (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 5-10 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; triazene ; bis-triazene ; nitrile substituent ; methoxy substituent ; hydrogen bonding
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal and molecular structure of 1,2-bis-{1-(2-cyanophenyl)-3-methyltriazen-3-yl-}ethane (1) and 1,2-bis-{1-(2-methoxyphenyl)-3-methyltriazen-3-yl-}ethane (2) have been determined by single crystal X-ray diffraction analysis. Bis-triazene (1) exists as the “staggered” conformation in the solid state, with an anti-anti configuration around the N2–N3 bond of the triazene units, whereas 2 assumes a “gauche” conformation with the syn-syn configuration in the triazene units. Crystal data: 1 C18H18N8, triclinic, space group P −1, a = 6.108(2), b = 8.118(3), c = 9.600(4)Å, α = 101.37(7)°, β = 96.47(7)°, γ = 102.71(5)°, V = 449.1(3)Å3, Z = 2; 2 C18H24N6O2, monoclinic, space group P 21/n, a = 13.119(5), b = 7.745(2), c = 19.201(2)Å, β = 96.47(7)°, V = 1910.3(9)Å3, Z = 4.
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    Crystal structures of the hydrated disodium and paraquat salts of 1,8-disulfonato-3,4,5,6-acridinetetracarboxylic acid (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 39-46 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; 1,8-disulfonato-3,4,5,6-acridinetetracarboxylic acid ; 3,4,5,6-tetracarboxyacridine-1,8-disulfonate ; paraquat ; hydrate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Two hydrated salts of 1,8-disulfonato-3,4,5,6-acridinetetracarboxylic acid, H2L, have been characterized by single-crystal X-ray analysis. Compound 1, Na2L·9 $$ - \frac{1}{2}$$ H2O, crystallizes in the monoclinic space group C2/c with a = 42.005(1), b = 6.838(1), c = 23.807 (1) Å, β = 122.71 (1)°, and Z = 8. Compound 2, (paraquat)L·2H2O, belongs to the triclinic space group $${P\bar 1}$$ with a = 9.940(1), b = 11.543(1), c = 14.033(1) Å, α = 105.45(1), β = 95.82(1), γ = 100.14(1)° and and Z = 2. All four carboxyl groups in the 3,4,5,6-tetracarboxyacridine-1,8-disulfonate dianion L2− are un-ionized. In 1 the distorted octahedrally coordinated sodium cations, the anions, and the lattice water molecules are joined together by hydrogen bonds to generate a three-dimensional network. In the crystal structure of 2, a host framework composed of L2− ions and water molecules accommodate the paraquat dications within two channel systems running parallel to the a and b axes.
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    Crystal structures of four dibromomethylene-functionalized cage compounds (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 259-266 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; heptacyclotetradecane ; hexacyclotetradecane
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Crystal structures of four dibromomethylene-functionalized hexa- and heptacyclotetradecane cages are reported. 7-(Dibromomethylene)heptacyclo[6.6.0.02,6.03,13.04,11.05,9.010,14]tetradecane (3): orthorhombic, Pnma, a = 14.744(1), b = 11.237(1), c = 7.4625(7) Å Z = 4; R = 0.0531 for 504 observed reflections. 7,12-Bis(dibromomethylene)heptacyclo[6.6.0.02,6.03,13-04,11 .05,9.010,14]tetradecane (4): monoclinic, I2/a, a = 11.257(1), b = 9.5844(8), c = 13.884(2) Å, β = 92.254(8)° Z = 4; R = 0.0413 for 663 observed reflections. 10,14-bis(dibromomethylene)hexacyclo[6.6.0.02,6.03,13.04,11.05,9]tetradecane (6): monoclinic, P21/n, a = 8.118(1), b = 15.273(4), c = 12.826(3) Å, β = 104.20(1)° Z = 4; R = 0.0384 for 1392 observed reflections. 14-(dibromomethylene)hexacyclo[6.6.0.02,6.03,13.04,11.05,9]tetradecan-10-one (7): monoclinic, P21/n, a = 8.2879(7), b = 15.273(1), c = 10.0565(9) Å, β = 92.271(8)° Z = 4; R = 0.0320 for 1402 observed reflections. The functional groups lead to slight shortening of bond lengths.
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    A dinuclear cyano-bridged complex based on hexacyanoferrate(III) and samarium(III) nitrate: synthesis and crystal structure (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 303-307 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; samarium(III) complexes ; iron(III) complexes ; cyanide-bridges ; dinuclear complexes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract A new complex, [Sm(DMF)4(H2O)4Fe(CN)6]·H2O (DMF = N, N-dimethylformamide), has been synthesized and characterized by X-ray single crystal structure and thermogravimetric analyses. The complex crystallizes in the P21/n space group, with lattice parameters a = 17.583(4) Å, b = 8.870(2) Å, c = 19.845(6) Å, β = 95.98(3)°, V = 3078(1) Å3, D x = 1.679 Mg m−3, D m = 1.65(1) Mg m−3, Z = 4. The molecular structure shows that a cyano-bridged bimetallic structure is obtained. The Sm atom is coordinated by eight oxygen atoms of four water molecules and four DMF molecules and one nitrogen atom of the bridging cyanide ligand. The iron atom assumes approximately an octahedral environment surrounded by six CN ligands. The hydrate water molecule is hydrogen-bonded to one of the O atoms bound to Sm. Each terminal CN ligand of the Fe(CN) 6 3− entity is hydrogen-bonded to some O atoms of water molecules. An infrared spectrum is also reported.
