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  • Electronic Resource  (195)
  • 2000-2004  (60)
  • 1990-1994  (135)
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  • 2000  (60)
  • 1993  (135)
  • crystal structure
  • 1
    Electronic Resource
    Electronic Resource
    Synthesis and structure of tetrakis(2,6-dichlorophenoxide) bis(THF) uranium(IV) (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 7-10 
    Details
    ISSN: 1572-8854
    Keywords: crystal structure ; uranium (IV) ; dichlorophenoxide
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The reaction of UCl4 with KO-2,6-Cl2C6H3 in tetrahydrofuran results in the preparation of the title compound. The six-coordinate complex possesses pseudo-octahedral geometry about uranium, with U-O(phenoxide) bond lengths in the range 2.161(11) to 2.178(10) Å and U-O(THF) bond lengths of 2.467(10) and 2.475(11) Å. This complex crystallizes in the monoclinic space group P21/n (a = 11.169(2), b = 11.588(2), c = 35.119(5) Å, β = 92.11(1)°, V = 4542.2(13) Å3, and Z = 4).
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1009594612946
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  • 2
    Electronic Resource
    Electronic Resource
    Synthesis and crystal structure of hexakis(N-methylimidazole) iron(II) pyridine-2-sulfonate (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 23-26 
    Details
    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.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1009537830693
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  • 3
    Electronic Resource
    Electronic Resource
    Crystal structure of [Cu2(II)(dmpa)2(p-Cl-C6H5COO)2] (Hdmpa = N,N-dimethyl-3-amino-1-propanol) (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 35-38 
    Details
    ISSN: 1572-8854
    Keywords: copper(II) ; aminoalcoholato ; hydrogen bonding ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The copper complex, [Cu2(II)(dmpa)2(p-Cl-C6H5COO)2], has been prepared and its structure determined using X-ray crystallography. The dimer is a di-μ2-alkoxo complex which is a five-coordinate copper dimer with unsupported alkoxo bridges. The complex crystallizes in the triclinic space group P-1 with a = 11.384(2), b = 14.636(5), c = 9.609(2) Å, α = 100.07(2), β = 104.33(3), γ = 72.79(2)°, V = 1471.8(7) Å3, and Z = 2. The structure is comprised of discrete binuclear clusters in which the metal atoms are bridged by two alkoxo oxygens of the dmpa− ligands. The Cu-O and Cu-N distances are in good agreement with those found for other copper(II) aminoalcoholato complexes. The Cu···Cu distance is 2.9765(6) Å. In the crystal, every two dimeric coordination molecules are combined together by the recognition through intermolecular hydrogen-bonding interactions between the apical water molecule and the non-coordinated O atom from the p-chlorobenzoato ligand, forminga tetramer.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1009542031602
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  • 4
    Electronic Resource
    Electronic Resource
    Synthesis and crystal structure of manganese(III) hydroxyl-containing Schiff base complexes: [Mn(III)(Hvanpa)2]N3 (H2vanpa = 1−(3-hydroxysalicylaldeneamino)-3-hydroxypropane) (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 39-42 
    Details
    ISSN: 1572-8854
    Keywords: manganese(III) ; Schiff base ; hydrogen bonding ; crystal structure ; Jahn-Teller distortion
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The manganese complex, [Mn(III)(Hvanpa)2]N3 has been prepared and the crystal structure determined using x-ray crystallography. The mononuclear complex has a six-coordinate octahedral geometry. The complex crystallizes in the monoclinic space group P21/c with a = 9.867(1), b = 13.316(2), c = 9.0110(1) Å, β = 107.870(1)°, V = 1126.8(2) Å3, and Z = 2. The Mn-O and Mn-N distances in the equatorial plane are in good agreement with those found for other manganese(III) Schiff base complexes. In the axial direction, the Mn-O distances of 2.274(2) Å is about 0.3 Å longer than those in the equatorial plane due to a Jahn-Teller distortion at the d4 manganese(III) center. In the crystal, each azido ion is linked through hydrogen bonding with two hydrogen atoms from the coordinate hydroxyl groups at the apical site.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1009594015672
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  • 5
    Electronic Resource
    Electronic Resource
    Preparation, characterization and crystal structure of an intermolecular compound based on H3PMo12O40·nH2O and diethylamine (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 43-48 
    Details
    ISSN: 1572-8854
    Keywords: molybodophosphoric acid ; crystal structure ; diethylamine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract An intermolecular compound, H3PMo12O40·5(CH3CH2)2NH·H2O, between the heteropolymolybdate α-H3PMo12O40 and the organic substrate diethylamine, has been synthesized and characterized. Light yellow crystals of the title compound were crystallized from a mixed solvent of water and acetonitrile with formula H3PMo12O40·5(CH3CH2)2NH·H2O. Spectroscopic data support the presence of a sizable electronic interaction between the organic substrate and the inorganic anion in the solid state. The single crystal x-ray structure analysis of the title compound revealed that it crystallized in the triclinic system, space group P $$\overline 1$$ with a = 12.0786(13), b = 12.102(5), c = 21.416(3) Å, α = 94.87(2), β = 94.755(9), γ = 113.81(2)°, V = 2830.3(13) Å3, and Z = 2.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1009546132511
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  • 6
    Electronic Resource
    Electronic Resource
    Synthesis and crystal structure of K3Sb4BO13 (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 53-53 
    Details
    ISSN: 1572-8854
    Keywords: boroantimonate ; borate ; antimonate ; crystal structure ; 49
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract K3Sb4BO13, Mr = 823.11 g.mol−1, crystallizes in the triclinic system, space group P $$\overline 1$$ , Z = 2. The lattice parameters are a = 7.133(1) Å, b = 7.232(1) Å, c = 13.259(2) Å, α = 82.00 (1)°, β = 99.77(1)° and γ = 117.08(1)°, V = 598.7(2) Å3, Dx = 4.566 Mg m−3. The final R index and weighted Rw index are 0.0251 and 0.0623, respectively. The three-dimensional network of the title compound is constituted by layers (Sb3O9)n, similar to that of hexagonal bronze of Magneli. These layers are linked together, in the c direction, alternatively by edge-sharing pairs of SbO6 octahedra and BO3 triangles. This framework has interconnected tunnels, running approximately along the a and b directions, in which the K+ ions are located.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1009598116581
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  • 7
    Electronic Resource
    Electronic Resource
    Crystal structure of a (25R)-2α,3α-epoxy-5α-spirostan-6, 23-dione hemi-ethyl acetate solvate (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 693-697 
    Details
    ISSN: 1572-8854
    Keywords: brassinosteroids ; steroids ; natural products ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The compound (25R)-2α,3α-epoxy-5α-spirostan-6,23-dione, crystallizes as a hemi-ethyl acetate solvate, having two host molecules of similar conformation per molecule of ethyl acetate, in the asymmetric unit. The O atom of the epoxy group is α-oriented. The presence of the epoxy group disturbs the chair conformation in the ring A of the steroidal nucleus. Ring A has a C5α,C10β half-chair conformation. The six-membered rings B, C, and F have chair conformation as expected. The D ring adopts a C14α-envelope conformation and the E ring is midway between a C22α,O3β half-chair and a C22α-envelope conformations. The A/B, B/C, and C/D ring junctions are trans. Crystal data: C27H38O5·1/2C4H8O2, Monoclinic, space group P21, a = 7.7363(18) b = 28.769(12) c = 12.038(6) Å, β = 90.88(5), V = 2679.0(10) Å3, Z = 4. The packing of the molecules is assumed to be dictated by van der Waals interactions and by intermolecular C—H ··· O hydrogen bonds.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1012277425969
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  • 8
    Electronic Resource
    Electronic Resource
    X-ray crystal structure of trans-bis(monoethanolamine) bis(saccharinato)nickel(II) (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 767-771 
    Details
    ISSN: 1572-8854
    Keywords: saccharin ; monoethanolamine ; nickel(II) complex ; hydrogen bonding ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal structure of trans-bis(monoethanolamine)bis(saccharinato)nickel(II), [Ni(C7H4NO3S)2(C2H7NO)2], has been determined from X-ray diffraction data. The metal complex is monoclinic, with a = 11.0555(5), b = 8.9103(4), c = 11.3890(5) Å, β = 105.0230(10)°, Z = 2, and space group P21/c . The structure consists of individual molecules. Two monoethanolamine molecules and two saccharinate anions coordinate the nickel atom forming a distorted octahedron. The monoethanolamine molecules act as a bidentate ligand and form five-membered trans chelate rings, which constitute the plane of the coordination octahedron, while two saccharinate ions behave as a monodentate ligand occupying the axial positions. Intermolecular hydrogen bonds link the molecules to form a three-dimensional infinite structure.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1013292406687
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  • 9
    Electronic Resource
    Electronic Resource
    Novel Cu–Te Clusters Synthesised from tBuTeSiMe3: [Cu18Te6(TetBu)6(PPh2Et)7], [Cu19Te6(TetBu)7(PEt3)8], [Cu27Te15(PiPr2Me)12] and [Cu58Te32(PtBu2nBu)14] (2000)
    Springer
    Journal of cluster science 11 (2000), S. 135-151 
    Details
    ISSN: 1572-8862
    Keywords: copper telluride clusters ; copper telluro-tellurolato clusters ; crystal structure ; influence of phosphine ligands ; Frank-Kasper polyhedron
    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 reactions of CuCl and tBuTeSiMe3 in the presence of phosphine ligands result in the formation of four new Cu/Te cluster complexes, [Cu18Te6(TetBu)6(PPh2Et)7], [Cu19Te6(TetBu)7(PEt3)8], [Cu27Te15(PiPr2Me)12] and [Cu58Te32(PtBu2 nBu)14], which have been structurally characterized by single crystal structural analysis. The former two clusters show a layer-type tellurium frameworks in which the copper atoms are asymmetrically spread. The latter two clusters possess a tellurium framework in a body-centered Te14-Frank-Kasper polyhedron or a Te28 polyhedron with four interstitial tellurium atoms and belong to mixed-valence Cu/Te compounds.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1009016832159
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  • 10
    Electronic Resource
    Electronic Resource
    Cluster Build-up Reactions using Di-gold Cationic Fragments: Synthesis and Structural Characterization of [Os7(CO)19(Au2dppm)] (2000)
    Springer
    Journal of cluster science 11 (2000), S. 217-226 
    Details
    ISSN: 1572-8862
    Keywords: gold ; osmium ; cluster ; carbonyl ; phosphine ; heteronuclear ; 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 reaction of the di-gold cation [Au2(dppx)]2+ with the heptanuclear cluster dianion [Os7(CO)20]2− affords the mixed metal cluster [Os7(CO)20{Au2(dppx)}] (x=m (1), e (2), b (3)). On standing, in solution, this complex undergoes decarbonylation to give the cluster [Os7(CO)19{Au2(dppx)}] (x=m (4), e (5), b (6)). The complexes have been characterised spectroscopically, and an X-ray structure determination of the dppm derivative shows that it contains a metal core based on an Os7 edge-bridged bicapped tetrahedron with the two μ 3-Au atoms capping adjacent triangular Os3 faces of the central tetrahedron. In an analogous reaction, the carbido anion [Os7(H)C(CO)19]− affords the neutral cluster [Os7C(CO)19{Au2(dppm)}] (7) when treated with [Au2(dppm)]2+ in the presence of base.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1009025101208
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  • 11
    Electronic Resource
    Electronic Resource
    Crystal structure of 2,2,3-trimethyl-3-(2′,4′,5′-tricyanophenyl) cyclopentyl-1-acetic acid, methyl ester, C20H21N3O2 (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 589-592 
    Details
    ISSN: 1572-8854
    Keywords: Phenylcyclopentaneacetate derivative ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound crystallizes in space group P21/n, with a = 14.600(2), b = 7.091(2), c = 18.211(5) Å, and β = 103.67(2)°. Owing to the centric space group, both C(1) and C(3) chiral centers are either R or S. The acetate group is equatorial, the H(1) and the methyl group at C(3) are axial and reciprocally trans.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1011358327087
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  • 12
    Electronic Resource
    Electronic Resource
    The crystal and molecular structure of spiro[1-(S)-Br-3-(S)-H-4-(R)-l-(1′ R,2′ S,5′R)-menthyloxy-5-oxo-6-oxa-bicyclo[3.1.0]hexane-2,3′-(R)-(4′-(R)-diphenylmethoxy-5′-l-(1′ R,2′ S,5′ R)-menthyloxy-butyrolactone)] (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 737-741 
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    ISSN: 1572-8854
    Keywords: crystal structure ; asymmetric synthesis ; spiro-cyclopropane derivatives
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Crystal structure of C41H53O7Br has been determined by single-crystal X-ray diffraction. The compound crystalline in the orthorhombic space group P212121, with a = 11.264(2), b = 12.058(2), c = 29.337(6) Å, Z = 4. The bond angles of cyclopropane moiety in the molecule are approximate to 60° and agree with theoretic values of the internal angles in a cyclopropane, and two chiral menthyloxy groups are located above and under the whole chiral molecule, respectively. The configuration of the pentacyclic lactone is shown as envelope form.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1012254312765
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  • 13
    Electronic Resource
    Electronic Resource
    Structural Redetermination of Rh4(CO)12 at 293 and 173 K and Analysis of the Thermal Motion in Relation to the Dynamical Behavior (2000)
    Springer
    Journal of cluster science 11 (2000), S. 39-53 
    Details
    ISSN: 1572-8862
    Keywords: thermal motion ; crystal structure ; rhodium carbonyl
    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 structure of Rh4(CO)12 (1) has been redetermined at room temperature and at 173 K. Crystallographic data for 1 at 293 K are as follows: C12O12Rh4, space group P21/c, a=9.209(3), b=11.790(7), c=17.721(8) Å, β=90.46(3)°, V=1924.0(16) Å3, Z=4, 5570 reflections to θ=30.0°, and R=0.030. For 1 at 173 K the data are as follows: space group P21/c, a=9.127(3), b=11.672(6), c=17.492(13) Å, β=90.64(5)°, V=1863.3(18) Å3, Z=4, 3782 reflections to θ=26.3°, and R=0.033. There was no detectable phase change on cooling to 173 K. Crystals of 1 are twinned by pseudo-merohedry, but a satisfactory refinement was obtained by assuming a (100) twinning mirror plane. TLS analysis of the anisotropic displacement parameters at both temperatures has been undertaken. Investigation of the mean square displacement difference between the observed and the rigid body displacement parameters reveals there is a signficant internal motion of the carbonyl ligands relative to the metal skeleton. This motion is consistent with a normal mode or modes of C 3 symmetry.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1009000428525
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  • 14
    Electronic Resource
    Electronic Resource
    A Novel Cluster Consisting of Seven Fused MX6 Octahedra, Li14(THF)8[Ni7Cl17(μ-formamidinate)3(μ-Cl)]2 (2000)
    Springer
    Journal of cluster science 11 (2000), S. 87-94 
    Details
    ISSN: 1572-8862
    Keywords: nickel cluster ; fluorinated formamidine ; 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 When a THF solution made from equimolar amounts of methyllithium and N,N′-bispentafluorophenyl formamidine, C6F5NC(H)N(H)C6F5, was added to a suspension of NiCl2 in THF and the mixture refluxed for 12 h, a bright yellow-green solution was formed, from which a bright green crystalline compound was obtained in 〉60% yield upon partial evaporation of the solvent. This compound, Li14(THF)8[Ni7Cl17(μ-formamidinate)3(μ-Cl)]2·9.4THF, crystallizes in the tetragonal space group P4 2/mnm (No. 136) with Z=2. The core consists of two Ni7 units bridged by two Cl atoms.
