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  • crystal structure  (60)
  • Springer  (60)
  • American Meteorological Society
  • MDPI Publishing
  • Nature Publishing Group
  • 2010-2014
  • 2000-2004  (60)
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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Journal of chemical crystallography 30 (2000), S. 7-10 
    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).
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  • 2
    ISSN: 1572-8854
    Keywords: iron ; crystal structure ; synthesis ; N-methylimidazole
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The compound [Fe(C4H6N2)6][C5H4NSO3]2 crystallized in the monoclinic space group, P21/n with unit cell parameters: a = 13.676(3), b = 8.345(2), c = 18.663(4) Å, β = 106.40(3)° and Z = 2. The title compound consists of a [Fe(C4H6N2)6]+2 hexacoordinated iron(II) cation and two C5H4NSO− 3 anions. In the cation the iron atom is coordinated to six N-methylimidazole imine nitrogen atoms in a distorted octahedral arrangement. The N1,N5,N1i,N5i atoms are coplanar and the iron lies in this plane.
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  • 3
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    Springer
    Journal of chemical crystallography 30 (2000), S. 35-38 
    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.
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  • 4
    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.
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  • 5
    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.
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  • 6
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    Journal of chemical crystallography 30 (2000), S. 53-53 
    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.
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  • 7
    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.
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  • 8
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    Journal of chemical crystallography 30 (2000), S. 767-771 
    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.
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  • 9
    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.
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  • 10
    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.
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  • 11
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    Journal of chemical crystallography 30 (2000), S. 589-592 
    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.
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  • 12
    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.
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  • 13
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    Journal of cluster science 11 (2000), S. 39-53 
    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.
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  • 14
    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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  • 15
    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.
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  • 16
    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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  • 17
    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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  • 18
    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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  • 19
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    Journal of chemical crystallography 30 (2000), S. 483-487 
    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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  • 20
    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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  • 21
    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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  • 22
    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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  • 23
    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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  • 24
    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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  • 25
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    Journal of chemical crystallography 30 (2000), S. 633-639 
    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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  • 26
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    Journal of chemical crystallography 30 (2000), S. 777-782 
    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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  • 27
    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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  • 28
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    Journal of chemical crystallography 30 (2000), S. 805-809 
    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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  • 29
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    Journal of chemical crystallography 30 (2000), S. 181-184 
    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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  • 30
    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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  • 31
    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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  • 32
    ISSN: 1572-8854
    Keywords: phosphine ; nickel(II) complexes ; crystal structure
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    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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    Journal of chemical crystallography 30 (2000), S. 671-675 
    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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  • 34
    ISSN: 1572-8854
    Keywords: mixed metal diphosphates ; AI 2BII 3(P2O7)2 ; crystal structure
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    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
    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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  • 36
    ISSN: 1572-8854
    Keywords: macrocycle ; hydroxyethyl pendant ; crystal structure ; hydrogen bonds
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    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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    Journal of chemical crystallography 30 (2000), S. 799-804 
    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
    ISSN: 1572-8854
    Keywords: copper ; bis(benzimidazoles) ; crystal structure ; infrared
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    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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    Journal of chemical crystallography 30 (2000), S. 95-98 
    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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    Journal of chemical crystallography 30 (2000), S. 115-118 
    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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    Journal of chemical crystallography 30 (2000), S. 119-122 
    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
    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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    Journal of chemical crystallography 30 (2000), S. 131-134 
    ISSN: 1572-8854
    Keywords: 1,2,4-Oxadiazole ; crystal structure ; phthalimide derivative ; AM1 method ; STO-3G basis set
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    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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    Journal of chemical crystallography 30 (2000), S. 135-138 
    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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    Journal of chemical crystallography 30 (2000), S. 159-162 
    ISSN: 1572-8854
    Keywords: crystal structure ; cobalt (II) complex ; one-dimensional chain ; hydrogen bond
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    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
    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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    Journal of chemical crystallography 30 (2000), S. 329-333 
    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
    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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    Journal of chemical crystallography 30 (2000), S. 455-458 
    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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    Journal of chemical crystallography 30 (2000), S. 563-571 
    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
    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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    Journal of thermal analysis and calorimetry 60 (2000), S. 595-604 
    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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    Chemistry of heterocyclic compounds 36 (2000), S. 672-678 
    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.
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  • 54
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    Journal of inclusion phenomena and macrocyclic chemistry 37 (2000), S. 219-230 
    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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  • 55
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    Journal of superconductivity 13 (2000), S. 121-128 
    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).
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  • 56
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    Journal of inclusion phenomena and macrocyclic chemistry 36 (2000), S. 259-266 
    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.
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  • 57
    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.
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  • 58
    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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  • 59
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    Journal of inclusion phenomena and macrocyclic chemistry 36 (2000), S. 461-472 
    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.
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  • 60
    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.
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