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    Gold(III)-pteridine compounds: synthesis, spectral, and X-ray diffraction studies on new adducts between sodium tetrabromoaurate(III) and lumazine derivatives (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 565-570 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; complexes ; pteridine ; lumazine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract In aqueous hydrobromic medium, Na[AuCl4] reacts with 1,3-dimethyllumazine (1,3-dimethyl-pteridine-2,4(1H,3H)-dione, DLM) or 1,3,6,7-tetramethyllumazine (DLMD) to give three adducts with simplified formulas Na[AuBr4](DLMD), Na[AuBr4](DLM), and Na[AuBr4](DLM)2. These compounds have been characterized by means of analytical techniques, and IR and NMR spectroscopies. Single-crystal x-ray diffraction studies have been made on the Na[AuBr4](DLM)2 compound. The crystals belong to the orthorhombic Pbca space group, with a = 15.249(1), b = 15.238(2), c = 21.563(2) Å, Z = 8, and R = 0.053. The structure consists of planar [AuBr4]− anions and Na+ cations weakly linked to two crystallographically independent DLM molecules. The Na+ cation interacts weakly with four oxygen and one nitrogen atoms from four different pteridine molecules, its environment may be described as a very distorted square pyramid.
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    The synthesis and crystallographic characterization of the heterotrimetallic linear complex [Et4N][(Ph3P)2{CuS2MoS2Fe}Br2] (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 713-716 
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    ISSN: 1572-8854
    Keywords: Heterotrimetallic sulfido cluster ; linear ; synthesis ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The complex Cu(PPh3)3I reacts with [Et4N]2MoS4 and FeBr2 to give the heterotrimetallic complexes [Et4N][(Ph3P)2{CuS2MoS2Fe}Br2] (1). [Et4N][(Ph3P)2{CuS2MoS2Fe}Br2] (1) crystallizes in the triclinic space group P-1, a = 13.537(4), b = 15.316(4), c = 12.381(4) Å, α = 105.16(2), β = 93.27(3), γ = 101.18(2)°, and V = 2415.0(12) Å3 for Z = 2. The three metal atoms of the structure [Et4N][(Ph3P)2{CuS2MoS2Fe}Br2] (1) are nearly distributed along a line, where three metal atoms (Mo, Cu, Fe) are each in an approximate tetrahedral coordination, the lengths Mo-Fe and Mo-Cu distances are 2.772(2) and 2.798(2) Å, respectively.
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    Molecular structure of AlH3[N(CH2CH2)3CH]2 (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 649-651 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; aluminum ; hydride ; complex ; quinuclidine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Reaction of AlH3[N(CH2CH2)3CH] with hexamethyltrisiloxane, (OSiMe2)3, gives rise to the bis-quinuclidine complex AlH3[N(CH2CH2)3CH]2, which has been characterized by 1H and 13C NMR spectroscopy and X-ray crystallography. The molecular structure of AlH3[N(CH2CH2)3CH]2 consists of a trigonal bipyramidal aluminum with axial coordination of the quinuclidine ligands. Crystal data: orthorhombic, space group Pbcn, a = 10.6895(9), b = 12.266(1), c = 12.3794(9) Å, V = 1623.2(2) Å3, and Z = 4.
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    Synthesis and crystal structure of a new lithium cyclohexaphosphate hydrate: Li6P6O18·10H2O (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 323-327 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; cyclohexaphosphate ; hydrate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The synthesis and crystal structure of a novel hydrate of lithium cyclohexaphosphate are reported. Li6P6O18·10H2O crystallizes in the space group C2/c with a = 15.113(5), b = 12.006(2), c = 15.892(2) Å, β = 122.85(2)°, and Z = 4. The structure consists of P6O18 ring layers stacked along the c direction in between which are located the lithiumions and water molecules. Two LiO4 tetrahedra share common edges with LiO5 pseudosquare pyramids to form two independant Li3O9 units. About 50% of the water molecules have fractional occupancy rates and form fragments of molecules. A linear relationship is established between the relative cell volume V/Z and the hydration degree, n, for all the known hydrates: Li6P6O18·nH2O.
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    Synthesis and structure of a bis(ethynyl)-substituted oxahexacyclic cage ether (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 347-349 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; pentacycloundecane ; triple bonds
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Intramolecular dehydration of a cage-diol results in the title compound. This crystallizes in the monoclinic space group P21/c; a = 8.6403(8), b = 9.5698(7), c = 14.062(1) Å β = 107.47(7)° and Z = 4.
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    A cobalt(II) complex with the N,N,O-tridentate ligand 6-amino-5-formyl-1,3-dimethyluracilato-benzoyl-hydrazone (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 283-286 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; complexes ; cobalt ; benzoylhydrazone
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal structure of bis-(6-amino-5-formyl-1,3-dimethyluracilato benzoylhydrazone)cobalt(II) dimethylformamide solvate is described. This compound crystallizes in the triclinic system, space group P1¯, Z = 2 with a = 9.7368(8), b = 12.346(1), c = 17.184(1) Å, α = 78.372(6), β = 74.585(6), γ = 71.113(5)°, and V = 1869.0(3) Å3. The coordination polyhedron around the metal ion displays a slightly flattened M(NNO)2 octahedral shape. Both ligands bind in a trident fashion through the benzoylic oxygen atom, the hydrazone nitrogen atom closer to the uracil ring, and the deprotonated nitrogen atom of the amino group. The two ligands exhibit quite different conformations: one of them is almost planar, whereas the other is severely twisted.