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    URL: http://dx.doi.org/10.1023/A:1009008630342
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  • 15
    Electronic Resource
    Electronic Resource
    Organically Templated Vanadium Oxide Phases: Synthesis and Structures of [H3NCH2CH2NH3][V2O6] and [HN(CH2CH2)3NH][VV2VIV4O14]·H2O (2000)
    Springer
    Journal of cluster science 11 (2000), S. 433-447 
    Details
    ISSN: 1572-8862
    Keywords: crystal structure ; vanadium oxide ; organic template ; mixed valence
    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 synthesis and crystal structures of [H3NCH2CH2NH3][V2O6] (1) and [HN(CH2CH2)3NH][VV 2VIV 4O14]·H2O (2) are described. The structure of the oxidized compound 1 consists of parallel stacks of vanadium oxide chains of corner sharing {VO4} tetrahedra. The chains are stabilized by extensive hydrogen bonding involving oxide ligands of the chains and ethylenediammonium ions which fill the space between the stacks of chains. The structure of compound 2 consists of vanadium oxide layers separated by doubly protonated 1,4-diazabicyclo[2.2.2]octane and lattice water. The vanadium oxide layers, containing mixed-valence vanadium (VV and VIV) centers, are composed of zigzag ribbons of edge-sharing {VO5} square pyramids interconnected by {VO4} tetrahedra. Crystal data. C2H10N2O6V2 , 1: monoclinic, space group P21/c (No. 14), a=5.5359(5), b=12.9430(12), c=5.6856(5) Å, α=90, β=97.460(2), γ=90°, V=403.93(6) Å3, Z=2. A total of 2506 reflections (θ max=27.89°) was collected, of which 954 were used to resolve the structure. The structure was solved by direct methods and least-squares refinement converged at R=0.0592. C6H16N2O15V6, 2: monoclinic, space group C2 (No. 5), a=19.303(4), b=6.667(2), c=7.579(2) Å, α=90, β=111.31(2), γ=90°, V=908.4(4) Å3, Z=2. A total of 1779 reflections was collected, of which 1591 unique reflections were used for structural elucidation. The structure was solved by direct methods and least-squares refinement converged at R=0.0314.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1009051500265
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  • 16
    Electronic Resource
    Electronic Resource
    Crystal and molecular structure studies of tris(2-hydroxy-3-t-butyl-5-methylbenzene)-methane trihydrate and N-benzyl-N-phenyl benzamide (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 255-258 
    Details
    ISSN: 1572-8854
    Keywords: THBMBM ; BPB ; crystal structure ; helical packing ; columnar packing ; mesophase transition
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The structures of the title compounds, tris(2-hydroxy-3-t-butyl-5-methylbenzene)-methane)C34H46O3.3H2O, 3) and N-benzyl-N-phenylbenzamide (C20H17NO, 6), have been investigated by X-ray crystallography. Compound 3 crystallizes in the trigonal space group $$P\bar 3 $$ with cell parameters a = 14.090(5) Å, b = 14.090(5)Å, c = 10.485(5)Å, Z = 2. Compound 6 crystallizes in the monoclinic space group C2/c with cell parameters a = 24.533(4)Å, b = 9.176(4)Å, c = 16.711(5)Å, β = 125.88(2)°, Z = 8. Compound 3 has both intra-and intermolecular hydrogen bonds. It also exhibits a helical columnar arrangement of the molecules and goes into mesophase before melting into an isotropic liquid.
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    URL: http://dx.doi.org/10.1023/A:1009595123416
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  • 17
    Electronic Resource
    Electronic Resource
    Synthesis and crystal structure of 4-(p-methoxyphenyl)-3, 5-bis(4-pyridyl)-1,2,4-triazole (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 429-432 
    Details
    ISSN: 1572-8854
    Keywords: Triazole ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The 4-(p-methoxyphenyl)-3,5-bis(4-pyridyl)-1,2,4-triazole has been synthesized and its crystal structure has been determined by X-ray diffraction methods. It crystallizes in the monoclinic space group P21/n, with a = 12.5832(6) Å, b = 7.0512(5) Å, c = 18.4669(12) Å, β = 96.826(1)°, and Dcalc = 1.345 g cm−1 for Z = 4. In the structure, two pyridyl rings, phenyl ring, and triazole ring do not share a common plane. The most favored orientation of the pyridyl rings in the crystal is that their planes are inclined toward opposite directions with respect to the triazole ring.
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    URL: http://dx.doi.org/10.1023/A:1009542208264
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  • 18
    Electronic Resource
    Electronic Resource
    Crystal structure and spectroscopy of the low-spin iron(II) compound: tris(bipyrimidine)iron(II) bis(triflate), [Fe(bipym)33](CF3SO3)2 (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 441-444 
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    ISSN: 1572-8854
    Keywords: 2,2′-Bipyrimidine ; low-spin ; iron ; crystal structure ; infrared
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The compound [Fe(bipym)33](CF3SO3)2 (in which bipym = 2,2′-bipyrimidine) crystallizes in the space group P21/c, with a = 13.7641(11), b = 18.7557(19), c = 12.3627(11) Å, β = 103.085(8)° and Z = 4. The low-spin Fe(II) atom is octahedrally surrounded by six nitrogen atoms of three bipyrimidine groups with Fe—N distances that vary from 1.968(4) to 1.975(4) å. In the far-infrared region the Fe—N vibrations are observed at 359 and 372 cm-1.
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    URL: http://dx.doi.org/10.1023/A:1011339214337
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  • 19
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    Electronic Resource
    Crystal structure of a novel bis(guanidiniums) compound incorporated by sulfate anion (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 483-487 
    Details
    ISSN: 1572-8854
    Keywords: Bis(guanidiniums) ; sulfate anion ; hydrogen bond ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Crystal structure of a novel bis(guanidiniums) compound 1 by sulfate anion and water, C11H20N6OċSO4ċH2O, was measured by X-ray crystallographic analysis with an “imaging plate” method. It possesses space group P21/c, with a = 7.6433(15), b = 19.447(4), c = 12.115(2) Å, β = 107.81(3)°, and φcalc = 1.420 mg/m3 for Z = 4. Crystal data indicate that the architecture network is formed through hydrogen bonds, electrostatic interactions, and arene–arene stacking interaction among the bis(guanidiniums) compound, the sulfate anion and water molecule.
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    URL: http://dx.doi.org/10.1023/A:1011359702042
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  • 20
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    Electronic Resource
    Redetermination of the structure of bis[chloro-2-(2-hydroxy-4,5-dimethylphenylazo)-5,5-dimethyl-4,5,6,7-tetrahydrobenzothiazol-7-on] copper(II) complex (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 505-507 
    Details
    ISSN: 1572-8854
    Keywords: Bis[chloro-2-(2-hydroxy-4,5-dimethylphenylazo)-5,5-dimethyl-4,5,6,7-tetrahydrobenzothiazol-7-on]copper(II) ; thiazolylazo dye ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal structure of C17H18ClCuN3O2S (M = 854.78, monoclinic, P21/c, a = 8.316(2), b = 18.461(4), c = 11.774(2) Å, β = 99.64(3)°, V = 1782.0(7) Å3, Z = 4) is formed by dimeric molecules [C17H18ClCuN3O2S]2 with two monomeric units linked together by two chlorine atoms. The Cu atom is coordinated by two chlorine atoms, an oxygen atom, the azo nitrogen atom attached to the benzene ring, and the nitrogen atom of the thiazole ring, in the form of a distorted tetragonal pyramid.
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    URL: http://dx.doi.org/10.1023/A:1011377120727
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  • 21
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    Electronic Resource
    Synthesis and crystal structure of the perchlorate salt of diprotonated N,N′-bis(1-methylimidazole-2-methyl)1,5-diazacyclooctane (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 531-534 
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    ISSN: 1572-8854
    Keywords: 1,5-Diazacyclooctane (DACO) ; crystal structure ; boat/chair configuration
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The diprotonated perchlorate salt of a new 1,5-diazacyclooctane (DACO) mesocycle functionalized by two imidazole pendants, N,N′-bis(1-methylimidazole-2-methyl)-1,5-diazacyclo-octane (C16H28N6Cl2O8), has been synthesized and the structure determined by X-ray diffraction analysis. The title compound crystallizes in the monoclinic system, space group P21/c with a = 11.964(2), b = 13.251(3), c = 14.741(3) Å, β = 106.00(3)°, Mr = 503.34, V = 2246(1) Å3, Z = 4. The crystal structure of the title compound reveals that the DACO ring is also folded up into the “chair/boat” configuration, which is consistent with the configuration in most of the transition metal complexes of DACO and its derivatives. The two imidazole pendants of the compound are in cis position with a dihedral angle of 16.0(4)°.
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    URL: http://dx.doi.org/10.1023/A:1011337722544
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  • 22
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    Electronic Resource
    Structural and spectroscopic characterization of tris (o-phenanthroline)iron(II) disaccharinate monosaccharin hexahydrate (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 539-544 
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    ISSN: 1572-8854
    Keywords: Iron(II) ; o-phenanthroline ; saccharinate ; crystal structure ; spectroscopic properties ; thermal behavior
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal and molecular structure of the title compound, for short [Fe(o-phen)3](sac)2·(Hsac)·6H2O, has been determined by X-ray diffraction methods. It crystallizes in the monoclinic space group P21/n with a = 16.3190(1), b = 19.2890(1), c = 17.4490(2) Å, β = 92.586(1)°, V = 5486.95(8) Å3 and, Z = 4. The investigated compound constitutes the first example of a species in which uncoordinated saccharin and saccharinate anions are present in the structure. The crystallographic results reveal the subtle differences between the structure of the neutral molecule and its anion. The complex was also characterized by means of infrared, electronic, and 57Fe-Mössbauer spectroscopy. Its magnetic susceptibility was determined at room temperature and its thermal behavior investigated by means of thermogravimetric and differential thermal analytical techniques.
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    URL: http://dx.doi.org/10.1023/A:1011341823452
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  • 23
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    Electronic Resource
    Synthesis and X-ray structure of [(H3O)(C14H20O5)2][Me2NH2]2 [PMo12O40] · 2C14H20O5 (C14H20O5 = benzo-15-crown-5; Me2NH = dimethylamine) (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 577-581 
    Details
    ISSN: 1572-8854
    Keywords: Oxonium ions ; crystal structure ; molybdophosphate ; crown ether
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract [(H3O)(C14H20O5)2][Me2NH2]2 [PMo12O40] · 2C14H20O5 1 was synthesized from benzo-15-crown-5 and H3PMo12O40·24H2O in N,N′-dimethylformamide for the first time. 1 crystallizes in the monoclinic space group C2/c with a = 18.583(4), b = 25.510(5), c = 19.904(4) Å, β = 94.66(3)° D c = 2.124 mg/m3 for Z = 4. Refinement based on 7358 observed reflections led to a R1(wR2) = 0.0378(0.0761). The complex cation, [(H3O)(C14H20O5)2]+, exhibits a sandwich structure by hydrogen-bonding in the mean distance of 2.955 Å. The anion, PMo12O40 3−, is a α-Keggin structure.
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    URL: http://dx.doi.org/10.1023/A:1011354226178
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  • 24
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    Electronic Resource
    Synthesis, spectroscopy, and X-ray structure of the polymer catena-[bis(azido-N)-copper(II)-μ-bis(2-benzimidazolyl)butane] (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 69-72 
    Details
    ISSN: 1572-8854
    Keywords: azido ; crystal structure ; copper(II) ; infrared ; polymeric
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound, catena-[bis(azido-N)-copper(II)-μ(bis(2-benzimidazolyl)butane), [Cu(C18H18N4)(N3)2]n, was obtained from the reaction of the ligand bis(2-benzimidazolyl)butane and Cu(N3)2. The x-ray crystal structure is reported. The compound crystallizes in the monoclinic space group P21/c with a = 8.2524(10), b = 12.765(5), c = 9.1125(15) Å, β = 106.423(12)°, Z = 2. The Cu(II) ions are square-planar coordinated with trans-oriented end-on binding azido ligands. The structure is a polynuclear chain with the benzimidazole bridging at each end. In addition a N(ligand)-H···N(azido) H-bridge [N(ligand)···N(azido) = 2.994(7) Å] is present, resulting in a pseudo 2-dimensional lattice. The characteristic azido infrared vibrations are found at 2060 and 2077 cm−1 (νas(N3)) and 1284 and 1297 cm−1 (ν(N3)).
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    URL: http://dx.doi.org/10.1023/A:1009506418398
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  • 25
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    Electronic Resource
    Synthesis and crystal structure of [Tb4(H2O)2](C2O4)2(C5H6O4)4 (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 633-639 
    Details
    ISSN: 1572-8854
    Keywords: Lanthanide ; oxalate ; glutarate ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract A terbium complex associating two ligands, oxalate and glutarate, was prepared under hydrothermal conditions at 200°C by treating an aqueous suspension of terbium oxalate decahydrate with glutaric acid and guanidinium carbonate. Its structure was solved by X-ray diffraction on a single crystal. It crystallizes in the monoclinic space group P21 with lattice constants, a = 9.514(1) Å, b = 9.0681(8) Å, c = 19.702(2) Å, and β = 97.90(1)°. The terbium atoms and the oxalate ligands build dense chains which are connected by one side of the carboxylic group of some glutarate ligands, thus forming a sheet at the c level ≅ 0 and 1/2. These sheets are bridged by glutarate groups. The terbium atoms are ninefold coordinate with nine oxygen atoms of the ligands or with one water molecule and eight oxygen atoms of the ligands. Each polyhedron of the terbium atoms share one edge and one face of oxygen atoms with the two neighboring ones. The oxalate ligands are bischelating and bismonodentate. The coordination scheme of glutarate differs: either they are bismonodentate from one side and chelating and monodentate from the other side or they are chelating and monodentate from both sides.
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    URL: http://dx.doi.org/10.1023/A:1011992031111
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  • 26
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    Electronic Resource
    Terbium and holmium trans-2,3-dimethylacrylic acid complexes with 1,10-phenanthroline (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 777-782 
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    ISSN: 1572-8854
    Keywords: terbium complex ; holmium complex ; crystal structure ; trans-2,3-dimethylacrylic acid
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Novel dinuclear complexes, [REL3(phen)]2 (where RE = Tb, Ho; HL = trans-2,3-dimethylacrylic acid; phen = 1,10-phenantheoline), were synthesized and determined by elemental analysis, infrared absorption spectra (IR), thermogravimetric analysis (TGA), and X-ray diffraction. The Tb complex crystallizes in space group P21/n with the cell dimensions a = 12.939(2) Å, b = 13.018(2) Å, c = 15.400(3) Å and β = 94.72(1)°. The Ho complex crystallizes in P (9) with a = 12.406(3) Å, b = 13.280(3) Å, c = 9.823(2) Å, α = 110.80(2)°, β = 103.42(2)°, γ = 63.67(1)°. The Tb atom is nine coordinate and the separation of Tb...Tb* is 3.97 Å. The Ho atom is eight coordinate and the separation of Ho...Ho* is 4.01 Å.
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    URL: http://dx.doi.org/10.1023/A:1013220207596
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  • 27
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    Electronic Resource
    Synthesis and crystal structure of 1-(1′,3′-dimethyl-5′-chloropyrazol-4′-carbonyl′-3-(2′-chlorophenyl)-5-amino-4-cyanopyrazole (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 789-792 
    Details
    ISSN: 1572-8854
    Keywords: crystal structure ; pyrazolide
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound 1-(1′,3′-dimethyl-5′-chloropyrazol-4′-carbonyl)-3-(2′-chlorophenyl)-5-amino-4-cyanopyrazole (C16H12Cl2N6O) has been synthesized and characterized by X-ray diffraction: Triclinic, space group P1, with a = 8.6712(8) Å, b = 9.5091(10) Å, c = 11.2170(11) Å α = 71.531(2)°, β = 84.683(2)°, γ = 74.099(2)° Z = 2; V = 843.7(14) Å3. C(10), O(1), C(11), and N(2) atoms are coplanar with the average deviation of 0.0071 Å, which form 11.03° and 43.93° dihedral angles with pyrazole planes (I) and (II), respectively.
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    URL: http://dx.doi.org/10.1023/A:1013224308504
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  • 28
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    Structure, thermal behavior, and IR investigation of bis(3-amino-1,2,4-triazolium)monohydrogen monophosphate (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 805-809 
    Details
    ISSN: 1572-8854
    Keywords: organic phosphate ; crystal structure ; DTA/TG/DSC ; IR spectra
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Chemical preparation, calorimetric studies, crystal structure, and IR spectrometric investigation of (C2H5N4)2HPO4, denoted ATZP, are described. The compound crystallizes in the monoclinic system with C2/c space group. Its unit cell dimensions are a = 13.589(2) Å b = 11.105(2) Å c = 15.734(3) Å β = 104.68(2)°, V = 2296.8(7) Å3, and Z = 8. The structure of the title compound consists of a three dimensional network of H-bonds connecting all its components. The IR spectrum of ATZP is reported and discussed on the basis of group theoretical analysis.
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    URL: http://dx.doi.org/10.1023/A:1013280426251
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  • 29
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    Electronic Resource
    Crystal structure of [WI2(CO)2{P(OiPr)3}(η2-EtC2Et)] (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 181-184 
    Details
    ISSN: 1572-8854
    Keywords: tungsten(II) ; diiodo ; dicarbonyl ; triisopropylphosphite ; 3-hexyne ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract [WI2(CO)2{P(OiPr)3}(η2-EtC2Et)] crystallizes in the monoclinic space group P21/n, with a = 11.101(12), b = 16.272(18), c = 14.892(17) Å, β = 93.27(1), Z = 4. The geometry can be considered to be pseudo-octahedral, with the 3-hexyne ligand occupying one site, with two iodo-groups, and the P(OiPr)3 ligand completing the equational plane of ligands, with two trans-carbonyl groups occupying the axial sites.
