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  • 1
    Digitale Medien
    Digitale Medien
    Synthesis, crystal structure, and molecular modeling (AM1) of Methyl 6-chloro-4-(2-chlorophenyl)-5-formyl-2-methyl-1, 4-dihydropyridine-3-carboxylate (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 237-243 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Crystal structure ; AM1 ; x-ray diffraction ; dihydropiridines
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The synthesis and structural characterization of Methyl 6-chloro-4-(2-chlorophenyl)-5-formyl-2-methyl-1,4-dihydropyridine-3-carboxylate is described. The structure was refined to R1 = 0.0470 for 2665 reflections (with I 〉 2σ(I)). Crystal data: C15H13C12NO3, monoclinic,space group P21/c, a = 11.163(9), b = 14.484(8), c = 9.422(7) Å, V = 1512.9(19) Å3, Z = 4. The results of crystallographic and molecular modeling (AM1) were compared. The Cl atom attached to the phenyl group has two possible orientations, having 75% (sp) and 25% (ap) occupancy, respectively. The molecules in the crystal are held together by means of intermolecular hydrogen bonds of the type N=H...O and by C=H...O interactions.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009539005669
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  • 2
    Digitale Medien
    Digitale Medien
    Synthesis and crystal structure of a tetranuclear manganese(IV) cluster [L4Mn4O6](ClO4)4·2H2O (L = 1,4,7-triazacyclononane) (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 251-254 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Crystal structure ; manganese(IV) cluster ; adamantane-shaped complex ; tetranuclear complex
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract A tetranuclear manganese (IV) complex, [L4Mn4O6](ClO4)4·2H2O (1), with 1,4,7-triazacyclononane (L) as the capping ligands, has been synthesized and characterized by X-ray diffraction; monoclinic, space group P21/n with a = 21.335(6) Å, b = 11.387(3) Å, c = 21.788 (6) Å, β = 111.410 (6)°, V = 4928 (2) Å, Z = 4. Each manganese atom has a distorted octahedral environment comprised of three facially coordinated amine nitrogen atoms and three oxygen atoms, and the cation is an idealized tetrahedron. The Mn4O6 4+ cation corresponds to an adamantane skeleton.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009543106577
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  • 3
    Digitale Medien
    Digitale Medien
    Synthesis and crystal structure of 4,4′-bis(4-pyridylethyl)biphenyl, noncovalently hydrogen bonded two-dimensional networks (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 641-646 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Crystal structure ; hydrogen bonds ; 1H and 13C NMR ; FTIR
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract A new pyridine containing compound, 4,4′-bis(4-pyridylethyl)biphenyl 1, was synthesized and its structure was determined by X-ray crystallography. Two kinds of two-dimensional networks linked by hydrogen bonds were obtained with different crystal solvents: 1·2H2O, monoclinic, space group P21/n with a = 8.3280(10), b = 5.5990(10), c = 24.054(4) Å, β = 98.79(2)°, V = 1108.4(3) Å3, Z = 2, Dc = 1.200 g cm−3, R1 = 0.0558; 1·CH3OH·2H2O, triclinic, space group P-1 with a = 8.3310(10), b = 12.861(2), c = 13.111(2) Å, α = 64.110(10), β = 75.000(10), γ = 83.750(10)°, V = 1220.7(3) Å3, Z = 2, Dc = 1.177 g cm−3, R1 = 0.0529. It is interesting that in the hydrate the host molecule of 1 contains an essentially flat biphenyl section, while in the methanol complex the host molecule of 1 contains a substantial twist in the center of the biphenyl section. The compounds were also characterized by NMR and FTIR spectroscopies. The 1H and 13C NMR assignments for 1 were carried out by 2D NMR spectral measurements in acetonitrile-d 3.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1011944115181
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  • 4
    Digitale Medien
    Digitale Medien
    X-ray crystal structures of [HB(3,4,5-Me3pz)3[2Zn, [H2B(3,4,5-Me3pz)2]Zn(μ-3,4,5-Me3pz)2Zn[H2B(3,4,5-Me3pz)2], and [H2B(pz)2]2Zn (pz = pyrazolyl ring) (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 665-670 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Crystal structure ; poly(pyrazolyl)borate ligands ; zinc(II)
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract [HB(3,4,5-Me3pz)3]2Zn (1) and [H2B(3,4,5-Me3pz)2]Zn(μ-3,4,5-Me3pz)2Zn[H2B(3,4,5-Me3pz)2] (2) are present in equal amounts in a crystal in the triclinic space group, P-1 with a = 11.5924(11) Å, b = 12.7799(12) Å, c = 15.7317(14) Å α = 107.905(2)° β = 96.796(2)°, γ = 105.786(2)°, and Z = 1. The structure of 1 is a trigonally distorted octahedron and is very similar to the structure of [HB(3,5-Me2pz)3]2Zn showing that the introduction of the third methyl group on the pyrazolyl ring does not impact on structure. [H2B(pz)2]2Zn (3) is orthorhombic, Pca2(1) with a = 10.1473(3) Å, b = 11.1117(2) Å, c = 14.1831(5) Å, α = β = γ = 90° and Z = 4. The zinc(II) centers in both 2 and 3 are similar and have pseudotetrahedral structures.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1011900300160