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    Synthesis and crystal structure of 4,4′-bis(4-pyridylethyl)biphenyl, noncovalently hydrogen bonded two-dimensional networks (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 641-646 
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    ISSN: 1572-8854
    Keywords: Crystal structure ; hydrogen bonds ; 1H and 13C NMR ; FTIR
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract A new pyridine containing compound, 4,4′-bis(4-pyridylethyl)biphenyl 1, was synthesized and its structure was determined by X-ray crystallography. Two kinds of two-dimensional networks linked by hydrogen bonds were obtained with different crystal solvents: 1·2H2O, monoclinic, space group P21/n with a = 8.3280(10), b = 5.5990(10), c = 24.054(4) Å, β = 98.79(2)°, V = 1108.4(3) Å3, Z = 2, Dc = 1.200 g cm−3, R1 = 0.0558; 1·CH3OH·2H2O, triclinic, space group P-1 with a = 8.3310(10), b = 12.861(2), c = 13.111(2) Å, α = 64.110(10), β = 75.000(10), γ = 83.750(10)°, V = 1220.7(3) Å3, Z = 2, Dc = 1.177 g cm−3, R1 = 0.0529. It is interesting that in the hydrate the host molecule of 1 contains an essentially flat biphenyl section, while in the methanol complex the host molecule of 1 contains a substantial twist in the center of the biphenyl section. The compounds were also characterized by NMR and FTIR spectroscopies. The 1H and 13C NMR assignments for 1 were carried out by 2D NMR spectral measurements in acetonitrile-d 3.
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    Synthesis and Electrochemistry of Alkylidynetrihydridotriruthenium Clusters with Apical π-Substituents (2000)
    Springer
    Journal of cluster science 11 (2000), S. 373-379 
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    ISSN: 1572-8862
    Keywords: Ruthenium ; clusters ; synthesis ; electrochemistry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract The clusters, (μ-H)3Ru3(μ 3-CY)(CO)9−n (PPh3) n [Y=–CH2CHCH2, n=0 (1); Y=–CH2CHCH2, n=3 (2); Y=–C6H4CH3, n=0 (3); Y=–C6H4CH3, n=3 (4)], have been synthesized in good yields and characterized by IR and NMR spectroscopy and by elemental analysis. The electrochemical properties of these clusters is also reported. These data indicate that the π-system of the apical substituent does not interact significantly with the cluster and should be available for further chemistry.
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    Tetranuclear planar metal clusters with two capping ligands (1996)
    Springer
    Journal of cluster science 7 (1996), S. 1-36 
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    ISSN: 1572-8862
    Keywords: Clusters ; Planar ; tetranuclear ; synthesis ; capping ligands
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract Background information and current research activity dealing with tetrametal planar clusters containing two capping ligands is briefly reviewed. The synthetic methods leading to these clusters and their chemical properties are presented. The structure and bonding in lo some representative example is discussed. Their application as models of heterogeneous catalysts, homogeneous catalysts, and precursors to materials is highlighted. Such information can have important implications in the design of a more sophisticated tetranuclear cluster systems for improved process applications.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01166174
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    Synthesis and Characterization of the Isocyanide Ligated Centered Zirconium Halide Cluster [(Zr6Be)Cl12(CNXyl)6] (1997)
    Springer
    Journal of cluster science 8 (1997), S. 521-531 
    Details
    ISSN: 1572-8862
    Keywords: Zirconium clusters ; isocyanide ; synthesis ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract The first isocyanide ligated hexanuclear zirconium halide cluster is reported. The unoxidized [(Zr6Be)Cl12(CNXyl)6] (CNXyl = 2,6-dimethylphenyl isocyanide) was obtained from the solid state precursor K3Zr6Cl15Be by dissolution in CH3CN in the presence of CNXyl. The CNXyl ligands occupy all the axial positions on the cluster. The compound was recrystallized from CH2Cl2 and Et2O. [(Zr6Be)Cl12(CNXyl)6].2CH2Cl2 crystallizes in the space group $${\text{P}}\overline {\text{1}} $$ (#2) with a = 12.092(5) Å, b=12.728(5) Å, c = 14.102(8) Å, α = 104.98(4)°, β =107.11°, γ = 100.94°, V = 1919(2) Å3, Z = l, R = 11.3% and R W = 27.0%. For the bound isocyanide ligands, v CN increases to 2140 cm−1.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1022605113866
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  • 80
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    Synthesis and Characterization of Some Poly(1,2-Phenylenedithiocarbamate)–Metal Complexes (1998)
    Springer
    Journal of inorganic and organometallic polymers and materials 8 (1998), S. 167-178 
    Details
    ISSN: 1572-8870
    Keywords: Poly(1,2-phenylenedithiocarbamate) ; poly(1,2-phenylenedithiocarbamate)–metal complexes ; synthesis ; characterization ; structure ; DC electrical conductivity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Poly(1,2-phenylenedithiocarbamate) (PPDTC) was prepared by the reaction of 2-aminothiophenol with carbon disulfide followed by condensation through the removal of H2S gas. PPDTC was used as a ligand to prepare four poly(1,2-phenylenedithiocarbamate)–metal complexes of iron(II), cobalt(II), copper(II), and lead(II), by refluxing with the metal salts. The polymer and its metal complexes were investigated by elemental analyses, UV–visible and IR spectroscopy, inherent viscosity, and magnetic susceptibility. The DC electrical conductivity variation with the temperature in the range 298–498 K of PPDTC and its polymeric copper complex was measured. Both polymer and polymer metal complexes showed an increase in electrical conductivity with an increase in temperature: typical semiconductor behavior. The proposed structure of the complexes is (MLX2·mH2O) n .