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    URL: http://dx.doi.org/10.1023/A:1009531014474
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  • 30
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    Electronic Resource
    Synthesis, crystal structure and molecular modeling (AM1) of two 5-arylidene derivatives of Meldrum's acid (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 189-194 
    Details
    ISSN: 1572-8854
    Keywords: crystal structure ; AM1 ; x-ray diffraction ; Meldrum's acid
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The synthesis and structural characterization of two 5-Arylidene derivatives of Meldrum's acid (2,2-dimethyl-1,3-dioxane-4,6-dione) are described: 5-(4-Nitrobenciliden)-2,2-dimethyl-1,3-dioxane-4,6-dione (3a), and 5-(4-Methoxybenciliden)-2,2-dimethyl-1,3-dioxane-4,6-dione (3b). The structure of 3a was refined to R1 = 0.0421 for 2148 reflections (with I 〉 2σ (I)). Crystal data for 3a: C13H11NO6, orthorhombic, space group Pbca, a = 16.008(3), b = 6.137(1), c = 25.281(5) Å, V = 2483.6(8) Å3, Z = 8. The structure of 3b was refined to R1 = 0.0496 for 4681 reflections (with I 〉 2σ(I)). Crystal data for 3b: C14H14O5, triclinic, space group P1, a = 9.131(2), b = 9.922(2), c = 14.490(3)Å, α = 85.076(6), β = 84.80(3), γ = 89.37(2)°,V = 1302.4(5) Å3, Z = 4. The results of crystallographic and molecular modeling (AM1) were compared. The molecules in the crystal are held together, in both compounds, by van der Waals forces and C—H···O hydrogen bond interactions.
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    URL: http://dx.doi.org/10.1023/A:1009535215383
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  • 31
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    Separation of rosin acids by molecular recognition: crystal structure of the complex of neoabietic acid with 2-amino-6-methyl-pyridine (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 195-198 
    Details
    ISSN: 1572-8854
    Keywords: neoabietic acid ; amino(methyl)pyridine ; crystal structure ; molecular recognition ; H-bonding ; rosin acid
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Neoabietic acid has been separated from gum rosin mixture by the aid of molecular recognition using 2-amino-6-methyl-pyridine as recognition reagent. The complex of neoabietic acid with 2-amino-6-methy-pyridine crystallizes from ether solution in the monoclinic, space group P21 with cell parameters of a = 7.370(1), b = 8.692(1), c = 18.365(2) Å, β = 92.53(1)°,V = 1175.3(2) Å3 and Z = 2. X-ray structure analysis shows that an extensive H-bonding network exists between neoabietic acid and amino(methyl)pyridine, which is considered as one of the factors resulting in successfully separating the neoabietic acid from the gum rosin mixture.
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    URL: http://dx.doi.org/10.1023/A:1009587232221
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  • 32
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    Crystal structure of a novel tertiary phosphine coordination complex: dichlorobis(tribenzylphosphine)nickel(II) (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 173-176 
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    ISSN: 1572-8854
    Keywords: phosphine ; nickel(II) complexes ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound dichlorobis(tribenzylphosphine)nickel(II), Ni[P(CH2C6H5)3]2Cl2, belongs to a type of tertiary phosphine coordination complex, M(PR3)2X2. There are two molecules in the unit cell which do not appear to interact chemically. Both molecules have a trans-square planar configuration with each nickel atom on a center of symmetry. Three benzyl groups are bonded to each phosphorus atom as rotors in a propeller, and the threefold axis is along the P—Ni bond, which has a mean length of 2.23(1) Å. Crystal data: C42H42Cl2NiP2, Triclinic, space group $$P\bar 1 $$ , a = 10.4892(15) b = 10.5249(12) c = 19.453(2) Å, α = 83.872(8), β = 76.839(9), γ = 62.241(8)°, V = 1850.5(4) Å3, Z = 2. There is an intramolecular hydrogen bond between the C3 and C11 atoms.
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  • 33
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    A dinuclear cyanide-bridged complex, [(DMF)4(H2O)3LuCo(CN)6]·H2O (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 671-675 
    Details
    ISSN: 1572-8854
    Keywords: Synthesis ; crystal structure ; lutetium(III) ; cobalt(III) hexacyanide ; cyanide bridging
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal structure of the bimetallic cyanide bridged complex [(DMF)4(H2O)3LuCo(CN)6]·H2O (1) was obtained by single-crystal X-ray diffraction. The central lutetium(III) ion is eight coordinate arranged in a square antiprism while the cobalt(III) ion is six coordinate, oriented octahedrally. Molecules in the crystal lattice are held together by a network of hydrogen bonding. Crystallization of 1 occurs in the centrosymmetric monoclinic space group P21/c (No. 14) with a = 13.875(2), b = 8.8352(9), c = 24.633(2) Å β = 96.392(8)° and Z = 4.
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    URL: http://dx.doi.org/10.1023/A:1011952316999
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  • 34
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    Identification of a new family of diphosphate compounds, AI2BII3(P2O7)2: Structures of Ag2Co3(P2O7)2, Ag2Mn3(P2O7)2, and Na2Cd3(P2O7)2 (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 705-716 
    Details
    ISSN: 1572-8854
    Keywords: mixed metal diphosphates ; AI 2BII 3(P2O7)2 ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Syntheses and single-crystal X-ray structural results are reported for three new mixed diphosphates of the family AI 2BII 3(P2O7)2; Ag2Co3(P2O7)2 (I), Ag2Mn3(P2O7)2 (II), and Na2Cd3(P2O7)2 (III). All crystallize in the triclinic system, space group P1 bar: (I) a = 5.351(4), b = 6.375(4), c = 16.532(4) Å, α = 80.83(6) β = 81.45(4), γ = 72.87(5)°, V = 528.9(6) Å3, Z = 2, D calc = 4.649 mg/m3, R/Rw = 0.0428/0.0548 for 3949 obs. reflns; (II) a = 5.432(7), b = 6.619(6), c = 16.51(3) Å, α = 80.78(8) β = 82.43(9), γ = 72.82(7)°, V = 557.7(13) Å3, Z = 2, D calc = 4.338 mg/m3, R/Rw = 0.0679/0.1303 for 2100 obs. reflns and (III) a = 5.67(3), b = 7.08(4), c = 7.90(4) Å, α = 77.0(2), β = 82.5(2), γ = 67.8(2)°, V = 286(3) Å3, Z = 2, D calc = 4.249 mg/m3, R/Rw = 0.0307/0.0342 for 1945 obs. reflns. (I) and (II) are isostructural but (III) is of a different type. All three structures are characterized by layers of P2O7 groups alternating with layers of mixed metal atoms. Differences are seen in the conglomerate bonding patterns of B atoms and in the irregular geometry of Ag in (I) and (II) compared to the octahedral bonding seen for Na in (III). The differences in structure may be understood in terms of the ratios of the ionic radii of A and B atoms.
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  • 35
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    Crystal structure of diethoxynitrobenzene-p-tert-butylcalix [4]arene⋅2(CH3)2C=O: Evidence of intra- and intermolecular CH/π interactions forced by crystal packing (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 717-720 
    Details
    ISSN: 1572-8854
    Keywords: calix[4]arene ; CH/π interaction ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Diethoxynitrobenzene-p-tert-butylcalix[4]arene⋅2(CH3)2C=O crystallized in the monoclinic system, space group P21/c, with cell dimensions a = 16.1437(2) Å, b = 21.0292(2) Å, c = 18.9685(3) Å and β = 110.308(1)°. The asymmetric unit consists of a diethoxynitrobenzene-p-tert-butylcalix[4]arene molecule and two solvated acetone molecules. Besides the usual CH/π interaction between p-tert-butylcalix[4]arene π cavity and a solvated acetone, this structure shows the intra- and intermolecular CH/π interactions among a nitrobenzene ring, ethylene bridge of the ethoxynitrobenzene side chain and a solvated acetone molecule.
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    URL: http://dx.doi.org/10.1023/A:1012246110948
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  • 36
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    Crystal structure of a 26-membered hexaaza macrocycle bearing hydroxyethyl pendants containing p-xylyl spacers (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 743-747 
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    ISSN: 1572-8854
    Keywords: macrocycle ; hydroxyethyl pendant ; crystal structure ; hydrogen bonds
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The new macrocyclic compound bearing hydroxyethyl pendant arms containing p-xylyl spacers, 3,6,9,16,19,22-hexaaza-6,19-bis(2-hydroxyethyl)-tricyclo[22,2,2,211,14] triaconta-1,11,13,24,27,29-hexaene, crystallizes in the monoclinic space group P21/c with a = 8.700(2) Å, b = 18.301(4) Å, c = 11.766(2) Å, β = 108.57(2)°. The two hydroxyethyl pendants are at the opposite sides of the macrocyclic plane. Benzene rings in macrocycle are parallel and exist the π-π weak interaction with distance of 4.28 Å. The crystal packing of the macrocycle is stabilized by the hydrogen bonds.
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  • 37
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    Electronic Resource
    Crystal structure, thermal analysis, and IR spectrometric investigation of bis(tert-butylammonium) sulfate (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 799-804 
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    ISSN: 1572-8854
    Keywords: organic sulfate ; crystal structure ; DTA/TG/DSC ; IR spectra
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Chemical preparation, X-ray single crystal, thermal analysis, and IR spectrometric investigation of (C4H12N)2SO4, denoted tBAS, are described. The compound crystallizes in the monoclinic system with C2/c space group. Its unit cell dimensions are a = 11.1585(5) Å, b = 6.2148(4) Å, c = 20.070(1) Å, β = 102.004(4)°, V = 1361.4(1) Å3, and Z = 4. The crystal structure of tBAS can be described as a typical thick layered organization built by all the components of the structure and centered by planes z = 1/4 and 3/4. Connection in these layers are established by N—H···O hydrogen bonds. Thermal analysis shows a reversible weak phase transition.
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  • 38
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    Electronic Resource
    Crystal structure and spectroscopy of bis-[bis(2-benzimidazolyl)propane]copper(II) bis(triflate)monohydrate, a copper complex with a geometry intermediate between tetrahedral and square planar (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 793-797 
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    ISSN: 1572-8854
    Keywords: copper ; bis(benzimidazoles) ; crystal structure ; infrared
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The structure of a mononuclear copper(II) compound with the ligand bis(2-benzimidazolyl)propane (abbreviated as tbz) is reported. The compound [Cu(tbz)2](CF3SO3)2(H2O) crystallizes in the triclinic space group P $$\bar 1$$ , with a = 12.363(6), b = 13.218(9), c = 15.365(8) Å, α = 82.74(5), β = 68.04(4), γ = 65.30(5), and Z = 2. The Cu(II) atom has a geometry intermediate between tetrahedral and square planar, consisting of four nitrogen atoms of two tbz ligands. The Cu—N—Cu angles are about 135°, while the dihedral angle between them amounts to 62° (0° for square planar and 90° for a tetrahedron). Ligand field bands are observed at 10.2 × 103, 13.8 × 103, and 20.3 × 103 cm−1, while the most characteristic infrared vibrations of the triflate anion are observed at 1273, 1260, 1238, 1221, 1171, and 1157 cm−1.
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  • 39
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    Electronic Resource
    Crystal structure and thermal analysis of 1,5-diammonium-2-methyl pentane sulfate monohydrate (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 95-98 
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    ISSN: 1572-8854
    Keywords: organic sulfate ; crystal structure ; DTA/TG/DSC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Chemical preparation, x-ray single crystal, and thermal analysis of C6H18N2SO4·H2O (denoted DMPS) are described. The compound crystallizes in the triclinic system with P $$\overline 1$$ space group. Its unit cell dimensions are a = 5.826(1) Å, b = 10.014(1) Å, c = 11.221(1) Å, α = 66.716(1)°, β = 84.395(1)°, γ = 83.759(1)°, V = 596.7(1) Å3, and Z = 2. The DMPS structure is built up from inorganic chains parallel to the a axis and linked via O(W)-H···O hydrogen bonds. These chains are interconnected by organic groups. Thermal analysis reveals the presence of one water molecule in the structure and shows a reversible weak phase transition.
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  • 40
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    Molecular structure and 1H, 13C NMR assignments of 1,3,5-tris(imidazol-1-ylmethyl)-2,4,6-trimethylbenzene (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 115-118 
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    ISSN: 1572-8854
    Keywords: 1,3,5-tris(imidazol-1-ylmethyl)-2,4,6-trimethylbenzene (titmb); crystal structure; hydrogen bonding; 2D NMR ; crystal structure ; hydrogen bonding ; 2D NMR
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The molecule 1,3,5-tris(imidazol-1-ylmethyl)-2,4,6-trimethylbenzene (titmb) crystallizes as a monohydrate in the monoclinic space group C2/c with a = 20.888(4), b = 13.220(2), c = 14.385(2) Å, β = 90.36(1)°. Two of three imidazole groups are on one side of the central benzene ring, and the other one is on the opposite side. The crystal packing of titmb is stabilized by O-H--N hydrogen bonding between the water molecule and nitrogen atoms of the imidazole group. The complete 1H and 13C NMR assignments for titmb were carried out by 2D NMR spectral measurements.
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  • 41
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    Crystal structure of 2,6-dimethylpyridinium hydrogen phthalate (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 119-122 
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    ISSN: 1572-8854
    Keywords: phthalic acid ; 2, 6-dimethylpyridine ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract A new crystal of 2,6-dimethylpyridinium hydrogen phthalate (DPMHP) has been prepared and characterized by x-ray crystallography. DPMHP crystallizes in the monoclinic space group C2/c with a = 26.105(3), b = 8.2250(10), c = 13.8750(10) Å, β = 116.02(1)°, V = 2677.2(5) Å3, and Z = 8. The 2,6-dimethylpyridinium (DPM) is held with the hydrogen phthalate ion (HPI) by intermolecular hydrogen bond of N-H-O. A noncentered hydrogen atom is involved in the short intramolecular hydrogen of O-O [2.398(2) Å] between the neighboring carboxylic groups. The phenyl ring of the HPI appears to be deformed in comparison with the original. The entity of HPI in itself and DMPMHP as a whole are arranged in a rumple pattern. The geometrical arrangement in the crystal structure is characterized by the formation of laminar ribbons of DPMHP.
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  • 42
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    The crystal structures of two reaction products of α-halopyruvamide with nitrogen and sulfur nucleophiles (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 109-113 
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    ISSN: 1572-8854
    Keywords: α-halopyruvamide derivatives ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Two compounds have been prepared during the investigation of the reactivity of α-halopyruvamides. The reaction products: 3-(4-chlorophenyl)imidazo[1,2-a]pyridine-2-carboxamide (1) and 7-carbamoyl-5-phenyl-2,3-dihydro[1,3]thiazolo[4,3-b][1,3]thiazol-4-ium chloride (2) were structurally characterized by x-ray crystallography. Compound 1 crystallizes in the orthorhombic space group Pca21 with a = 28.813(2), b = 9.369(1), and c = 9.361(1) Å. The structure contains two crystallographically different molecules. Compound 2 crystallizes in the monoclinic space group P21/c with the following cell parameters: a = 8.5895(8), b = 22.499(2), c = 7.4133(6) Å, and β = 110.204(1)°.
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  • 43
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    Synthesis and molecular structure of N-[3-(p-bromophenyl)-1,2,4-oxadiazol-5-yl]methylphthalimide. III. (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 131-134 
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    ISSN: 1572-8854
    Keywords: 1,2,4-Oxadiazole ; crystal structure ; phthalimide derivative ; AM1 method ; STO-3G basis set
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The synthesis, spectroscopic studies and crystal structure of the title compound is described. The crystallographic studies showed that the p-bromophenyl group is very nearly coplanar with the 1,2,4-oxadiazole ring. The nearly planar phthalimide group makes an angle of about 98° with the bromophenyloxadiazole plane. Semi-empirical (AM1) and ab initio (STO-3G, 6-31G) molecular orbital calculations have been carried out for this compound and a comparison of bond angles, bond lengths and torsion angles has been made with the experimental values, which are remarkably close to each other. This compound crystallizes in the monoclinic space group P21/c with a = 13.6299(2),b = 13.9836(2), c = 8.4817(2) Å, β = 101.9070(10)°, V = 1581.79(5) Å3, and Z = 4.