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  • 5
    Digitale Medien
    Digitale Medien
    Structure and properties of cobalt(II) complex with a tetraaza macrocycle containing 2-pyridylmethyl pendant arms (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 335-338 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Crystal structure ; cobalt(II) complex ; tetraaza macrocycle ; 2-pyridylmethyl pendant arms
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The complex [Co(L)]Cl2·10H2O (1) (L = 2,13,-bis(2-pyridylmethyl)-3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,01.18,07.12]docosane) has been synthesized and structurally characterized. Compound 1 crystallizes in the triclinic system, space group P-1 with a = 9.731(2) Å, b = 9.789(2) Å, c = 11.998(1) Å, α = 66.66(1)°, β = 76.95(1)°, γ = 87.99(2)°, V = 1020.4(3) Å3, and Z = 1. The crystal structure of 1 shows that the complex is centrosymmetric and the cobalt(II) ion has a slightly distorted octahedral geometry with four nitrogen atoms of the macrocycle and two nitrogen atoms of the pendent arms at the axial positions. Cyclic voltammetry for 1 undergoes reversible one-electron oxidation to the Co(III) and irreversible one-electron reduction to the Co(I).
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009513308611
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  • 6
    Digitale Medien
    Digitale Medien
    Crystal structure of 2,3-dihydronaphto[2,3-b) [1,5] dioxepin (2000)
    Springer
    Journal of chemical crystallography 30 (2000), S. 459-462 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Crystal structure ; chemical synthesis ; 2,3-dihydronaphto[2,3-b] [1,5) dioxepin
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The X-ray single crystal structure of C13H12O2 compound was determined. It crystallizes in the orthorombic space group P212121 with a = 7.8847(7), b = 9.639(1), c = 13.432(2) Å, Z = 4 and V = 1020.8(3) Å3. The final R converged to 0.037 for 1763 independent reflexions. The title compound forms layers parallel to (1 0 0) planes and the three dimensional cohesion of the crystal is assumed by Van der Waals interactions. The molecule consists of two six-membered rings (A and B) and a seven-membered ring (C). A and B rings are planar, whereas the C ring has a chair conformation
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1011399416154
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  • 7
    Digitale Medien
    Digitale Medien
    Crystallographic relations between Ti3SiC2 and TiC (2000)
    Springer
    Materials research innovations 3 (2000), S. 286-291 
    Details
    ISSN: 1433-075X
    Schlagwort(e): Key words Titanium silicon carbide ; Titanium carbide ; Crystal structure ; InterfaceRID=""ID=""〈E6〉Acknowledgements 〈/E6〉This work was supported by the National Outstanding Young Scientist Foundation under Grant No. 59925208, National Science Foundation of China under Grant No. 59772021, and the ”863” program.RID=""ID=""〈E5〉Correspondence to:〈/E5〉Y. Zhou
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Maschinenbau
    Notizen: Abstract Ti3SiC2 is a so-called not-so-brittle ceramic that combines the merits of both metals and ceramics. However, many previous works demonstrated that its bonding nature and properties were strongly related to TiC. In this paper the crystallographic relations between Ti3SiC2 and TiC were established and described based on the transmission electron microscopy investigation on the Ti3SiC2/TiC interface in Ti3SiC2 based material. At Ti3SiC2/TiC interface, the following crystallographic relationships were identified: (111)TiC//(001)Ti3SiC2, (002) TiC//(104)Ti3SiC2, and [11¯0]TiC//[110]Ti3SiC2. Based on the above interfacial relations an interfacial structure model was established. The structure of Ti3SiC2 could be considered as two-dimensional closed packed layers of Si periodically intercalated into the (111) twin boundary of TiC0.67 (Ti3C2). The intercalation resulted in the transformation from cubic TiC0.67 to hexagonal Ti3SiC2. In the opposite case, de-intercalation of Si from Ti3SiC2 caused the transformation from hexagonal Ti3SiC2 to cubic TiC0.67. Understanding the crystallographic relations between Ti3SiC2 and TiC is of vital importance in both understanding the properties and optimizing the processing route for preparing pure Ti3SiC2.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/PL00010876
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  • 8
    Digitale Medien
    Digitale Medien
    Chemical preparation, thermal behavior and crystal structure of ammonium barium cyclotriphosphate dihydrate (2000)
    Springer