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1021630204888
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  • 81
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    Organozeolite materials and their properties (1999)
    Springer
    Catalysis surveys from Japan 3 (1999), S. 119-126 
    Details
    ISSN: 1572-8803
    Keywords: organozeolite ; microporous and mesoporous material ; inorganic-organic composite ; synthesis ; phosphonate ; aluminomethylphosphonate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Attempts in developing organozeolites, namely microporous and mesoporous crystalline inorganic-organic composites with a zeolite-like three-dimensional framework and organic moieties covalently connected to the framework, are briefly reviewed. MCM-41 type mesoporous materials modified by organic functional groups have been prepared by use of organosiloxane as a part of Si sources and by post-modification of the purely inorganic materials using organosiloxane. Also, the incorporation of organic moieties into the zeolite frameworks has been tried. Recently, several novel metal organophosphonates with a three-dimensional framework, which can be regarded as organozeolites, have been prepared. Along with these new attempts, the authors' studies in preparation, structural analysis and gas adsorption properties of microporous aluminomethylphosphonates are introduced.
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    URL: http://dx.doi.org/10.1023/A:1019023702312
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  • 82
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    Synthesis of optically pure chrysobactin and immunoassay development (1996)
    Springer
    BioMetals 9 (1996), S. 377-383 
    Details
    ISSN: 1572-8773
    Keywords: chrysobactin ; Erwinia chrysanthemi ; immunoassay ; siderophore ; synthesis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Chrysobactin (α-N-(2,3-dihydroxybenzoyl)-d-lysyl-l-serine), a siderophore that is essential for systemic virulence by plant pathogenic Erwinia chrysanthemi, was synthesized with high diastereomeric purity. Chrysobactin was prepared by coupling the N-hydroxysuccinimide ester of α-N-(2,3-dibenzyloxybenzoyl)-ε-N-Cbz-d-lysine with l-serine benzyl ester followed by deprotection via hydrogenolysis. Optically pure chrysobactin was obtained with 98% overall yield. A monoclonal antibody to ferric chrysobactin was developed and characterized as IgM. The antibody reacts with chrysobactin, ferric chrysobactin and less strongly with ferric dihydroxybenzoic acid. The antibody reacts weakly with the siderophores ferrichrome, A, ferric pseudobactin and ferric rhodotorulic acid. This antibody was used in a competitive immunoassay to detect ferric chrysobactin at 10−8 to 10−10 mol. This immunoassay may provide a useful method for the detection of chrysobactin in plant samples.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00140607
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  • 83
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    X-ray crystal structures of [HB(3,4,5-Me3pz)3[2Zn, [H2B(3,4,5-Me3pz)2]Zn(μ-3,4,5-Me3pz)2Zn[H2B(3,4,5-Me3pz)2], and [H2B(pz)2]2Zn (pz = pyrazolyl ring) (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 665-670 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; poly(pyrazolyl)borate ligands ; zinc(II)
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract [HB(3,4,5-Me3pz)3]2Zn (1) and [H2B(3,4,5-Me3pz)2]Zn(μ-3,4,5-Me3pz)2Zn[H2B(3,4,5-Me3pz)2] (2) are present in equal amounts in a crystal in the triclinic space group, P-1 with a = 11.5924(11) Å, b = 12.7799(12) Å, c = 15.7317(14) Å α = 107.905(2)° β = 96.796(2)°, γ = 105.786(2)°, and Z = 1. The structure of 1 is a trigonally distorted octahedron and is very similar to the structure of [HB(3,5-Me2pz)3]2Zn showing that the introduction of the third methyl group on the pyrazolyl ring does not impact on structure. [H2B(pz)2]2Zn (3) is orthorhombic, Pca2(1) with a = 10.1473(3) Å, b = 11.1117(2) Å, c = 14.1831(5) Å, α = β = γ = 90° and Z = 4. The zinc(II) centers in both 2 and 3 are similar and have pseudotetrahedral structures.
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  • 84
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    Structure and properties of cobalt(II) complex with a tetraaza macrocycle containing 2-pyridylmethyl pendant arms (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 335-338 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; cobalt(II) complex ; tetraaza macrocycle ; 2-pyridylmethyl pendant arms
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The complex [Co(L)]Cl2·10H2O (1) (L = 2,13,-bis(2-pyridylmethyl)-3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,01.18,07.12]docosane) has been synthesized and structurally characterized. Compound 1 crystallizes in the triclinic system, space group P-1 with a = 9.731(2) Å, b = 9.789(2) Å, c = 11.998(1) Å, α = 66.66(1)°, β = 76.95(1)°, γ = 87.99(2)°, V = 1020.4(3) Å3, and Z = 1. The crystal structure of 1 shows that the complex is centrosymmetric and the cobalt(II) ion has a slightly distorted octahedral geometry with four nitrogen atoms of the macrocycle and two nitrogen atoms of the pendent arms at the axial positions. Cyclic voltammetry for 1 undergoes reversible one-electron oxidation to the Co(III) and irreversible one-electron reduction to the Co(I).
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    URL: http://dx.doi.org/10.1023/A:1009513308611
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    Polynuclear copper (II) complexes with aminoalcohol ligands (1995)
    Springer
    Journal of cluster science 6 (1995), S. 463-484 
    Details
    ISSN: 1572-8862
    Keywords: Copper (II) complex ; aminoalcohol ; structure ; synthesis ; magnetism
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract Copper complexes with aminoalcoholato ligands have attracted much attention recently because of their potential applications in ceramic materials. This review deals with polynuclear copper (II) complexes containing bidentate and triden-tate aminoalcoholato ligands. The focus of this article is on the synthesis, structure, and magnetic properties of polynuclear copper (II) complexes obtained recently by our group. Some relevant work reported previously by other researchers is also included.