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  • 44
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    Electronic Resource
    Crystal and molecular structure of augustamine (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 135-138 
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    ISSN: 1572-8854
    Keywords: alkaloid ; tazettine type ; amaryllidaceae ; crystal structure ; molecular mechanics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal and molecular structure of augustamine (1), C17H19NO4 an amaryllidaceae alkaloid of the tazettine group has been determined by direct methods from single crystal x-ray diffractometer data and refined by full-matrix least squares. The alkaloid (1) crystallizes in the space group P212121, with cell parameters: a = 7.833(8) b = 11.08(2) å, c = 16.69(6) Å, Z = 4, Dc = 1.381 g/cm−3, R = 7.6% for 1115 observed reflections. The molecule, having a hexacyclic ring system, is very rigid with the ring B in a chair conformation. Molecular mechanics calculations have been made using MM3(2000) force field.
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  • 45
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    Electronic Resource
    Synthesis, crystal structure of a one-dimensional cobalt—azide complex through hydrogen bond (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 159-162 
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    ISSN: 1572-8854
    Keywords: crystal structure ; cobalt (II) complex ; one-dimensional chain ; hydrogen bond
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract A one-dimensional chain complex, {[Co(bpm)2(N3)2][Co(bpm)2(H2O)2]} (ClO4)2, (bpm being bis(pyrazol-l-yl)methane), has been synthesized and characterized by X-ray diffraction: triclinic, space group P - 1 with a = 8.805(2) Å, b = 8.902(2) Å, c = 13.621(3) Å, α = 84.27(3)°, β = 84.63(3)°, γ = 80.05(3)°, V = 1043.2(4) Å3, Z = 1. Two cobalt atoms have ideal octahedral environments with different coordination atoms. One cobalt atom is six-coordinated with nitrogen atoms from two bpm ligands and two azide ligands, while the other cobalt atom is coordinated by four nitrogen atoms from bpm and two oxygen atoms from water molecules. The complex forms one-dimensional chain through hydrogen bonds.
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  • 46
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    Electronic Resource
    Syntheses, characterization, and structural analyses of several f-block isothiocyanatonitrato complexes (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 301-309 
    Details
    ISSN: 1572-8854
    Keywords: Synthesis ; crystal structure ; dioxouranium(VI) ; lanthanide(III) ; thiocyanate ; nitrate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Reactions of tetra-n-butylammonium thiocyanate with lanthanide and uranyl nitrates yield complexes of the general type [(Bu)4N]x[M(NCS)y(NO3)z]. Samples of [(Bu)4N]2 [UO2(NCS)3( NO3)] (1), [(Bu)4N]3[Yb(NCS)4(NO3)2] (2), and [(Bu)4N]3[Nd(NCS)4(NO3)2rsqb; (3) were prepared from alcohol solutions. Crystallization of 1 occurs in the centrosymmetric monoclinic space group C2/c (No. 15) with a = 17.949(4) Å, b = 16.587(3) Å, c = 16.763(3) Å; β = 99.77(3)°; and Z = 4. The seven-coordinate uranium(VI) ion exhibits a pentagonal bipyramid coordination environment. Crystallization of 2 occurs in the centrosymmetric orthorhombic space group Pnnn (No. 48) with a = 12.530(2) Å, b = 12.9440(10) Å, c = 21.203(2) Å; Z = 2. The eight-coordinate ytterbium(III) ion expresses a dodecahedral coordination environment. Crystallization of 3 occurs in the noncentrosymmetric monoclinic space group Cc (No. 9) with a = 16.556(2) Å, b = 18.130(2) Å, c = 23.984(4) Å; Z = 4. The 10-coordinate neodymium(III) ion exhibits a dodecahedral coordination environment. Characterization includes physical property determinations, conoscopic studies, IR spectroscopic identifications, and UV spectral data. Details of the syntheses along with selected bond distances and angles are presented and discussed.
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  • 47
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    Electronic Resource
    A dimeric pervanadyl (VO2+) complex with a tridentate Schiff base ligand (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 329-333 
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    ISSN: 1572-8854
    Keywords: Pervanadyl complex ; Schiff base ; di(μ-oxo)-bridged dimer ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract A di(μ-oxo)-bridged dinuclear complex, [VO2(pamh)]2 was isolated by reacting bis(acetylacetonato)vanadium(IV) and the Schiff base, N-(anisoyl)-N′-(picolinylidene)-hydrazine (Hpamh) in acetonitrile. The complex crystallizes in the space group $$P\bar 1 $$ ;1; (#2) on crystallographic inversion center. Crystal data: a = 8.2202(12) Å, b = 9.8389(19) Å, c = 10.1907(17) Å, α = 68.245(15)°, β = 74.47(2)°, γ = 66.710(19)°, V = 696.0(2) Å3, and Z = 1. The physical properties of the complex and the structural parameters are consistent with the +5 oxidation state of the metal ions. The monomeric VO2(pamh) unit is square-pyramidal. The planar mononegative ligand (pamh−) coordinates the metal ion via the pyridine-N, the imine-N, and the amide-O atoms. One of the oxo groups completes the NNOO basal plane and also participates in the Vndash;Ondash ;V bridge formation. The other oxo group satisfies the fifth apical coordination site. The molecular structure of the dimeric complex, [VO2(pamh)]2 can be described as two edge-shared distorted VO4N2 octahedra.
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  • 48
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    Electronic Resource
    Crystal structure and spectroscopy of a hydrogen-bridged one-dimensional Cu(II) complex containing both octahedral and square pyramidal geometries in the same unit cell (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 351-357 
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    ISSN: 1572-8854
    Keywords: Helical hydrogen-bridged one-dimensional Cu(II) complex ; trans-4-styrylpyridine ; crystal structure ; IR and electronic spectroscopy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Single crystals of the helical hydrogen-bridged one-dimensional Cu(II) complex, [Cu(stpy)2(CH3COO)2(H2O)2] (1) [Cu(stpy)2(CH3COO)2(H2O)] (2), are prepared and characterized by elemental and thermal analyses, IR, electronic and X-ray crystal structure determination. The crystals are monoclinic, of space group C2/c, with unit cell parameters a = 31.842(7) Å, b = 5.9829(10) Å, c = 30.970(14) Å, β = 111.78(3)°, Z = 4. The asymmetric unit contains two different types of Cu(II) polyhedra, namely, octahedron and square pyramid within the same unit cell. 1 has elongated octahedral geometry with two nitrogen atoms from stpy and two oxygen atoms from synmonodentate acetate ligands, transcoordinated to Cu(II) in the basal plane. The oxygen atoms of the two water molecules occupy the axial positions. 2 has Cu(II) coordination polyhedra similar to 1, except that only one of the apical positions is occupied by a water molecule. The structure consists of two independent linear chains, one involving octahedral (1) and the other involving square-pyramidal (2) polyhedra, held by hydrogen bridges. The Cu–Cu intra- and interchain separations in both 1 and 2 are 5.983 and 8.214 Å. The unit cell packing shows weak π-stacking between adjacent coordinated stpy ligands in the chain, resulting in ladder-type structure. Further, the extended packing reveals helical arrangement of Cu(II) polyhedra in the lattice.
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  • 49
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    Crystal structure of [Yb(L(NO3)2(H2O)2](NO3), L = bromo-N,N,N′,N′-tetraethylmalonamide (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 455-458 
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    ISSN: 1572-8854
    Keywords: Ytterbium ; malonamide ; crystal structure ; extraction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract [Yb(L(NO3)2(H2O)2](NO3), L = bromo-N,N,N′,N′-tetraethylmalonamide crystallizes in the triclinic spacegroup P-1 with cell dimensions a = 9.030(9), b = 12.036(12), c = 12.392(13) Å, α = 84.52(1), β = 77.58(1), γ = 67.21(1)° , dcalc = 1.935 g cm-3 for Z = 2. The ytterbium atom in the complex cation is nine-coordinate being bonded to two oxygen atoms from the malonamide ligand, two nitrate anions, and three water molecules.
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  • 50
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    Electronic Resource
    N-Arylmaleimide derivatives (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 563-571 
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    ISSN: 1572-8854
    Keywords: Maleimide ; crystal structure ; photopolymerization ; monomer ; conformation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Nine phenyl substituted N-phenylmaleimide monomers for photopolymerization studies have been characterized by x-ray crystallography. Structures for N-(2′-t-butylphenyl)maleimide (1), P21/n, a = 10.197(3) Å, b = 11.904(4) Å, c = 10.496(5) Å, β = 100.61(3)° N-(2′-trifluoromethylphenyl)maleimide (2), P21/c, a = 11.763(8) Å, b = 10.699(9) Å, c = 8.284(5) Å, β = 90.02(5)° N-(2′,6′-diisopropylphenyl)maleimide hemibenzene solvate (3), Pc, a = 16.747(6) Å, b = 8.552(3) Å, c = 12.899(4) Å, β = 105.08(3)° N-(2′,6′-diisopropylphenyl) maleimide (unsolvated) (4), C2/c, a = 28.146(10) Å, b = 8.434(4) Å, c = 12.881(4) Å, β = 92.20(4)° N-(2′-bromo-3′,5′-bis(trifluoromethyl)phenyl) maleimide (5), P21/n, a = 8.7115(16) Å, b = 16.125(3) Å, c = 9.6707(19) Å, β = 99.757(15)° N-(2′-phenylphenyl)maleimide (6), P21/n, a = 8.519(4) Å, b = 13.742(5) Å, c = 11.147(4) Å, β = 92.25(3)° N-(4′-methoxyphenyl)maleimide (7), P21/n, a = 9.320(3) Å, b = 6.621(2) Å, c = 16.059(6) Å, β = 99.58(3)° N-(2′-trifluoromethylphenyl)-2-methylmaleimide (8), Fdd2, a = 43.362(12) Å, b = 8.202(2) Å, c = 12.720(4) Å and N-(2′-trifluoromethylphenyl)-2-methanosuccinimide (9), Cc, a = 7.708(2) Å, b = 22.191(9) Å, c = 7.137(2) Å, β = 115.76(2)° are described. Molecules with bulky 2′-substituents show larger rotations between the mean phenyl and maleimide ring planes, and varying degrees of distortion to the imide group.
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  • 51
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    Oxygen Configuration in the Superconductor (Hg0.7Mo0.3)Sr2(Ca1−xRx)Cu2Oz (R = Nd and Pr) (2000)
    Springer
    Journal of superconductivity 13 (2000), S. 111-119 
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    ISSN: 1572-9605
    Keywords: superconductivity ; Hg-based cuprate ; Hg-1212 (Hg,Mo)Sr2(Ca,R)Cu2O z ; neutron diffraction ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Physics
    Notes: Abstract Two series of Hg-based oxides (Hg0.7Mo0.3)Sr2(Ca1−x R x )Cu2O z (R = Nd and Pr, 0.2 ≤ x ≤ 0.7) have been synthesized. Electrical-resistivity measurements show that these compounds are superconductors with maximum onset T c of 107 and 102 K for Nd- and Pr-containing samples, respectively. The neutron powder diffraction experiments on both as-prepared and O2-annealed samples of R = Nd revealed that the O(3) site at the HgOδ sheets are fully occupied and shifted towards the Hg/Mo site to form Mo–O bonds.
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  • 52
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    Evaluation of Kinetic Data for Crystallization of Tio2 Prepared by Hydrolysis Method (2000)
    Springer
    Journal of thermal analysis and calorimetry 60 (2000), S. 595-604 
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    ISSN: 1572-8943
    Keywords: crystal structure ; DSC ; oxides ; X-ray diffraction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The formation of TiO2 prepared by hydrolysis method was presented. Thermodynamics and kinetics of anatase crystallization reaction were investigated. Differential method of kinetic data evaluation in non-isothermal conditions according toKissinger, Ozawa and Kazeev-Yerofeev was applied. Starting, crystallized and thermally treated powders were determined using X-ray powder diffraction analysis. The characteristic parameters (the activation energy, constant rate and formal kinetic order of reaction) of TiO2 formation were calculated using DSC data.
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  • 53
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    Tosyiate of ethyl 3-amino-2-phenyliodoniocrotonate: Synthesis, crystal structure, and synthesis of heterocyclic compounds based on it (2000)
    Springer
    Chemistry of heterocyclic compounds 36 (2000), S. 672-678 
    Details
    ISSN: 1573-8353
    Keywords: aminocrotonate ester ; pyridinium salts ; phenyliodonium salts ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Ethyl 3-aminocrotonate, when reacted with hydroxy(tosyloxy)iodobenzene, forms the tosylate of ethyl 3-amino-2-phenyliodoniocrotonate which crystallizes well in up to 80% yield. X-ray analysis confirms the structure of the phenyliodonium salt, revealing intramolecular and unusual intermolecular hydrogen bonds, stabilizing the compound in the crystalline state. Reaction with pyridine, its 4-substituted derivatives, and 4,4′-bipyridine yields tosylates of 2-pyridinio-substituted ethyl 3-aminocrotonates.1H NMR and IR spectra support formation of an intramolecular hydrogen bond for the E-isomer, and iodonium salts in the case of pyridinium salts for the Z-isomer. The UV spectra of the pyridinium salts show an intramolecular charge transfer band.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02297675
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  • 54
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    Electronic Resource
    Solid-State Supramolecular Chemistry of Porphyrins. Ligand-Bridged Tetraphenylmetalloporphyrin Dimers (2000)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 37 (2000), S. 219-230 
    Details
    ISSN: 1573-1111
    Keywords: porphyrin complexes and clathrates ; coordination oligomers ; supramolecular chemistry ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Eight new crystalline materialsbased on ligand-bridged dimers of either Zn(II)- orCo(II)-tetraphenylporphyrins have been prepared andcharacterized by X-ray diffraction analysis. These supramolecular entities have a ``wheel-and-axle'' typeshape, the elongated bidentate ligands1,3-diaminopropane, 1,4-diaminobutane, 4,4'-bipyridyl, 1,2-bis(4-pyridyl)ethene or1,2-bis(4-pyridyl)ethane coordinating axially on bothsides to the metal centers of the porphyrin species. They vary from one another by the length of the ligandspacer, the distance between the two porphyrincomponents ranging from 9.4 Å to 14.0 Å. Theintermolecular organization in these structures ischaracterized by a similar chain motif in whichadjacent oligomeric units interlock into one another. In spite of the steric constraint imposed by thebridging ligand, this packing preserves the typicalcorrugated stacked arrangement of the porphyrinframeworks which has been commonly observed inclathrates of monomeric tetraarylporphyrins. It alsoinduces in most cases large voids between theinterlocked motifs, causing enclathration of solventmolecules in the crystal lattice. The experimentallyestablished geometries of these oligomers and theircrystal packing modes provide useful information forfurther crystal engineering efforts of polymericmultiporphyrin domains.
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    URL: http://dx.doi.org/10.1023/A:1008118119529
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  • 55
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    Electronic Resource
    Synthesis, Structure, and Superconductivity of (La1.5Pb0.5−xSrx)CuOz (2000)
    Springer
    Journal of superconductivity 13 (2000), S. 121-128 
    Details
    ISSN: 1572-9605
    Keywords: superconductivity ; crystal structure ; magnetization ; 214
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Physics
    Notes: Abstract The substitution of strontium for lead in the material (La1.5Pb0.5−x Sr x )CuO z , x = 0–0.15 has been carried out. A stable and reproducible single phased superconducting materials can be obtained inside an evacuated quartz tube. The X-ray diffraction pattern shows that the superconducting phase can be indexed on the basis of an orthorhombic symmetry (F mmm) for x = 0 and on the basis of tetragonal symmetry (I 4/mmm) for x 〉 0. The transition temperature T c increases as the strontium substitution parameter x increases. We observed the maximal T c around x = 0.15 with 38 K with fairly large Meissner volume fraction of 38% (FC).