    Materials research innovations 3 (2000), S. 352-359 
    Details
    ISSN: 1433-075X
    Schlagwort(e): Keywords Chemical preparation ; Thermal behavior ; Crystal structure ; Cyclotriphosphate ; Long-chain polyphosphate ; Dehydration ; Calcination ; Infrared spectrometry ; Thermal analyses (TGA-DTA) ; X-ray diffraction
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Maschinenbau
    Notizen: Abstract  Ammonium and barium cyclotriphosphate mo-nohydrate, BaNH4P3O9·1H2O, was prepared for the first time by using Boullé’s process [1] by Durif et al. [2] who reported a complete description of the atomic arrangement. BaNH4P3O9·1H2O is monoclinic P21/n with the following unit-cell dimensions: a=11.70(1)Å, b=12.12(1)Å, c=7.559(5)Å, β=101.05(5) and Z=4. There-fore, some discrepancies appear in the literature and stimulated further investigation of this compound to conclude concerning hydration level and structure. The thermal behavior of BaNH4P3O9·nH2O [3] showed that this cyclotriphosphate is a dihydrate and up to now no other hydrate has been described for this salt. So, the present study reports the chemical preparation, thermal behavior and crystal structure of BaNH4P3O9·2H2O, the first cyclotriphosphate of mixed ammonium-bivalent cations MII with a new general formula MIINH4P3O9·nH2O. Dehydration and decomposition of such cyclotriphosphates lead generally to long-chain polyphosphates, [MII(PO3)2]∞ which can be used as corrosion inhibitors [4]. The title compound has been studied through the following techniques: X-ray diffraction, IR spectrometry and thermal analyses TGA-DTA coupled.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/s100190000057
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  • 9
    Digitale Medien
    Digitale Medien
    Compression of witherite to 8 GPa and the crystal structure of BaCO3II (2000)
    Springer
    Physics and chemistry of minerals 27 (2000), S. 467-473 
    Details
    ISSN: 1432-2021
    Schlagwort(e): Key words Witherite ; High pressure ; Aragonite ; Crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie , Geologie und Paläontologie , Physik
    Notizen: Abstract Natural witherite (Ba0.99Sr0.01CO3) has been studied by single-crystal X-ray diffraction in the diamond anvil cell at eight pressures up to 8 GPa. At ambient pressure, cell dimensions are a = 5.3164(12) Å, b = 8.8921(19) Å, c = 6.4279(16) Å, and the structure was refined in space group Pmcn to R(F) = 0.020 from 2972 intensity data. The unit cell and atom position parameters for the orthorhombic cell were refined at pressures of 1.2, 2.0, 2.9, 3.9, 4.6, 5.5, 6.2, and 7.0 GPa. The volume-pressure data are used to calculate equation of state parameters K T0 = 50.4(12) GPa and K′ = 1.9(4). At approximately 7.2 GPa, a first-order transformation to space group P3¯1c was observed. Cell dimensions of the high-pressure phase at 7.2 GPa are a = 5.258(6) Å, c = 5.64(1) Å. The high pressure structure was determined and refined to R(F) = 0.06 using 83 intensity data, of which 15 were unique. This high-pressure phase appears to be more compressible than the orthorhombic phase with an estimated initial bulk modulus (K 7.2GPa) of 10 GPa.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/s002690000087
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  • 10
    Digitale Medien
    Digitale Medien
    The Effect of Al Implantation on the Thermal Oxidation of Stainless Steel in Aggressive Environments (2000)
    Springer
    Oxidation of metals 53 (2000), S. 303-323 
    Details
    ISSN: 1573-4889
    Schlagwort(e): ion implantation ; oxidation ; thermal ; stainless steel ; ion-beam analysis ; aluminum
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Maschinenbau
    Notizen: Abstract AISI-321 steel samples were implanted with Al ions (implantation-energy:40 keV; dose: 2×1017 ions/cm2). Thermal oxidationof the samples was performed at 450, 550, 600, and 650°C for periodsvarying from 1 to 6 days in air and in a corrosive CO2-containingenvironment. Nuclear Reaction Analysis (NRA) and Rutherford BackscatteringSpectrometry (RBS) were used to investigate the oxidized samples. Asignificant improvement of the oxidation resistance of the implantedmaterial in comparison to the nonimplanted material was observed. Thisespecially applies for samples oxidized at high temperatures. The aluminumdepth distribution determined by NRA [using the resonance at 992 keV of the27Al(p, γ )28Si nuclear reaction] and RBS,indicated no variation of the Al profile in the temperature region450–600°C, whereas at 650°C a slight Al diffusion wasobserved. Scanning electron microscopy (SEM–EDS) was applied to studythe surface morphology and the constitution of the oxide scale formed, aswell as to explain the influence of Al implantation on the oxidation behaviorof AISI-321 austenitic stainless steel.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1004541220830
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