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    URL: http://dx.doi.org/10.1007/BF01165768
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  • 86
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    Crystal structure of 2,3-dihydronaphto[2,3-b) [1,5] dioxepin (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 459-462 
    Details
    ISSN: 1572-8854
    Keywords: Crystal structure ; chemical synthesis ; 2,3-dihydronaphto[2,3-b] [1,5) dioxepin
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The X-ray single crystal structure of C13H12O2 compound was determined. It crystallizes in the orthorombic space group P212121 with a = 7.8847(7), b = 9.639(1), c = 13.432(2) Å, Z = 4 and V = 1020.8(3) Å3. The final R converged to 0.037 for 1763 independent reflexions. The title compound forms layers parallel to (1 0 0) planes and the three dimensional cohesion of the crystal is assumed by Van der Waals interactions. The molecule consists of two six-membered rings (A and B) and a seven-membered ring (C). A and B rings are planar, whereas the C ring has a chair conformation
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    URL: http://dx.doi.org/10.1023/A:1011399416154
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  • 87
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    Regular σ–π Organosilane Copolymers with Alternating Oligomeric Dimethylsilylene and Cis or Trans Stilbene Units (1997)
    Springer
    Journal of inorganic and organometallic polymers and materials 7 (1997), S. 1-18 
    Details
    ISSN: 1572-8870
    Keywords: Alternating copolymers ; cis and trans stilbenes and oligomeric dimethylsilylenes ; synthesis ; spectral properties ; photoisomerization and degradation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A series of perfectly alternating copolymers containing oligomeric dimethylsilylene and cis or trans stilbene units has been prepared by the condensation polymerization of silyl ditriflates with the corresponding stilbene dianion. As expected, the spectral characteristics and the polymer processability were very different for the isomeric polymers. Evidence of σ–π interaction was obtained from absorption measurements and the excited state of the Si4 catenates was characteristic of a polar charge transfer state. The polymers are all photoactive and irradiation in the long-wavelength absorption band leads to cis–trans isomerization followed by complete disappearance of the long-wavelength (λ〉300 nm) absorption. The latter was not observed for the monomeric model compounds.
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    URL: http://dx.doi.org/10.1023/A:1021609600345
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  • 88
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    Synthesis and Structure of Octamethylcyclo-di(meta-silphenylenesiloxane) (1999)
    Springer
    Journal of inorganic and organometallic polymers and materials 9 (1999), S. 63-77 
    Details
    ISSN: 1572-8870
    Keywords: Octamethylcyclo-di(meta-silphenylenesiloxane) ; poly(silphenylene-siloxane) ; synthesis ; X-ray structure ; 4-dimethylaminopyridine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Octamethylcyclo-di(meta-silphenylenesiloxane) 1 (cyclic meta-dimer) was synthesized from 1,3-bis(dimethylhydroxysilyl)benzene 7 in a dilute THF solution, in the presence of a catalytic amount of 4-dimethylaminopyridine (DMAP). In contrast, only small amounts of the cyclic meta-dimer 1, cyclic meta-trimer 2, cyclic meta-tetramer, etc. were obtained when the condensation reaction was carried out with the catalyst n-hexylamine 2-ethylhexoate or sodium hydroxide. The major product in these reactions is polymer 8. The structure of compound 1 was confirmed by X-ray crystallography. This cyclic molecule is most likely unstrained since the X-ray structure reveals that the Si–O–Si bond angle is 142.1(1)° which is similar to that in most unstrained siloxane compounds.
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    URL: http://dx.doi.org/10.1023/A:1021483115907
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    Preparation and catalytic properties of new mesoporous materials (1997)
    Springer
    Topics in catalysis 4 (1997), S. 249-260 
    Details
    ISSN: 1572-9028
    Keywords: mesoporous materials ; synthesis ; pore size ; activity ; selectivity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The development of ordered mesoporous solids is revised. Acid, base, and redox catalytic properties are presented together with their application for a series of organic reactions of fundamental and practical interest. Finally it is explained that it is possible to make use of the high surface and regular porosity of MCM–41 to prepare supported metals, and bifunctional catalysts. The above properties together with the presence of a large number of surface silanol groups allow the grafting of catalytically active transition metal complexes.
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    URL: http://dx.doi.org/10.1023/A:1019108810337
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  • 90
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    Shock waves propagation in the turbulent interplanetary plasma (1996)
    Springer
    Astrophysics and space science 243 (1996), S. 23-28 
    Details
    ISSN: 1572-946X
    Keywords: Interplanetary Plasma ; Shock Waves ; Turbulence
    Source: Springer Online Journal Archives 1860-2000
    Topics: Physics
    Notes: Abstract Effect of turbulence on interplanetary shock waves propagation is considered. It is shown that background turbulence results in the additional shock wave deceleration which may be comparable with the deceleration due to plasma sweeping. The turbulent deceleration is connected with the energy losses due to the strong turbulence amplification behind the moving shock front.
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    URL: http://dx.doi.org/10.1007/BF00644028
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  • 91
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    The crystal structure of PbFe[AsO4][AsO3(OH)] (1996)
    Springer
    Monatshefte für Chemie 127 (1996), S. 127-133 
    Details
    ISSN: 1434-4475
    Keywords: PbFe[AsO4][AsO3(OH)] ; Synthesis,hydrothermal ; Crystal structure ; Crystal chemistry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Hellgrüne bis nahezu farblose Kristalle von PbFe[AsO4][AsO3(OH)] wurden unter niedrig-hydrothermalen Bedingungen synthetisiert (a=4.846(2),b=8.482(4),c=15.560(6) Å, β=92.82(3)°, Raumgruppe P21/n, Z=4). Für die Einkristall-Strukturbestimmung wurden 110 freie Parameter aufR=0.042,R w=0.031 verfeinert (1545 Röntgenbeugungsreflexe mitF 0 〉3σ(F 0) und sinϑ/λ⩽70°). Die Kristallstruktur wird durch eine dreidimensionale Ecken-Verknüpfung der FeO6-Oktaeder mit den Arsenattetraedern und den protonierten Arsenatgruppen charakterisiert. Jeweils zwei PbO7-Polyeder sind über eine Kante zu Pb2O12-Dimeren verknüpft, die in Zwischenräumen angeordnet sind.