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1007790512982
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  • 56
    Electronic Resource
    Electronic Resource
    Octa(p-hydroxy)octakis(propyloxy)calix[8]arene: The First Crystal Structure of a p-Hydroxy Calixarene (2000)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 36 (2000), S. 259-266 
    Details
    ISSN: 1573-1111
    Keywords: calixarene ; hydroquinone derivative ; crystal structure ; hydrogen bonding
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Octa(p-ydroxy)octakis(propyloxy)calix[8]arene.9(pyridine).2(H2O) crystallises in the triclinic space group P-1, a = 14.083(2), b = 14.478(2), c = 15.652(2) Å, α = 70.109(4), β = 74.146(3), γ = 75.572(4)°, V = 2843(1) Å3, Z = 1. Refinement led to a final R1 value of 0.0757 for 4693 reflections. The calixarene sits around a crystallographic centre of inversion and is in the `chair-like' conformation. All p-hydroxyl groups form hydrogen bonds with either pyridine or water molecules leading the extended structure to be composed of infinite ribbons parallel to the [1,0,-1] direction.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1008018628939
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  • 57
    Electronic Resource
    Electronic Resource
    A Bridged High-Spin Complex Bis-[Ni(II)( rac-5,5,7,12,12,14-hexamethyl- 1,4,8,11-tetraazacyclotetradecane)]-2,5-pyridinedicarboxylate Diperchlorate Monohydrate (2000)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 38 (2000), S. 45-56 
    Details
    ISSN: 1573-1111
    Keywords: [Ni(rac-Me6[14]aneN4)] ; 2,5-pyridinedicarboxylate ; preparation ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A bridged high-spin complex,bis-[Ni(II)(rac-5,5,7,l2,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)]-2,5-pyridinedicarboxylate diperchlorate monohydrate has been obtained by reaction of [Ni(II)(rac-5,5,7, 12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)](ClO4)2 and 2,5-pyridinedicarboxylic acid in aqueousalkaline (NH4OH) medium. C39H77Cl2N9Ni2O13, chemical formula weight 1068.42, orthorhombic, P212121, a = 11 .423(3) Å,b = 14.770(6) Å, c = 31.608(7) Å,α = β = γ =90.00°, V = 5333(3) Å3, Z = 4, Dcalc = 1.331 g cm-3, μcalc = 0.869 mm-1, F(000) = 2272, T = 293(2), R = 0.0870 for 2686 observed reflections [I 〉 2σ(I)]. The complexincludes two folded [Ni(rac- Me6[14]aneN4)]2+ units havingopposite diastereomeric configuration. They are bridged through a dianion of2,5-pyridinedicarboxylic acid, with one Ni-atom coordinated to the O-atom ofthe 2-carboxylic group and the pyridine N-atom (forming a 5-membered chelatering), and with the second Ni-atom coordinated to both O-atoms of the 5-carboxylic group (forming a 4-membered chelate ring). Hydrogen bonding involving macrocyclic NH groups, both 2- and 5-carboxylic groups, perchlorate anions and water molecules gives rise to the formation of an infinite supramolecular network in the title compound's crystals.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1008100726771
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  • 58
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    Electronic Resource
    Synthesis, Structure and Spectroscopy of Clathrate Inclusion Compounds of Cobalt(II), Cadmium(II) and Zinc(II) trans-4-styrylpyridine nitrates as Host with trans-4-styrylpyridine as Guest (2 : 1) (2000)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 38 (2000), S. 233-249 
    Details
    ISSN: 1573-1111
    Keywords: trans-4-styrylpyridine complex ; Werner-type clathrates ; crystal structure ; IR spectra ; electronic spectra and thermal analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract New clathrate inclusion compounds with the general formula,MA3X2 β 1/2G (M = Co(II)(1),Cd(II)(2), and Zn(II)(3), X = NO3 - andA and G = trans-4-styrylpyridine), differing from the usualWerner clathrates, MA4X2 β2G, have been prepared and characterized by elemental and thermal analyses,IR and electronic spectroscopy and X-ray crystallography. Tworepresentative compounds [Co(stpy)3(NO3)2] β 1/2stpy (1) and [Cd(stpy)3(NO3)2] β 1/2 stpy (2)are investigated by single crystal X-ray diffraction. Compound (1)crystallizes in the triclinic space group P¯1 with a = 10.966(2),b = 12.802(4), c = 16.063(5) Å α = 83.38(3),β = 71.30(2), γ = 76.88(3) °,Z = 2. The structure is made up of discretemolecules of [Co(stpy)3(NO3)2]. The central Co(II) issurrounded by three stpy nitrogen atoms and four oxygen atoms of twoasymmetrically coordinated bidentate nitrate ligands. One of the oxygensis semicoordinated leading to a distorted octahedral geometry for Co(II).Compound (2) crystallizes in the monoclinic space group P21/nwith a = 15.597(3), b = 18.313(5), c = 16.188(3) Åβ = 115.998(14)° and Z = 4. The structure consists of neutralmolecules of [Cd(stpy)3(NO3)2]. The geometry aroundCd(II) is best described as pentagonal bipyramid with four oxygen atomsfrom symmetrical bidentate nitrate groups and one stpy nitrogen atom inthe equatorial positions. Two other nitrogen atoms from stpy ligands occupythe axial positions. The guest stpy molecules are trapped in the centrosymmetricalcavities in lattices of both 1 and 2. Compound 3is found to beisomorphous with 2. A large splitting of the symmetric and asymmetricNO2 stretching vibrations reveals the presence of bidentate nitrate ligands.Thermogravimetric and DTA studies on the Cd(II) compound, show it to be athermally stable inclusion compound.
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    URL: http://dx.doi.org/10.1023/A:1008137311908
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  • 59
    Electronic Resource
    Electronic Resource
    Crystal Structure of a Calix[4]crown Ether-Ester and Molecular Recognition of Alkyl- and Arylalkylamines (2000)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 36 (2000), S. 461-472 
    Details
    ISSN: 1573-1111
    Keywords: calix[4]arene ; calixcrown ; ether ester ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal and molecular structure of3 has been determined by X-ray analysis. Thecrystal data are: triclinic, space group P'1,a = 12.999(2),b = 14.114(3),c = 16.132(3) Å,α = 91.62(2),β = 97.71(1),γ = 91.38(2)°,V = 2930.6(9) Å3,Z = 2,Dm = 1.046 g cm-3.Rotational disorder has been seen in the t-butyl groups whichwere refined isotropically. Least-squares refinementbased on F2, using 4827 observedreflections with I 〉 2σ(I) and 18 restraints,led to R = 0.123. The calix is found in a coneconformation. The crown ether part of the molecule isnot in a fully extended conformation but has foldsin the chain. The calix[4]crown ether-ester exhibitsmolecular recognition properties toward alkylamines.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1008134703152
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  • 60
    Electronic Resource
    Electronic Resource
    X-ray structure analysis of triacetyllagochilin and lagochilin tetraformate (2000)
    Springer
    Chemistry of natural compounds 36 (2000), S. 181-184 
    Details
    ISSN: 1573-8388
    Keywords: triacetyllagochilin ; lagochilin tetraformate ; crystal structure ; x-ray structure analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The molecular structures of two diterpene lagochilins, triacetyllagochilin and lagochilin tetraformate, are determinated by x-ray structure analysis.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02236426
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  • 61
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    Electronic Resource
    The synthesis and structural analysis of Pt2Ru4(CO)18 and the products obtained from its reactions with 1, 2-bis(diphenylphosphino)ethane (1993)
    Springer
    Journal of cluster science 4 (1993), S. 119-132 
    Details
    ISSN: 1572-8862
    Keywords: Platinum ; ruthenium ; crystal structure ; heteronuclear cluster
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract From the reaction of Ru(CO)5 and Pt(COD)2, COD = 1, 5-cyclooctadiene, the new platinum-ruthenium heteronuclear cluster complex Pt2Ru4(CO)18,1, was obtained in 60% yield.1 has a folded ladder-like structure with alternating pairs of ruthenium atoms and platinum atoms. The cluster of1 can be split to yield the known compound PtRu2(CO)8(η2-dppe),2, (54% yield) by reaction with 1, 2-bis(diphenylphosphino)ethane, dppe, at 25°C. When1 was treated with excess dppe at 40°C, thebis-diphos compound3, PtRu2(CO)6(μ-η2-dppe)2 was obtained (39% yield). Under the similar reaction conditions,2 was converted to3 in 44% yield. All these complexes were characterized by single crystal X-ray diffraction analyses. Compounds2 and3 both contain a triangular cluster of one platinum and two ruthenium atoms, but in2 the bidentate ligand, dppe, chelates the platinum atom and in3 the two dppe ligands bridge the two Pt-Ru metal-metal bonds. Crystal data for1: space group C2/c,a=12.542(2)Å,b=15.350(4)Å,c=15.252(3)Å, β=105.32(2)°,Z=4, 2192 reflections,R=0.025. For2: space group P21/c,a=14.351(2)Å,b=13.486(3)Å,c=19.218(3)Å, β=108.48(1)°,Z=4, 3029 reflections,R=0.027. For3: space group P21/c,a=18.836(6)Å,b=15.559(5)Å,c=23.259(7)Å, β=111.26(2)°,Z=4, 4204 reflections,R=0.038.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00702713
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  • 62
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    Electronic Resource
    Preparation and structural characterization of the hexatungsten cluster complex (EDTEH)2[W6(μ3-Cl)8Cl6], (EDTEH=(MeO2CCH2)2N(H)CH2CH2N(CH2CO2Me)2+ (1993)
    Springer
    Journal of cluster science 4 (1993), S. 271-277 
    Details
    ISSN: 1572-8862
    Keywords: Tungsten ; chloride ; hexatungsten ; 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 hexanuclear tungsten cluster complex [W6(μ3-Cl)8Cl6]2−,1 was isolated as a salt of the cation (MeO2CCH2)2N(H)CH2CH2N(CH2CO2Me)2+, EDTEH+, by crystallization from methanol solvent of the product obtained from the reaction of (H3O)2[W6(μ3-Cl)8Cl3] with the disodium salt of ethylenediaminetetraacetic acid. The compound was charcterized by single-crystal X-ray diffraction analysis. The cluster anion contains an octahedral arrangement of six tungsten atoms with chloride ligands bridging the eight triangular faces of the cluster and one chloride ligand terminally coordinated to each of the six tungsten atoms. The cation (EDTEH)+ achieves its positive charge by protonation of one of the nitrogen atoms. Crystal data: space group = P21/a,a=10.689(2) Å,b=22.931(6) Å,c=12.093(3) Å, β=98.41(2)°,Z=2, 2476 reflections,R=0.028.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00703743
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  • 63
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    Preparation and structural characterization of a hexanuclear molybdenum (II) cluster containing carboxylate ligands (Bu4N)2[Mo6(μ3-Cl)8(O2CMe)6] (1993)
    Springer
    Journal of cluster science 4 (1993), S. 151-157 
    Details
    ISSN: 1572-8862
    Keywords: Molybdenum ; acetate, carboxylate ; hexamolybdenum ; 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 hexamolybdenum cluster complex [Mo6(μ3-Cl)8(O2CMe)6]2−, 1 was isolated as the Bu4N+ salt in 71% yield from the reaction of (Bu4N)2[Mo6(μ3-Cl)8Cl6] with AgO2CMe in CH2Cl2 solvent. The compound was characterized by single crystal X-ray diffraction analysis. The cluster contains an octahedral arrangement of six molybdenum atoms with eight chloride ligands bridging the eight trianglar faces and six carboxylate ligands terminally coordinated through one oxygen atom to each of the six molybdenum atoms. Crystal data: space group =P21/n,a=10.713(3)Å,b=14.43(1)Å,c=21.919(4)Å, β=94.37(2)°,Z=2, 1965 reflections,R=0.036.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00702715
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  • 64
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    Synthesis, characterization and x-ray structure of V3(μ3-O)(μ-Cl)Cl6(μ-η1-η1-PhNHNH2)2(PhNHNH2)2(THF) · 6THF: A new binding mode for phenylhydrazine (1993)
    Springer
    Journal of cluster science 4 (1993), S. 439-451 
    Details
    ISSN: 1572-8862
    Keywords: Vanadium ; phenylhydrazine ; nitrogenase ; 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 Addition of phenylhydrazine to a mixture of VCl3 · THF/N,N-propyl-bis (salicyladimine) and sodium hydride yielded a trinuclear vanadium complex, V3(μ3-O)(μ-Cl)Cl6(μ-η1-η1PhNHNH2)2(PhNHN H2)2(THF), containing two bridging and two terminal phenylhydrazine ligands. The product has been crystallographically characterized (P21/n, a=12.949(2) Å,b=24.061(4) Å,c=22.504(4) Å, β=107.22(1) deg.,V=6697(2) Å3 withZ=4) and was found to contain the first example of bridging monosubstituted hydrazine (phenylhydrazine) ligands.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00703736
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  • 65
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    Electronic Resource
    Effects of higher-order structure of poly(3-hydroxybutyrate) on its biodegradation. II. Effects of crystal structure on microbial degradation (1993)
    Springer
    Journal of polymers and the environment 1 (1993), S. 65-80 
    Details
    ISSN: 1572-8900
    Keywords: Biodegradable plastic ; microbial degradation ; bacterial poly(d-(−)-3-hydroxybutyrate) ; crystal structure ; physiological behavior
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Energy, Environment Protection, Nuclear Power Engineering , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract As one of a series of studies concerning the relationship between the higher-order structure and the biodegradability of a biodegradable plastic, the effects of the crystal structure of the plastic on microbial degradation were investigated. Bacterial poly(d-(−)-3-hydroxybutyrate) (PHB) films which had a wide range of crystallinity were prepared by the melt-quenching method. Results of the microbial degradation indicated that the development of crystallinity evidently depressed the microbial degradability. From scanning electron microscopy (SEM) observations, it is suggested that the microbial degradation proceeded in at least two manners. One was preferential degradation of the amorphous region leaving the crystalline lamellae intact, which was considered to be a homogeneous enzymatic degradation over the surface. The other was nonpreferential spherical degradation on the surface. The SEMs indicate that the spherical holes were the result of colonization by degrading bacteria. The holes varied in size and number with the change of crystal structure. Therefore, it is considered that the crystal structure of PHB also influenced the physiological behavior of the degrading bacteria on the PHB surface.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01457654
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  • 66
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    Analysis of atomic displacement parameters and molecular motion in crystals. Part 2. X-ray crystal structure of K2Ru(SO4)2 * 6H2O at 160 K and 295 K (1993)
    Springer
    Structural chemistry 4 (1993), S. 23-31 
    Details
    ISSN: 1572-9001
    Keywords: Atomic displacement ; molecular motion ; vibrational analysis ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Atomic displacement parameters determined from a single-crystal X-ray-diffraction study on K2Ru(SO4)2 * 6H2O are analyzed in the molecular mean field approximation. The motion of SO2 2− can be described with a rigid-body model, whereas for [Ru(H2O)6]2+ internal stretching motion and coupling between stretching motion and overall translation are found to be necessary for explaining the observed atomic displacement parameters. Frequencies and force constants of internal motion are not significantly affected by such couplings. K2Ru(SO4)2 * 6H2O crystallizes in the monoclinic space groupP21/c (No. 14), witha = 6.1211(7)Å,b = 12.226(2) Å,c = 8.916(2)Å,β = 105.11(1)°,Z = 2 at 160 K anda = 6.1402(7)Å,b = 12.274(2)Å,c = 8.957(1)Å,β = 105.25(1)°,Z = 2 at 295 K. The structure was refined to a finalR(F) of 0.017 at 160 K and of 0.019 at 295 K for 1438 and 1299 observed reflections withF 0 〉 6σ(F0) and sin θ/λ 〉 0.617 Å1−.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00672096
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  • 67
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    Synthesis and structural chemistry of novel heteropolymolybdates and -tungstates (1993)
    Springer
    Molecular engineering 3 (1993), S. 43-59 
    Details
    ISSN: 1572-8951
    Keywords: Heteropolymolybdates ; heteropolytungstates ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The chemistry of polynuclear oxometalate anions is dominated by molybdenum and tungsten in their highest oxidation state. During the past twenty years this class of compounds has attracted much attention because of their variable applications, e.g. as reagents in analytical procedures, as industrial catalysts and as potential anticancer drugs. In order to obtain model systems for the investigation of the catalytic activity of heteropolyanions we have synthesized and structurally characterized some organo derivatives of polyoxoanions. We secondly focus on Sb(III) and Bi(III) heteropolytungstates to examine the important influence of the unshared electron pair on the resulting structures and properties. Some of these compounds may be regarded as supramolecular aggregates showing inclusion phenomena. In 9 two [SbW9O33]9− anions are linked by a set of six sodium ions forming a nearly planar hexagon. The sodium ions are enveloped by an oxygen cage formed by terminal oxygen atoms of the polyanions and by water molecules. Furthermore, the four anions [Sb2W22O74(OH)2]12−, [Sb2W20Fe2O70(H2O)6]8−, [Sb2W20Co2O70(H2O)6]10− and [Bi2W20Fe2O68(OH)2(H2O)6]6− (in10, 11, 12, 13) may be regarded as transition metal complexes of novel [Sb2W20O70]14− or [Bi2W20O70]14− anions which are serving as ligands. The octahedral coordination sphere of each transition metal is formed by three oxygen atoms of the anion and completed by three water molecules. The Sb(III) heteropolyanion, [Na2Sb8W36O132(H2O)4]22− in (14) includes two sodium and four antimony ions besides four water molecules. Each anion consists of four β-B-SbW9-Keggin fragments linked together by four SbO4-groups, incorporating two sodium and four water molecules effecting an additional connection of the subunits.