    Notes: Summary Light green to nearly colourless crystals of PbFe[AsO4][AsO3(OH)] were synthesized under moderate hydrothermal conditions (a=4.846(2),b=8.482(4),c=15.560(6) Å, β=92.82(3)°, space group P21/n, Z=4). For a single-crystal structure determination, 110 variable parameters were refined toR=0.042,R w=0.031 (1545 X-ray reflections withF 0 〉3σ(F 0) and sinϑ/λ⩽70°). The crystal structure is characterized by a three-dimensional corner-connection of the FeO6 octahedra with the arsenate tetrahedra and the protonated arsenate groups. Each two PbO7 polyhedra are edge-connected to Pb2O12 dimers which are located within interstitial holes.
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    Crystal structure of Ag2TeS3 and Na(Na1−x Ag x )TeS3 (x≈0.5) and the geometry of Te(IV)S3 polyhedra (1997)
    Springer
    Monatshefte für Chemie 128 (1997), S. 157-163 
    Details
    ISSN: 1434-4475
    Keywords: Ag2TeS3 ; Na(Na1−x Ag x )TeS3 (x≈0.5) ; Hydrothermal syntheses ; Crystal structure ; Crystal chemistry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Es wird über die mittels Röntgenbeugungsexperimenten an Einkristallen bei 300 K bestimmten Strukturen von Ag2TeS3 (monoklin Cc-C s 4 ;a=6.783(1),b=11.567(2),c=7.693(1) Å; β=114.44(1)°;Z=4;R=0.044) und Na(Na1−x Ag x )TeS3 (x≈0.5; monoklin, P21/c-C 2h 5 ;a=5.761(9),b=12.171(8),c=8.342(4)Å; β=92.26(6)°;Z=4;R=0.030) berichtet. In beiden Verbindungen ist die Atomanordnung durch isolierte trigonal-pyramidale TeS3-Polyeder, unregelmäßig koordinierte Ag- und Na-Atome, AgS4- und (Na, Ag)S4-Polyeder bildend, sowie leicht verzerrte NaS6-Oktaeder charakterisiert. Kristalle der beiden Verbindungen wurden unter moderaten Hydrothermalbedingungen aus einem equimolaren Gemenge der Elemente und konzentrierter wäßriger Ammoniaklösung bzw. 5N NaOH-Lösung gezüchtet.
    Notes: Summary Structural data determined by single crystal X-ray experiments (T=300 K) are reported for Ag2TeS3 (monoclinic, Cc-C s 4 ;a=6.783(1),b=11.567(2),c=7.693(1) Å; β=114.44(1)°;Z=4;R=0.044) and for Na(Na1−x Ag x )TeS3 x≈0.5; monoclinic, P21/c-C 2h 5 ;a=5.761(9),b=12.171(8),c=8.342(4) Å; β=92.26(6)°;Z=4;R=0.030). In both compounds the atomic arrangements are characterized by isolated trigonal pyramidal TeS3 polyhedra, irregularly coordinated Ag and Na atoms forming AgS4 and (Na, Ag)S4 polyhedra, and slightly distorted NaS6 octahedra. Crystals of both compounds were synthesized under moderate hydrothermal conditions from an equimolar mixture of the elements in concentrated aqueous ammonia and 5N NaOH solution, respectively.
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    Enantiomere und diastereomere 2-Methoxymethyl-pyrrolidin-1-dithiocarbonsäureester (1997)
    Springer
    Monatshefte für Chemie 128 (1997), S. 881-891 
    Details
    ISSN: 1434-4475
    Keywords: 2-Methoxymethylpyrrolidine ; Carbon disulfide ; Pyrrolidine-1-dithiocarboxylates ; Crystal structure ; Diastereomers ; HPLC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Formation of the 2-methoxymethyl-pyrrolidine-1-dithiocarboxylates2–4 and alkylation of2 and3 were studied. Enantiomeric and diastereomeric derivatives of4, the preparation of diastereomeric mixtures of4 by alkylation of3 in the presence of strong bases, and formation of6 by phase transfer alkylation of2 are described. The two enantiomers of 2-(4-bromophenyl)-2-oxo-ethyl 2-methoxymethylpyrrolidine-1-dithiocarboxylate2 have been characterized by X-ray analysis.
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    URL: http://dx.doi.org/10.1007/BF00807097
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    Einkristallstrukturanalyse vonBis(trimethylsilyl)peroxid (1996)
    Springer
    Monatshefte für Chemie 127 (1996), S. 1221-1227 
    Details
    ISSN: 1434-4475
    Keywords: Crystal structure ; Silylperoxide ; Crystal growth
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary Bis(trimethylsilyl)peroxide has been prepared from trimethylchlorsilane, hydrogen peroxide, and 1,4-diazobicyclo[2.2.2]octane. Crystal growth was achievedin situ on a diffractometer and characterized by crystal structure analysis (T=193(2) K, 2522 reflections, P21/c;a=606.7(1) pm,b=1098.5(1) pm,c=858.2(1) pm, β=101.88(2)°,Z=2,R=0.045). The molecule's conformation in the crystalline solid is determined by C-H...O-bridges.
    Notes: Zusammenfassung Bis(trimethylsilyl)peroxid wurde aus Trimethylchlorsilan, Wasserstoffperoxid und 1,4-Diazobicyclo[2.2.2]octan dargestellt. Ein Einkristall wurdein situ auf einem Vierkreisdiffraktometer gezüchtet und mittels Einkristallstrukturanalyse charakterisiert (T=193(2) K, 2522 Reflexe, P21/c;a=606.7(1) pm,b=1098.5(1) pm,c=858.2(1) pm, β=101.88(2)°,Z=2,R=0.045). Die Konformation des Moleküls im Kristall ist durch C-H...O-Brücken bestimmt.
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    URL: http://dx.doi.org/10.1007/BF00807788
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    Tetrakis(2-fluorophenylamino)silan und sein erstes Kondensationsprodukt N-(2-fluorophenyl)-Si, Si, Si, Si′, Si′, Si′-hexakis(2-fluorophenylamino)-disilazan. Synthesen und Kristallstrukturen (1996)
    Springer
    Monatshefte für Chemie 127 (1996), S. 117-126 
    Details
    ISSN: 1434-4475
    Keywords: Condensation ; Crystal structure ; Disilazane ; Silanetetramine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary The synthesis and crystal structure determination of silanetetramine N,N′,N″,N‴2-fluorophenyl(C2/c;a=16.771(7) Å,b=16.827(5) Å,c=16.753(6) Å, ß=111.00(2)°, z=8) are reported. In a search for suitable condensation pathways to silicon/nitrogen based porous solids, N-(2-fluorophenyl)-Si,Si,Si,Si′,Si′,Si′-hexakis(2-fluorophenylamino)disilazane (2) has been obtained from the ammonium carbamate catalyzed condensation of the silanetetramine in teflon lined autoclaves. The X-ray crystal structure determination ( $$P\bar 1$$ ;a=9.331(1) Å,b=13.698(5) Å,c=16.164(4) Å, α=90.34(2)°, ß=103.03(2)°, γ=103.04(3)°, Z=2) shows the disilazane to be a dimer formed by linear condensation from the monomeric silazane.
    Notes: Zusammenfassung Tetrakis(2-fluorophenylamino)silan (1) wurde als Precursor zur Darstellung poröser, nitridischer Festkörper synthetisiert und mit Hilfe der Einkristallröntgenstrukturanalyse charakterisiert (C2/c;a=16.771(7) Å,b=16.827(5) Å,c=16.753(6) Å, ß=111.00(2)°,z=8). Beim Erhitzen mit Ammoniumcarbamat als Katalysator wurde N-(2-fluorophenyl)-Si, Si, Si, Si′, Si′, Si′, -hexakis(2-fluorophenylamino)disilazan (2) als erstes Kondensationsprodukt isoliert ( $$P\bar 1$$ ;a=9.331(1) Å,b=13.698(5) Å,c=16.164(4) Å, α=90.34(2)°, ß=103.03(2)′, γ=103.04(3)°, Z=2).
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00807392
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  • 96
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    Untersuchungen des Hydroxylammonium-Fluorogallats (1996)
    Springer
    Monatshefte für Chemie 127 (1996), S. 581-586 
    Details
    ISSN: 1434-4475
    Keywords: (NH3OH)3GaF6 ; Hydroxylammonium compounds ; Fluorogallates ; Crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Crystals of (NH3OH)3GaF6 have been isolated from aqueous solution. The compound crystallizes triclinic, with cell parametersa=6.539(5) Å,b=6.924(5) Å,c=9.403(1) Å, α=87.01(9)°, β=83.98(8)°, γ=70.28(8)°. The thermal decomposition was studied by TG and DSC analysis.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00817249
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  • 97
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    Reaction of titanocene dihalides with Na2H2 EDTA. Crystal structure of [Ti(EDTA)(H2O)] (1997)
    Springer
    Monatshefte für Chemie 128 (1997), S. 1201-1206 
    Details
    ISSN: 1434-4475
    Keywords: Titanium ; EDTA ; Crystal structure ; Sevenfold coordination
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Titanocenkomplexe ([Ti(η5-C5H4 R)2 X 2];R=H, SiMe3;X=Cl, Br) reagieren in wäßrigem Methanol mit Na2H2 EDTA unter Verdrängung der Halogen- und Cyclopentadienylliganden zum selben Produkt ([Ti(EDTA)(H2O)]). Die Struktur von ([Ti(EDTA)(H2O)]) wurde röntgenographisch bestimmt. Kristalldaten: monoklin,a=13.923(6),b=7.048(3),c=13.252(5) Å, β=90.81(1)°, RaumgruppeP21/c,Z=4. In diesem Komplex ist das Titanatom mit einem sechszähnigenEDTA-Liganden und einem Wassermolekül, das eine zusätzliche Koordinationsstelle besetzt, siebenfach koordiniert.
    Notes: Summary Titanocene complexes ([Ti(η5-C5H4 R)2 X 2];R = H, SiMe3;X=Cl, Br) react with Na2H2 EDTA in aqueous methanol to give an identical product ([Ti(EDTA)(H2O)] by cleavage of the halogen and cyclopentadienyl ligands. The structure of [Ti(EDTA)(H2O)] has been determined by X-ray diffraction; crystal data: monoclinica=13.923(6),b=7.048(3),c=13.252(5) Å, β=90.81(1)°, space groupP21/c,Z=4. In this complex, Ti has a sevenfold coordination with a hexadentateEDTA 4− ligand and a water molecule occupying an additional coordination site.