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    URL: http://dx.doi.org/10.1007/BF00999623
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  • 68
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    Redetermination of the cobaltocene crystal structure at 100 K and 297 K: Comparison with ferrocene and nickelocene (1993)
    Springer
    Structural chemistry 4 (1993), S. 91-101 
    Details
    ISSN: 1572-9001
    Keywords: Cobaltocene ; molecular geometry ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The molecular and crystal structures of the monoclinic modification of cobaltocene Cp2Co (P21/n, Z=2) was determined at 100 K and 297 K with new sets of X-ray diffraction data (MoKα radiation, 3995 and 6534 reflections, refinement toR = 0.026 and 0.030 using 1061 and 1299 independent observable reflections, respectively). At 297 K the structure is disordered (similar to the isomorphous ferrocene and nickelocene) with two distinct orientations of the ring, differing in occupancy factors (80% and 20%) and by a rotation angle in the ring plane of approximately 34°. Just as for nickelocene but in contrast to ferrocene, no sharp phase transition was found on cooling Cp2Co to 100 K, but an essential ordering of the Cp-ring position was detected with a decrease of the contribution of the second minor orientation to nearly 10%. On the basis of a careful analysis of the molecular geometry, crystal packing, and anisotropic atomic displacement parameters, a dynamic temperature-dependent nature of the disorder in Cp2Co is assumed.
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    URL: http://dx.doi.org/10.1007/BF00677370
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  • 69
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    Polar bonds in π-complexes. Preparation and crystal structures of cyclopentadienylcarbonyl iron(II) and ruthenium(II) benzoates andp-fluorobenzoates (1993)
    Springer
    Russian chemical bulletin 42 (1993), S. 359-364 
    Details
    ISSN: 1573-9171
    Keywords: iron(II) and ruthenium(II) complexes ; synthesis ; carbonyl, cyclopentadienyl, benzoate ligands ; crystal structure ; X-ray diffraction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Complexes of Fe(II) and Ru(II) of the general formula Cp(OC)2MOC(O)C6H4X-p, where M=Fe, X=H, F (1, 2) or M=Ru, X=H, F (3, 4) have been prepared by reactingp-XC6H4COOAg with [CpFe(CO)2]2 or CpRu(CO)2I. The crystal structures of complexes1–3 have been determined using X-ray diffraction. Compounds1 and3 are isomorphous. The COO group in1–3 is coordinated as a monodentate ligand. As the latter and the CO ligands are electronically non-equivalent, the coordination of the Cp ligand to the metal is slightly asymmetric.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00697097
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  • 70
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    Electronic Resource
    Crystal and molecular structure of 1-(trimethylsilylmethyl)hexahydroazepine-2-thione and hexahydroazepine-2-thione (1993)
    Springer
    Russian chemical bulletin 42 (1993), S. 181-184 
    Details
    ISSN: 1573-9171
    Keywords: synthesis ; crystal structure ; azepinethiones ; trimethylsilyl derivative
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The title compounds were prepared and X-ray analysis was performed (R = 0.064 and 0.035 for 1309 and 1637 reflections, respectively). In the former the intramolecular S→Si coordination interactions are absent and the Si atom has undistorted tetrahedral coordination with an S...Si distance of 4.034 Å. Crystals of the latter are built of centrosymmetric dimeric H-complexes (S...H(N) 2.58 Å, the S...HN angle 168°).
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00700005
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  • 71
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    Electronic Resource
    Thermal stability and crystal structure of potassium fluoride monoperoxosolvate KF·H2O2 (1993)
    Springer
    Russian chemical bulletin 42 (1993), S. 30-35 
    Details
    ISSN: 1573-9171
    Keywords: peroxosolvates ; potassium fluoride ; monoperoxosolvate ; thermal stability ; crystal structure ; hydrogen bond
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Potassium fluoride peroxosolvate KF-H2O2 was obtained upon action of a 30% aqueous solution of hydrogen peroxide on solid potassium fluoride dihydrate. As compared to other peroxosolvates, KF-H2O2 is characterized by the highest thermal stability: the decomposition rate constantk 1, at 120°C is 1.4 10−3 min−1, the enthalpy of H2O2 addition to KF is 8.1 kcal/ mol. The correlation between the high stability of KF-H2O2 and the absence of catalytic properties of KF towards H2O2, and the formation of strong intermolecular O-H...F and intramolecular O-H...O hydrogen bonds in the crystal is discussed.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00699969
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  • 72
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    Crystal and molecular structure of the (N-Si) chelate of 2-(chlorodimethylsilylmethylthio)-1-pyrroline (1993)
    Springer
    Russian chemical bulletin 42 (1993), S. 173-176 
    Details
    ISSN: 1573-9171
    Keywords: synthesis ; crystal structure ; pentacoordinated silicon ; chelate cycle
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The X-ray diffraction structural study of the (N-Si)-chelate of 2-(chlorodimethyl-silylmethylthio)-1-pyrroline was carried out (R = 0.033 for 1894 reflections). The Si atom has a somewhat distorted trigonal bipyramidal coordination with the Cl and N atoms in axial positions. The Si-Cl and Si-N distances (2.423(1) and 1.945(1) Å) belong, respectively, to the longest and shortest known Si-Cl and Si-N distances in pentacoordinated silicon derivatives with an axial N-Si-Cl moiety.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00700003
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  • 73
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    Electronic Resource
    Structure of the neutral metal complex Pt(dddt)2 (1993)
    Springer
    Russian chemical bulletin 42 (1993), S. 1149-1151 
    Details
    ISSN: 1573-9171
    Keywords: Pt(dddt)2 ; organic conductors ; 5,6-dihydro-1,4-dithiin-2,3-dithiolate((dddt)2−) ; sulfur-containing platinum complexes ; crystal structure ; synthesis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A neutral metal complex, [Pt(dddt)2]° (1), has been obtained by oxidation of the [Pt(dddt)2]− anion with excess (Bu4N)AuBr4 in nitrobenzene. Crystallographic data for 1∶a=17.854(9) Å,b=18.409(9) Å,c=4.717(5) Å, γ=68.83(2)°, space group P21/n,Z=4,d calc=2.55 g/cm3. In1 two independent centrosymmetric [Pt(dddt)2]° molecules are packed in stacks that form layers parallel to the (110) plane. The molecules of1 in the layers have shortened S...S contacts 3.491(9) Å, and 3.594(10) Å. The average bond lengths Pt-S 2.242(7) Å, S-C 1.71(2) Å and C=C 1.40(3) Å, together with the square-planar coordination of Pt in PtS4, suggest considerable conjugation in the metal cycles.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00701993
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  • 74
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    Electronic Resource
    Crystal structure of 4-ethylvanadatrane-1-one (1993)
    Springer
    Russian chemical bulletin 42 (1993), S. 1415-1417 
    Details
    ISSN: 1573-9171
    Keywords: vanadatrane ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract An X-ray diffraction study of a substituted vanadatrane-1-one (space groupPna21,R= 0.019 for 1394 reflections, the absolute structure was determined) showed that the geometry of its atrane framework is similar to that of the Si- and Ge-analogs. The bond lengths are: V=O, 1.614(2) Å; V←N, 2.329(2) Å; V-O, 1.800–1.806(2) Å. The deviation of the V atom having distorted trigonal bipyramidal coordination from the equatorial plane of the O atoms is 0.35 Å, the 0=V←N bond angle is 179.4(1)°.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00699945
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  • 75
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    Crystal and molecular structure of organosilicon titanium(iv) derivatives: (Me3Si)3SiTi(NEt2)3 and ClTi[N(SiMe3)2]3 (1993)
    Springer
    Russian chemical bulletin 42 (1993), S. 1411-1414 
    Details
    ISSN: 1573-9171
    Keywords: titanasilanes ; titanasilazanes ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract An X-ray structural study of two titanium-containing organosilicon compounds, (Me3Si)3SiTi(NEt2)3 (1) and ClTi[N(SiMe3)2]3 (2), has been performed. The conformation of molecule1 in a crystal is staggered (approximate inherentC 3 symmetry), the Ti-Si and Ti-N bond lengths are 2.671(2) and 1.874–1.890(5) Å, respectively. A crystal of1 consists of one type of enantiomers (the space group is P41212; the absolute configuration has been determined). The structure of2 studied previously has been refined to the value of R=0.029 on the basis of 3442 reflections (the absolute structure has been determined), the Ti-Cl and Ti-N bond lengths are 2.260(1) and 1.926(1) Å, respectively. The strong distortions in the symmetry of the valence environment of the N atoms in the molecules of1, 2, and related structures are caused by electronic effects, in which the conformation of the relevant molecular fragments plays a determining role.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00699944
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  • 76
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    Electronic Resource
    Chain folding in single crystals of tetrafluoroethylene copolymers (1993)
    Springer
    Colloid & polymer science 271 (1993), S. 50-55 
    Details
    ISSN: 1435-1536
    Keywords: Polytetrafluoroethylene ; copolymer ; crystal structure ; chain folding
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract Molecular-mechanics calculations are performed on model folds proposed in the literature for single crystals of polytetrafluoroethylene crystallized in the phase stable below 19°C, in order to evaluate how they are modified when a fluorine atom is substituted by a bulky group, as occurs in fluorinated copolymers of tetrafluoroethylene. Only intramolecular effects are taken into account (isolated-chain model). An exhaustive analysis has been carried out of tetrafluoroethylene-hexafluoropropylene copolymer. Moreover, the lower energy folds found for such a copolymer have been examined for copolymers with chlorotrifluoroethylene and perfluoroalkylvinylethers, as comonomers. Our calculations show that all the considered comonomers can be arranged in the model folds proposed for the homopolymer, according to the imposed geometric constraints.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00652302
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  • 77
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    Electronic Resource
    Crystal structure of the complex of human α-thrombin and nonhydrolyzable bifunctional inhibitors, hirutonin - 2 and hirutonin - 6 (1993)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 17 (1993), S. 252-265 
    Details
    ISSN: 0887-3585
    Keywords: thrombin ; bifunctional inhibitor ; crystal structure ; hirutonis ; drugdesing ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The crystal structure of the complexes of hirutonin-2 and hirutonin-6 with human α-thrombin have been solved and refined to R-factors of 0.169 (2.0 Å resolution) and 0.162 (201Å), respectively. Hirutonins belong to a family of bifunctional inhibitors bearing a noncleavable moiety mimicking the scissile bond. Hirutonin-2 is an analog of (D)Phe-Pro-Arg-Gly-hirudin49-65; hirutonin-6 has the same N-terminal tripeptide connected to a shortened fibrinogen exosite-binding part by a short, non-peptidyl linker. The hirutonin-6 molecule is well defined in the electron density with the exception of the C-terminal Leu-h61. The linker follows near the bottom of the canyon connecting the active site with the exosite, forms a short antiparallel β-sheet-like arrangement with Leu-40-Leu41 and makes van der Waals contacts with Glu39-Leu40-Leu41 of thrombin. In the thrombin-hirutonin-2 complex, the N- and C-terminal parts of the inhibitor are well or dered (except the C-terminal Gln-h65) while the central portion of the linker is partially disordered. The glycine analog in the P1′ position of hirutonin-2 assumes a conformation similar to that of the canonical form (Bode and Huber (1992) Eur. J. Biochem. 204 : 433-451) and supports the identification of the S1′ site as restricted by His57, Trp60D, Lys60F, and the Cys42-Cys58 disulfide bridge. The carbonyl oxygen of the P1 arginine residue is located in the oxyanion hole formed by the NH groups of Gly193 and Ser195, while the carbonyl carbon is positioned within a short distance, 2.8 Å, from the Oγ of Ser195. This resembles the conformation of the substrate-like inhibitors bound to other serine proteases. The N-terminal (D)Phe-pro-Arg fragment common to both inhibitors binds to thrombin in a fashion very similar to that of other inhibitors having this motif. The binding of the C-terminus of hirutonins to the fibrinogen-binding exosite is similar to that observed in hirudin and hirulog complexes. © 1993 Wiley-Liss, Inc.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prot.340170304
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  • 78
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    Electronic Resource
    Calcium-independent subtilisin by design (1993)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 16 (1993), S. 205-213 
    Details
    ISSN: 0887-3585
    Keywords: calcium binding ; crystal structure ; protein stability ; site-directed mutagenesis ; subtilisin ; X-ray crystallography ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: A version of subtilisin BPN′ lacking the high affinity calcium site (site A) has been produced through genetic engineering methods, and its crystal structure refined at 1.8 Å resolution. This protein and the corresponding version containing the calcium A site are describedand compared. The deletion of residues 75-83 was made in the context of four site-specific replacements previously shown to stabilize subtilisin. The helix that in wild type is interrupted by the calcium binding loop, is continuous in the deletion mutant, with normal geometry. A few residues adjacent to the loop, principally those that were involved in calcium coordination, are repositioned and/or destabilized by the deletion. Because refolding is greatly facilitated by the absence of the Caloop, this proteinoffers a new vehicle for analysis and dissection of the folding reaction. This is among the largest internal changes to a protein to be described at atomic resolution. © Wiley-Liss, Inc.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prot.340160207
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  • 79
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    Electronic Resource
    Twelve-membered crown ethers: Crystal structures of benzo-12-crown-4 and naphtho-12-crown-4 (1993)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 15 (1993), S. 79-89 
    Details
    ISSN: 1573-1111
    Keywords: 12-membered crown ethers ; crystal structure ; conformation peculiarities ; X-ray analysis ; CH...O contacts
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structures of two 12-membered crown ethers, benzo-12-crown-4 (1) and naphtho-12-crown-4 (2), have been determined by X-ray analysis. Both structures are molecular. Compound1 is monoclonic,P21/b,a=8.466(3),b=8.019(3),c=33.590(10) Å, γ=90.99(3)o. The unit cell contains two crystallographically independent molecules of1 with similar conformations. Compound2 is also monoclinic,P21/a,a=24.148(8),b=14.535(4),c=7.987(5) Å, γ=102.87(2)o. Two independent molecules in the unit cell have significantly different conformations.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00706476
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  • 80
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    Crystal structure of the complex of dibenzo-30-crown-10 with dysprosium isothiocyanate (1993)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 15 (1993), S. 159-165 
    Details
    ISSN: 1573-1111
    Keywords: Dibenzo-30-crown-10 ; crystal structure ; complexation ; dysprosium isothiocyanate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Crystalline [Dy(NCS)3(dibenzo-30-crown-10)(H2O)2]·H2O·MeCN can be obtained by slowly evaporating a reaction mixture of Dy(NCS)3·nH2O with dibenzo-30-crown-10 in a solution of acetonitrile. The material crystallizes in the monoclinic space groupP21/n, the cell parameters area=11.450(5),b=23.284(4),c=18.424(6)Å, β=106.28(4)°,V=4715Å3,M=968.47,D x=1.36 g cm−1, μ=17.80 cm−1,F(000)=1972,Z=4.2740 independently observed [I≥3σI] reflections were used in the final least-squares refinement leading to an agreement index ofR=0.085. The Dy(III) ion coordination geometry approximates a square antiprism, involving two water oxygens and three dibenzo-30-crown-10 oxygen atoms and three isthiocyanate nitrogens. Hydrogen bonds are formed between the two water molecules and four uncoordinated crown ether oxygen atoms.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00710225
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  • 81
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    Structural study of the 1:1 clathrate of an asymmetric calix[4]arene and acetone (1993)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 15 (1993), S. 341-349 
    Details
    ISSN: 1573-1111
    Keywords: Molecular asymmetry ; calixarene ; acetone ; clathrate ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal and molecular structure of the 1:1 clathrate of the asymmetric calix[4]arene,1, and acetone has been determined by X-ray analysis. The crystal data are: tetragonal, space groupP4/n,a=b=12.574(6),c=12.572(6) Å,V=1988(2) Å3,Z=2,D x =1.111 g cm−3,D m =1.108 g cm−3. Least-squares refinement based on 1131 observed reflections withF 0〉3σ(F 0) and anisotropic temperature factors led toR=0.096. In spite of the molecular asymmetric calixarene1 the crystal structure has high symmetry, because a part of the host and guest molecules are in disordered states.
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    URL: http://dx.doi.org/10.1007/BF00708751
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  • 82
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    Helical tubulate inclusion compounds of ferrocene and squalene (1993)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 15 (1993), S. 385-398 
    Details
    ISSN: 1573-1111
    Keywords: Hydrogen bonding ; alicyclic diol ; helical tubulate ; crystal structure ; ferrocene ; squalene
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The inclusion compounds of 2,8-dimethyltricyclo[5.3.1.13,9]dodecane-syn-2,syn-8-diol,3, with ferrocene and with squalene have been prepared. The crystal structures of these helical tubulate compounds: (3)3·(ferrocene)0.75 [P3121,a=b=13.7480(6),c=7.0312(5) Å,Z=1,R=0.038] and (3)3·(squalene)0.23 [P3121,a=b=13.677(1),c=7.0533(9) Å,Z=1,R=0.042] are described.
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    URL: http://dx.doi.org/10.1007/BF00708755
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  • 83
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    Studies on werner clathrates. Part 131. Selective criteria in werner clathrates. Six crystal structures with bis(isothiocyanato)tetra(4-vinylpyridine)nickel(II) as host (1993)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 16 (1993), S. 25-54 
    Details
    ISSN: 1573-1111
    Keywords: Werner clathrate ; nickel octahedral complex ; tetrahydrofuran ; crystal structure ; NMR ; molecular recognition ; hydrocarbon
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract This paper addresses the general question: what are the significant guest properties selected by this host when interacting with guest molecules in the liquid phase, resulting in cocrystallization of the host and guest? In particular, to what extent do π electrons in a guest molecule effect its potential as a guest? Werner clathrates of the host [Ni(NCS)2(4-ViPy)4] with mixtures of tetrahydrofuran (THF) and cyclic hydrocarbons as guests have been synthesised and their structures elucidated. Clathrate (1): [Ni(NCS)2(4-ViPy)4](1.78 THF)(0.22 cyclohexane), crystallizes in the orthorhombic space groupP bcn a=9.976(6),b=20.630(25),c=19.861 (4) Å,V=4087Å3,Z=4,R=0.087 for 1461 reflections; (2): [Ni(NCS)2(4-ViPy)4](1.76 THF)(0.24 cyclohexene),P bcn ,a=9.987(7),b=20.614(4),c=19.898(4)Å,V=4096Å3,Z=4,R=0.084 for 1304 reflections; (3): [Ni(NCS)2(4-ViPy)4](0.48 THF)(0.52 1,3-cyclohexadiene), tetragonalI41/a,a=16.898(3),b=16.898(3),c=26.463(6)Å,V=7556Å3,Z=8,R=0.120 for 1698 reflections; (4): [Ni(NCS)2(4-ViPy)4](0.36 THF)(1.04 1,4-cyclohexadiene),I41/a,a=16.986(4),b=16.986(4),c=25.896(15)Å,V=7472Å3,Z=8,R=0.103 for 2025 reflections; (5): [Ni(NCS)2(4-ViPy)4](0.35 THF)(1.05 benzene),I41/a,a=17.102(10),b=17.102(10),c=25.498(8)Å,V=7458Å3,Z=8,R=0.118 for 2200 reflections; (6): [Ni(NCS)2(4-ViPy)4](3 benzene), triclinicP1,a=10.432(24),b=11.155(9),c=21.581(7)Å, α=78.70(5), β=82.60(7), γ=74.09(13)°,V=2361Å3,Z=2,R=0.078 for 3427 reflections. Host-guest ratios and, for mixtures of guests, guest1/guest2 ratios, were elucidated by density and NMR. We show that the conformational freedom of the substituted pyridines is not the primary reason for the clathrating ability of Werner hosts. All six structures show no host-guest interaction at the level of van der Waals interactions. As non-bonding interactions are not observed between the host and guest, this study shows that the above host's selectivity by enclathration of particular guest molecules cannot be accounted for by solid state structural analysis.
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    URL: http://dx.doi.org/10.1007/BF00708760
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  • 84
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    Host-guest chemistry. 2. Amine inclusion compounds of 2-[o-(triphenylphosphoranylidenamino)benzyliden]amino-1H-2,3-dihydroindazol-3-one. X-ray structure of its 1∶1∶1 inclusion complex with isopropylamine and water (1993)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 16 (1993), S. 155-168 
    Details
    ISSN: 1573-1111
    Keywords: Iminophosphoranes ; amine inclusion compounds ; 13C CPMAS NMR spectroscopy ; salt-like crystalline aggregates ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal and molecular structure is reported for the inclusion compound 2-[o-(triphenylphosphoranylidenamino)benzyliden]amino-1H-2,3-dihydroindazol-3-one/isopropylamine/water3b. The crystal structure consists of discrete dimeric salt-like aggregates joined together by strong N+−H...−O−C hydrogen bonds between pairs of centrosymmetrically-related indazolonate anions and isopropylammonium cations. Six other inclusion compounds have been prepared and characterized by NMR [with propylamine (3a), withtert-butylamine (3c), withsec-butylamine (3d), withtert-pentylamine (3e), with 1-methylbutylamine (3f) and withiso-pentylamine (3g)]. Two different arrangements are found, both with the host being in the anionic form. The guests are either: (i) one protonated amine and one water molecule (3b and3f); or (ii) one protonated amine and the corresponding neutral amine (3a, 3c, 3d, 3e and3g).
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00709149
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  • 85
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    Crystal structure of [Yb (NO3)3 (phen) (H2O)] · (12-crown-4) (1993)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 16 (1993), S. 267-272 
    Details
    ISSN: 1573-1111
    Keywords: Crown ether ; ytterbium nitrate ; phen ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The title complex was prepared by reacting Yb(NO3)3 (12-crown-4) with 1,10-phenanthroline (hereafter phen) in acetone. It crystallized in the triclinic space group $$P\bar 1$$ witha=10.095(5),b=17.415(4),c=8.710(2) Å α=92.45(2), β=115.83(3), γ=74.08(3)0 andD c=1.85 g cm−3;Z=2. The metal ion in this complex is nine-coordinated to three bidentate nitrate ions, two nitrogen atoms of a phen and a water molecule. The crown ligand is hydrogen bonded to the coordination water molecule. The symmetry change of the crown ether is also discussed.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00708796
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  • 86
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    Study of structure and polymerization of epitaxially grown SiPc(OH)2 thin films by high-resolution electron microscopy (1993)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 31 (1993), S. 1713-1723 
    Details
    ISSN: 0887-6266
    Keywords: phthalocyanine siloxane ; crystal structure ; epitaxial growth ; high-resolution electron microscopy ; molecular imaging ; polymerization ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Thin films of SiPc(OH)2 (Pc = phthalocyanine) were formed epitaxially on the (001) surface of mica by vacuum deposition and were then polymerized by heat treatment. The molecular packing of the SiPc(OH)2 was determined by electron diffraction and high-resolution electron microscopy as triclinic\documentclass{article}\pagestyle{empty}\begin{document}${\rm P\bar 1} $\end{document} having dimensions a = 0.727, b = 1.307, c = 0.688 nm, α = 102.5, β = 104.2, and γ = 97.4°. This monomer crystal grows with its c-axis parallel to the a-axis of the substrate mica and its bc-plane parallel to the (001) surface of mica. By heat treatment at 320°C, the SiPc(OH)2 polymerized with the c-axis of the polymer parallel to the c-axis of the monomer. At 420°C, the c-axis of the polymer became parallel to the a*-axis of the monomer (i.e., perpendicular to the film surface). From high-resolution electron microscopy of partially polymerized specimens, the polymerization was shown to start at the edges of small monomer crystals. This may be considered to be due to the volume expansion during the polymerization. © 1993 John Wiley & Sons, Inc.
    Additional Material: 16 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/polb.1993.090311207
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  • 87
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    poly(4,4′-oxybibenzoate): Polymerization, morphology, transitions, and crystal structures (1993)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 31 (1993), S. 1923-1940 
    Details
    ISSN: 0887-6266
    Keywords: poly(4,4′-oxybibenzoate) ; polymerization ; morphology ; transitions ; crystal structure ; disclination domains ; Iamellae ; single crystals ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: 4-Acetoxy 4′-carboxy biphenyl has been polymerized from solution, the bulk melt, and in constrained thin films, all below the melting point of the monomer as measured by differential scanning calorimetry (DSC). An isothermal sublimation-recrystallization-melting (and chemical change)-polymerization-crystallization process is proposed. From solution and in the thin films, single crystals consisting of ca. 100 Å thick lamellae are observed, with evidence for monomer addition-reaction on the end (top and bottom) surfaces. The bulk samples are fibrous, the “fibers” consisting of whisker-like single crystals. The polymer is highly heat and radiation (electron beam) resistant, with numerous successive electron diffraction (ED) patterns from the same crystal or sheared sample permitting comparison of the changes in ED patterns with transitions seen by DSC at ca. 350, 530, and 590°C. Phase I (a = 7.8, b = 5.5, c = 10.8 Å), a possible phase II (a = 15.6, b = 3.6 Å c = unknown), and a phase III (a = 9.0, b = 5.2 = √3a, c = 10.8 Å). Phases I and II are seen in samples polymerized at temperatures at and below 310°C; phase III is observed in samples polymerized at and above 350°C and in sheared samples. © 1993 John Wiley & Sons, Inc.
    Additional Material: 18 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/polb.1993.090311305
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  • 88
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    Liquid crystalline main chain polymers with a poly(p-phenyleneterephthalate) backbone. 2. Fiber spinning and mechanical properties of polyesters with alkoxy side chains (1993)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 31 (1993), S. 1759-1767 
    Details
    ISSN: 0887-6266
    Keywords: rigid rod polymer ; thermotropic ; aromatic polyester ; fiber ; modulus ; crystal structure ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Fiber spinning and mechanical properties of four rigid polyesters with alkoxy substituents of different length and placement were evaluated. Properties of oriented fibers from the polymer with dodecyloxy substituents on the terephthalate moiety, PTA12HQ, were significantly affected by the crystal modification. At room temperature the following properties (tensile modulus E, tensile strength σb, and strain at break εb) could be obtained: E = 9.5 GPa, σb = 85 MPa and εb = 1.1% for phase Lf (the “frozen in layered mesophase”); E = 10.4 GPa, σb = 59 MPa and εb = 0.6% for modification A; E = 17.3 GPa, σb = 158 MPa and εb = 1.2% for modification B. Because of the higher amount of main chains per cross sectional area the polymer with hexyloxy side chains, PTA6HQ, showed better properties at a comparable degree of molecular orientation: E = 24 GPa, σb = 270 MPa, εb = 1.4%. Fibers obtained from the polyester with dodecyloxy substituents on the hydroquinone moiety, PTAHQ12, were too brittle to handle. The polyester with dodecyloxy substituents on both moieties, PTA12HQ12, was spun from the isotropic melt. Because of the obtained low degree of orientation, properties (E = 1 GPa, σb = 40 MPa, and εb = 6.3%) were governed by interactions between the chains (the main chains are not load-bearing). © 1993 John Wiley & Sons, Inc.
    Additional Material: 15 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/polb.1993.090311209
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  • 89
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    Neubestimmung von Struktur und Eigenschaften isotyper Natriumtetraamidometallate des Aluminiums und Galliums (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 381-386 
    Details
    ISSN: 0044-2313
    Keywords: Sodium tetraamido aluminate ; sodium tetraamido gallate ; crystal structure ; IR spectra ; thermal behaviour ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Redetermination of Structure and Properties of the Isotypic Sodium Tetraamido Metallates of Aluminium and GalliumCrystals for x-ray structure determination of NaAl(NH2)4 and NaGa(NH2)4 were obtained by the reaction of the metals with ammonia in autoclaves at 100°C and P(NH3) = 60 bar within 7 days. The compounds crystallize isotypic in the space group P21/c with Z = 4 NaAl(NH2)4 a = 7.328(2) Å, b = 6.047(2) Å, c = 13.151(3) Å, β = 94.04(1)° NaGa(NH2)4 a = 7.4087(8) Å, b = 6.0917(5) Å, c = 12.855(2) Å, β = 92.10(1)°The structures were refined inclusively all H-positions of the amide ions. The ternay amides are furthermore characterized by their IR spectra and their thermal behaviour.
    Notes: Für röntgenographische Strukturbestimmungen geeignete Kristalle von NaAl(NH2)4 und NaGa(NH2)4 wurden durch Umsetzung der Metalle mit NH3 in Autoklaven bei 100°C und P(NH3) = 60 bar in 7d erhalten. Die Verbindungen kristallisieren isotyp in der Raumgruppe P21/c mit Z = 4 NaAl(NH2)4 a = 7,328(2) Å, b = 6,047(2) Å, c = 13,151(3) Å, β = 94,04(1)° NaGa(NH2)4 a = 7,4087(8) Å, b = 6,0917(5) Å, c = 12,855(2) Å, β = 92,10(1)°Die Strukturen wurden einschließlich aller H-Lagen der NH2--Ionen bestimmt. Die ternären Amide werden außerdem IR-spektroskopisch und bezüglich ihres thermischen Verhaltens charakterisiert.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190224
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  • 90
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    Über eine neu entdeckte Dimorphie an BaCoEr2O5 (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 421-423 
    Details
    ISSN: 0044-2313
    Keywords: Barium, cobalt, erbium, oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On a New Observed Dimorphism of BaCoEr2O5Single crystals of BaCoEr2O5 were prepared by CO2-LASER technique under N2-atmosphere and investigated by X-ray single crystal methods. It crystallizes with orthorhombic symmetry, space group D2h16-Pnma (a = 12.2787, b = 5.6826, c = 7.0344 Å; Z = 4). The so far unknown crystal structure of BaCoEr2O5 belongs to the BaCuLn2O5 type forming the dimorphic substance to the previously described Ni type of BaCoEr2O5.
    Notes: BaCoEr2O5 wurde mit CO2-LASER-Technik in Stickstoffatmosphäre einkristallin dargestellt und röntgenographisch untersucht. Es kristallisiert orthorhombisch, Raumgruppe D2h16-Pnma, mit den Gitterkonstanten a = 12,2787, b = 5,6826, c = 7,0344 Å; Z = 4. Die hier untersuchten Einkristalle von BaCoEr2O5 gehören zum BaCuLn2O5-Typ und bilden die dimorphe Form zum früher beschrieben Ni - Typ von BaCoEr2O5.
    Additional Material: 3 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190230
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  • 91
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    Zur Kenntnis der Dialkalimetalldichalkogenide β-Na2S2, K2S2, α-Rb2S2, β-Rb2S2, K2Se2, Rb2Se2, α-K2Te2, β-K2Te2 und Rb2Te2 (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 476-488 
    Details
    ISSN: 0044-2313
    Keywords: Dialkali metal dichalcogenides ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Dialkali Metal Dichalcogenides β-Na2S2, K2S2, α-Rb2S2, β-Rb2S2, K2Se2, Rb2Se2, α-K2Te2, β-K2Te2 and Rb2Te2The first presentation of pure samples of α- and β-Rb2S2, α- and β-K2Te2, and Rb2Te2 is described. Using single crystals of K2S2 and K2Se2, received by ammonothermal synthesis, the structure of the Na2O2 type and by using single crystals of β-Na2S2 and β-K2Te2 the Li2O2 type structure will be refined. By combined investigations with temperature-dependent Guinier-, neutron diffraction-, thermal analysis, and Raman-spectroscopy the nature of the monotropic phase transition from the Na2O2 type to the Li2O2 type will be explained by means of the examples α-/β-Na2S2 and α-/β-K2Te2. A further case of dimorphic condition as well as the monotropic phase transition of α- and β-Rb2S2 is presented. The existing areas of the structure fields of the dialkali metal dichalcogenides are limited by the model of the polar covalence.
    Notes: Die erstmalige Darstellung phasenreiner Proben von α- und β-Rb2S2, von α- und β-K2Te2 und von Rb2Te2 wird beschrieben. Mit Hilfe von ammonothermal synthetisierten Einkristallen des K2S2 und des K2Se2 wird die Struktur des Na2O2-Typs, mit Einkristallen des β-Na2S2 und des β-K2Te2 die des Li2O2-Typs verfeinert. Durch kombinierte temperaturabhängige Guinier-, Neutronenbeugungs-, thermoanalytische und Raman-spektroskopische Untersuchungen wird die Natur des monotropen Phasenübergangs vom Na2O2-Typ zum Li2O2-Typ an Hand der Beispiele α-/β-Na2S2 und α-/β-K2Te2 aufgeklärt. Ein weiterer Fall von Dimorphie, der ebenfalls monotrope Übergang von α-Rb2S2(Rb2O2-Typ) zu β-Rb2S2(Na2O2-Typ), wird vorgestellt. Die Existenzgebiete der Strukturfelder bei den Dialkalimentalldichalkogeniden werden mittels des Modells der polaren Kovalenz gegeneinander abgegrenzt.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190309
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  • 92
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    Synthese und Kristallstruktur von CaBiVO5 (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 521-524 
    Details
    ISSN: 0044-2313
    Keywords: Calcium ; bismuth ; vanadium ; oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of CaBiVO5Single crystals of the hitherto unknown compound CaBiVO5 were prepared and investigated by X-ray work. It crystallizes with orthorhombic symmetry, space group D2h15—Pbca, a = 11.2022, b = 5.4283, c = 15.5605 Å, Z = 8. The crystal structure is characterized by layers of the edge-linked CaO7 polyhedra, isolated VO4 tetrahedra and an asymmetric surrounding of Bi3+ by oxygen.