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    URL: http://dx.doi.org/10.1007/BF00807251
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  • 98
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    Untersuchungen der Hydroxylammonium-Fluorozirconate(IV) (1995)
    Springer
    Monatshefte für Chemie 126 (1995), S. 1279-1289 
    Details
    ISSN: 1434-4475
    Keywords: (NH3OH)2ZrF6 ; (NH3OH)3ZrF7 ; Hydroxylammonium compounds ; Fluorozirconates ; Crystal structure ; IR spectroscopy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Hydroxylammonium fluorozirconates have been investigated. Two new microcristalline phases have been isolated from aqueous solutions: (NH3OH)2ZrF6 (1) and (NH3OH)3ZrF7 (2). The crystals were prepared by slow evaporation of the solution of NH2OH, Zr, and HF. Different compositions of the crystals were achieved by varying the molar ratios of the components. They were characterized by thermal analysis, vibrational spectroscopy, and structure (single crystal x-ray methods). (NH3OH)2ZrF6 (1) crystallizes triclinic, P $$\overline 1 $$ (No.: 2),a=7.400(2),b=7.609(2),c=7.887(2) Å, α=57.29(3)°, β=62.16(3)°, γ=67.83(2)°. (NH3OH)3ZrF7 (2) crystallizes triclinic, P $$\overline 1 $$ (No.: 2),a=7.128(1),b=7.989(1),c=8.888(1) Å, α=109.72(1)°, β=91.01(1)°, γ=104.27(1)°.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00807057
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  • 99
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    The crystal structures ofbis-{(2-benzotrifluoride)-[(2-oxo-3H-naphth-3-ylidene)-methyl]-aminato} Copper(II) andbis-{(3-benzotrifluoride)-[(2-oxo-3H-naphth-3-ylidene)-methyl]-aminato} Copper(II) (1995)
    Springer
    Monatshefte für Chemie 126 (1995), S. 129-136 
    Details
    ISSN: 1434-4475
    Keywords: Hydroxy-naphthaleńicSchiff bases ; Schiff base Copper(II) complexes ; Crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung DieSchiffschen Basen 3-[(2-Benzotrifluorid)-2-hydroxy-3H-naphth-3-yliden)-methyl]-aldamin (1) und 3-[(3-Benzotrifluorid)-2-hydroxy-3H-naphth-3-yliden)-methyl]-aldamin (2) sowie ihre entsprechenden Cu(II)-Komplexe (I,II) wurden synthetisiert und ihre Struktur im Kristall bestimmt. VerbindungI kristallisiert triklin (a=15.561(3),b=16.211(4),c=8.007(2) Å, α=96.29(2), β=101.42(2), γ=97.10(2)°, Raumgruppe $$P_{\bar 1}$$ ,Z=2); VerbindungII kristallisiert monoklin (a=5.064(2),b=19.172(4),c=15.111(3) Å, β=95.05(2)°, Raumgruppe P21/c,Z=2). Aus der Röntgenstrukturanalyse ergibt sich eine quadratisch planare Geometrie der Komplexe.
    Notes: Summary TheSchiff base ligands 3-[(2-benzotrifluoride)-2-hydroxy-3H-naphth-3-ylidene)-methyl] aldamine (1) and 3-[(3-benzotrifluoride)-2-hydroxy-3H-naphth-3-ylidene)-methyl] aldamine (2) and their corresponding Cu(II) complexes (I, II) were synthesized. The crystal structures ofbis-{(2-benzotrifluoride)-[(2-oxo-3H-naphth-3-ylidene)]-methyl]-aminato} Copper(II) (I) andbis-{(3-benzotrifluoride)-[(2-oxo-3H-naphth-3-ylidene)-methyl]-aminato} Copper(II) (II) were determined. CompoundI crystallizes in the triclinic crystal system (a=12.561(3),b=16.211(4),c=8.007(2) Å, α=96.29(2), β=101.42(2), γ=97.10(2)°, space group $$P_{\bar 1}$$ ,Z=2); compoundII crystallizes in the monoclinic crystal system (a=5.064(2),b=19.172(4),c=15.111(3) Å, β=95.05(2)°, space group P21/c,Z=2). The X-ray diffraction study shows that the geometry around the metal atom is square planar for both copper complexes.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00812241
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  • 100
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    Three-Dimensional Analysis of CD6 Site-Directed Mutagenesis and Monoclonal Antibody Binding Studies Using the X-ray Structure of Mac-2 Binding Protein and a Molecular Model of the CD6 Ligand Binding Domain (1999)
    Springer
    Journal of molecular modeling 5 (1999), S. 263-270 
    Details
    ISSN: 0948-5023
    Keywords: Binding site ; Critical residues ; Crystal structure ; Model building ; Monoclonal antibodies ; Mutagenesis ; Receptor-ligand interactions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The extracellular region of CD6 consists of three scavenger receptor cysteine-rich (SRCR) domains and binds activated leukocyte cell adhesion molecule (ALCAM), a member of the immunoglobulin superfamily (IgSF). Residues important for the CD6-ALCAM interaction have previously been identified by mutagenesis. A total of 22 CD6 residues were classified according to their importance for anti-CD6 monoclonal antibody (mAb) and/or ALCAM binding. The three-dimensional structure of the SRCR domain of Mac-2 binding protein has recently been determined, providing a structural prototype for the SRCR protein superfamily. This has made a thorough three-dimensional analysis of CD6 mutagenesis and mAb binding experiments possible. Mutation of buried residues compromised both mAb and ALCAM binding, consistent with the presence of structural perturbations. However, several residues whose mutation affected both mAb and ALCAM binding or, alternatively, only ligand binding were found to map to the surface in the same region of the domain. This suggests that the CD6 ligand binding site and epitopes of tested mAbs overlap and provides an explanation for the finding that these mAbs effectively block ALCAM binding. An approximate molecular model of CD6 was used to delineate the ALCAM binding site.
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    URL: http://dx.doi.org/10.1007/s0089490050263
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