    Notes: Die bisher unbekannte Verbindung CaBiVO5 wurde einkristallin dargestellt und röntgenographisch untersucht. Sie kristallisiert orthorhombisch in der Raumgruppe D2h15-Pbca mit a = 11,2022, b =5,4283, c = 15,5605 Å, Z = 8. Die Kristallstruktur ist durch Schichten aus CaO7-Polyedern, isolierte VO4-Tetraeder und asymmetrisch koordinierte Bi3+-Ionen charakterisiert.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190315
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  • 93
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    Zwei neue Verbindungen mit Zink in tetragonal pyramidaler Koordination: BaZnDy2O5 und Ba1,25ZnHo2O5,25 (Ba5Zn4Ho8O21) (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 529-533 
    Details
    ISSN: 0044-2313
    Keywords: Barium-zinc-rare earth metal-oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Compounds with Zinc in Square Pyramidal Coordination: BaZnDy2O5 and Ba1.25ZnHo2O5.25 (Ba5Zn4Ho8O21).Single crystals of (I): BaZnDy2O5 and (II): Ba5Zn4Ho8O21 were prepared by high temperature reactions and investigated by X-ray technique. (I) belongs to the BaCuLn2O5 type, space group D2h16-Pbnm; a = 7.084; b = 12.368; c = 5.728 Å, Z = 4. (II) is isotypic to Ba5Mn4Ln8O21, space group C4h5-I4/m; a = 13.779; c = 5.707 Å, Z = 2. The two different structure types are caused by the small difference in the composition of 0.25 BaO. Analogies and differences will be discussed. In addition the lattice constants of powder samples of Ba5Zn4Ln8O21 (Ln = Eu, Gd, Dy, Ho, Er and Y) are given.
    Notes: Mit Hochtemperaturreaktionen wurden Einkristalle von (I): BaZnDy2O5 und (II): Ba5Zn4Ho8O21 dargestellt und röntgenographisch untersucht. (I) gehört zum BaCuLn2O5-Typ, Raumgruppe D2h16-Pbnm mit a = 7,084; b = 12,368; c = 5,728 Å, Z = 4. (II) ist isotyp zum Ba5Mn4Ln8O21-Typ, Raumgruppe C4h5-I4/m, mit a = 13,779; c = 5,707 Å, Z = 2. Der geringe Unterschied von 0,25 BaO führt zu zwei verschiedenen Strukturtypen. Gemeinsamkeiten und Unterschiede werden diskutiert. Weitere Verbindungen vom Typ Ba5Zn4Ln8O21 mit Ln = Eu, Gd, Dy, Ho, Er und Y wurden mikrokristallin dargestellt und die Gitterkonstanten bestimmt.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190317
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  • 94
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    Zur Kristallchemie von Ba3In2Zn5O11. Ein tOxoindat/zinkatsol;zinkat mit Zn10O20- und In4O16-Makropolyedern und erstmals O2- in tetraedrischer Koordination durch Zn2+ (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 559-562 
    Details
    ISSN: 0044-2313
    Keywords: Barium ; indium ; zinc ; oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Crystal Structure of Ba3In2Zn5O11. An Oxoindate/zincatesol;zincate with Zn10O20 and In4O16 Macropolyhedra with Zn2+ in Tetrahedral Coordination by O2-Ba3In2Zn5O11 was prepared for the first time by a flux technique and investigated by single crystal X-ray work. It crystallizes with cubic symmetry, space group T2d-F43m, a = 13.3588 Å, Z = 8. Zn2+ show tetrahedral coordination by O2-, forming Zn10O20 macropolyhedra. In addition the nZn/Osol;O part of the crystal structure is made up of Zn10O20 parts. Edge connection of four InO6 octahedra results in In4O16 groups. The crystal structure will be shown and discussed.
    Notes: Mit einer Schmelzmitteltechnik wurde erstmals Ba3In2Zn5O11 dargestellt und an Einkristallen röntgenographisch untersucht. Es kristallisiert kubisch, in der Raumgruppe T2d-F43m, mit a = 13,3588 Å und Z = 8. Zn2+ ist tetraedrisch von O2- koordiniert und bildet Zn10O20-Makropolyeder. Ferner wird der nZn/Osol;O-Teil der Kristallstruktur aus Zn10O20-Bausteinen zusammen-gesetzt. Die oktaedrisch koordinierten In3+-Ionen verknüpfen über Kanten zu In4O16-Baugruppen. Die Kristallstruktur wird vorgestellt und diskutiert.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190322
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  • 95
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    Darstellung und Kristallstruktur eines Kalium - Magnesium-Oxocuprat/-vanadats: KMg2Cu2V3O12 (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 617-620 
    Details
    ISSN: 0044-2313
    Keywords: Potassium ; magnesium ; copper ; vanadium ; oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of Potassium Magnesium Oxocuprate/-vanadate: KMg2Cu2V3O12.Single crystals of KMg2Cu2V3O12 were prepared by solid state reactions below the melting point of the reaction mixture (K2CO3, MgCO3, CuO, V2O5). It crystallizes with monoclinic symmetry space group C2h6—C2/c, a = 12.1592 Å, b = 12.7204 Å, c = 6.8557 Å, β = 111.73°, Z = 4. The structure type is characterized by VO4 tetrahedra, twisted CuO4 square units, MgO6 octahedra and a special 2 + 4 + 2 coordination around the potassium ion.
    Notes: Einkristalle von KMg2Cu2V3O12 wurden durch Feststoffreaktionen, dicht unterhalb des Schmelzpunktes des Reaktionsgemenges (K2CO3, MgCO3, CuO, V2O5), erhalten. Die Verbindung kristallisiert mit monokliner Symmetrie, Raumgruppe C2h6—C2/c, a = 12,1592 Å, b = 12,7204 Å, c = 6,8557 Å, β = 111,73°, Z = 4. Die Kristallstruktur ist durch VO4-Tetraeder, tordierte CuO4-Baugruppen, MgO6-Oktaeder und Kalium, in einer besonderen 2 + 4 + 2 Koordination charakterisiert.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190402
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  • 96
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    Crystallochemistry of some new niobium bromides with (Nb6Br18) units: Structures of CsErNb6Br18 and Cs2EuNb6Br18Dedicated to Professor Harald Schäfer in memoriam (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 621-627 
    Details
    ISSN: 0044-2313
    Keywords: Niobum bromides ; (Nb6Br18) units ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kristallchemie einiger neuer Niobbromide mit (Nb6Br18)-Einheiten: Die Strukturen von CsErNb6Br18 und Cs2EuNb6Br18.Zwei neue Reihen von Nb6-Bromiden, CsSENb6Br18 (SE = alle Lanthanoide außer Eu und Yb, + Y) (Typ H) und M2SENb6Br18 (M = Cs, Rb, Tl; SE = Eu, Yb) (Typ R) sind dargestellt worden. Die Kristallstrukturen von CsErNb6Br18 und Cs2EuNb6Br18, isotyp mit den entsprechenden Chloriden, wurden durch Einkristall-Röntgendaten bestimmt. Die Stabilität der (Nb6Br18)-Einheit hängt von der Art und der Ladung des Gegenkations ab. Ein Vergleich zwischen den entsprechenden Reihen der Chloride und Bromide wird anhand der chemischen Eigenschaften und der Größe des Halogens diskutiert.
    Notes: Two new series of Nb6 bromides, CsRENb6Br18 (RE = all the lanthanides excepted Eu and Yb, + Y) (type H) and M2RENb6Br18 (M = Cs, Rb, Tl; RE = Eu, Yb) (type R) have been isolated. The crystal structures of CsErNb6Br18 and Cs2EuNb6Br18, isotypic with the corresponding chlorides, have been determined by single crystal X-ray diffraction data. The (Nb6Br18) intra-unit strength is related to the nature and the charge of the counter cation. A comparison between the corresponding chlorides and bromides series, based on the chemical properties and the size of the halogen is discussed.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190403
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  • 97
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    Ein neues Syntheseverfahren für Vanadiumbronzen. Die Kristallstruktur von β—Ag0,33V2O5. Verfeinerung der Kristallstruktur von ∊—Cu0,76V2O5Professor Hartmut Bärnighausen zum 60. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 287-292 
    Details
    ISSN: 0044-2313
    Keywords: Silver vanadium bronze ; copper vanadium bronze ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Novel Means of Synthesis for Vanadium Bronzes. Crystal Structure of β—Ag0.33V2O5. Refinement of the Crystal Structure of ∊—Cu0.76V2O5Ag0.33V2O5 and Cu0.76V2O5 were obtained by heating equimolar mixtures of AgI + V2O5 (700°C) and CuI + V2O5 (525°C), respectively, in sealed quartz glass ampoules. In each case, one of the well-formed crystals served for an X-ray structure analysis. Ag0.33V2O5 has the structure known of the β phase of the vanadium bronzes, i. e. layers of edge-sharing, distorted VO6 octahedra are liked by certain common octahedron vertices, the Ag atoms randomly occupy two positions with occupation probabilities of 0.5. Cu0.76V2O5 has the previously determined structure of the ∊ phase, however, its space group is not Cm but C2/m.
    Notes: Ag0,33V2O2 und Cu0,76V2O5 wurden durch zweiwöchiges Erhitzen von äquimolaren Gemischen AgI + V2O5 (700°C) bzw. CuI + V2O (525°C) in einer Quarzglasampulle erhalten. Mit je einem der gut ausgebildeten Kristalle wurden eine Röntgenstrukturanalyse durchgeführt. Ag0,33V2O5 hat die für die β-Phase der Vanadiumbronzen bekannte Struktur, d. h. Schichten aus verzerrten, kantenverknüpften VO6-Oktaedern sind über bestimmte Oktaederecken verknüpft, die Ag-Atome nehmen statistisch zwei Atomlagen der Koordinationszahl 7 mit halber Besetzungswahrscheinlichkeit ein. Cu0,76V2O5 hat die früher bereits bestimmte Struktur der ∊-Phase, deren Raumgruppe jedoch nicht Cm sondern C2/m ist.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190211
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  • 98
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    Verbesserte Darstellung, Kristallzüchtung und Strukturanalyse von P4O6S2 und P4O6S3Professor Hartmut Bärninghausen zum 60. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 281-286 
    Details
    ISSN: 0044-2313
    Keywords: Tetraphosphorus hexaoxide disulfide and trisulfide ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Improved Syntheses, Crystal Growth, and Crystal Structure Determination of P4O6S2 and P4O6S3Syntheses and single crystal growths of the title compounds are described. Both compounds crystallize in the space group P21/c (P4O6S2: a = 11.293(4); b = 6.457(3); c = 11.588(4) Å; β = 90.29(2)°, 2 450 diffractometer data, Rw = 0.035/P4O6S3: a = 15.611(5); b = 8,303(3); c = 9.697(4) Å; β = 127.12(2)°, 2 481 diffractometer data, Rw = 0.034). The structural data for the series P4O6Sn (n = 1 - 4) thus completed are compared to their oxide analogues P4O6On (n = 1 - 4). The changes in the geometry of the P4O6-cage in course of its successive oxidation are discussed.
    Notes: Darstellung und Einkristallzucht der Titelverbindungen werden beschrieben. Beide Verbindungen kristallisieren in der Raumgruppe P21/c (P4O6S2: a = 11,293(4); b = 6,457(3); c = 11,588(4) Å; β = 90,29(2)°, 2 450 Diffraktometerdaten, Rw = 0,035/P4O6S3: a = 15,611(5); b = 8,303(3); c = 9.697(4) Å; β = 127,12(2)°, 2 481 Diffraktometerdaten, Rw = 0,034). Durch die neu gelösten Strukturen werden die Daten für das System P4O6Sn (n = 1 - 4) komplettiert und können mit denen der analog aufgebauten Oxide P4O6On (n = 1 - 4) verglichen werden. Die Veränderungen der Molekülgeometrie des zentralen P4O6-Käfigs im Zuge der schrittweisen Oxidation werden diskutiert.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190210
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  • 99
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    Li5B7S13 und Li9B19S33: Zwei Lithiumthioborate mit neuen hochpolymeren AnionengerüstenProfessor Hartmut Bärnighausen zum 60. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 293-302 
    Details
    ISSN: 0044-2313
    Keywords: Lithium thioborates ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Li5B7S13 and Li9B19S33: Two Lithium Thioborates with Novel Highly Polymeric Anion NetworksLi5B7S13 (C2/c; a = 17.304(2) Å, b = 21.922(3) Å, c = 12.233(2) Å, β = 134.91(1)°; Z = 8) and Li9B19S33 (C2/c; a = 23.669(9) Å, b = 14.361(3) Å, c = 12.237(3) Å, β = 103.77(2)°; Z = 4) were prepared by reaction of stoichiometric amounts of lithium sulfide, boron, and sulfur at 750°C (Li5B7S13) and 700°C (Li9B19S33) with subsequent annealing. The crystal structures consist of interpenetrating, polymeric boron sulfur anion networks which are formed by corner-sharing of B4S10 and B10S20 units (Li5B7S13), or B19S36 units (Li9B19S33). The lithium cations are situated in between with a strong disorder in Li9B19S33.
    Notes: Li5B7S13 (C2/c; a = 17,304(2) Å, b = 21,922(3) Å, c = 12,233(2) Å, β = 134,91(1)°; Z = 8 und Li9B19S33 (C2/c; a = 23,669(9) Å, b = 14,361(3) Å, c = 12,237(3) Å, β = 103,77(2)°; Z = 4 wurden durch Reaktion von stöchiometrischen Mengen Lithiumsulfid, Bor und Schwefel bei 750°C (Li5B7S13) und 700°C (Li9B19S33) mit anschließendem Tempern dargestellt. Die Kristallstrukturen bestehen aus sich durchdringenden, polymeren Bor-Schwefel-Anionengerüsten, die durch Eckenverknüpfung von B4S10- und B10S20-Einheiten (Li5B7S13) bzw. B19S36-Einheiten (Li9B19S33) gebildet werden. Dazwischen befinden sich die Lithiumkationen, wobei bei Li9B19S33 eine starke Fehlordnung beobachtet wird.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190212
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  • 100
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    Über Neue Oxoruthenate vom Typ der 6 L-Perowskite: Ba3SrRu2-xTaxO9 (x = 0,8 und 1,4) mit einem Beitrag über Ba3CaRu2O9 (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 517-520 
    Details
    ISSN: 0044-2313
    Keywords: Alkaline Earth ; ruthenium ; oxygen ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Novel Oxoruthenates of the 6 L-Perovskite Type: Ba3SrRu2-xTaxO9 (x = 0.8 and 1.4) with a Comment on Ba3CaRu2O9Single crystals of the phases Ba3SrRu2-xTaxO9 [(I): x = 0.8 and (II): x = 1.4] and the compound (III): Ba3CaRu2O9 were prepared by a BaCl2 flux and investigated by X-ray methods. (I)-(III) crystallizes with hexagonal symmetry space group P62c with lattice constants: (I) a = 6.003 Å; c = 15.227 Å; (II) a = 5.988 Å; c = 15.220 Å and (III) a = 5.891 Å; c = 14.571 Å. The crystal structures of these substances corresponds to the 6 layer perovskites with the stacking sequence (hcc)2. All of them show a so far not described slightly distorted oxygen framework caused by the Sr2+ and Ca2+ ions.
    Notes: Einkristalle der Phasen Ba2SrRu2-xTaxO9 [(I): x = 0,8 und (II): x = 1,4] sowie der Verbindung (III): Ba3CaRu2O9 wurden in einer BaCl2-Schmelze präpariert und mit Hilfe von Röntgenbeugungsmethoden untersucht. (I)-(III) kristallisieren in der hexagonalen Raumgruppe P62c mit den Gitterkonstanten: (I) a = 6,003 Å; c = 15,227 Å; (II) a = 5,988 Å; c = 15,220 Å und (III) a = 5,891 Å; c = 14,571 Å. Ihre Kristallstrukturen entsprechen den 6 L-Perowskiten mit der Stapelsequenz (hcc)2. Sie zeigen eine bislang noch nicht beschriebene leichte Verzerrung im Aufbau der Sauerstoffteilgitter, die auf die Sr2+ - bzw. Ca2+-Ionen zurückgeführt werden kann.
    Additional Material: 3 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190314
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