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  • 1
    Electronic Resource
    Electronic Resource
    Problems in the low-temperature synthesis of 92K Superconducting YBCO (1994)
    Springer
    Il nuovo cimento della Società Italiana di Fisica 16 (1994), S. 1671-1678 
    Details
    ISSN: 0392-6737
    Keywords: Effects of material synthesis ; crystal structure ; chemical composition ; Y-based compounds ; Conference proceedings
    Source: Springer Online Journal Archives 1860-2000
    Topics: Physics
    Notes: Summary YBCO with high granulometric perfection and low dispersion can be obtained by a low-temperature reaction (≈800°C) of atomic-scale dispersed powders, produced through the thermal decomposition of liquid precursors. As reacted such powders are tetragonal and not superconducting, but they transform into the high-T c phase after optimized annealing treatments. We describe the method we developed and the characteristics of the materials we achieved, and we discuss the main features of the process in the light of the current know-how.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02462158
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  • 2
    Electronic Resource
    Electronic Resource
    Structure of TiO2 in TiO2-SiO2 prepared by a complexing agent-assisted sol-gel procedure (1994)
    Springer
    Journal of sol gel science and technology 1 (1994), S. 113-121 
    Details
    ISSN: 1573-4846
    Keywords: crystal structure ; complexing agent ; TiO2 ; TiO2-SiO2
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Many types of TiO2-SiO2 (Ti:Si=50:50 mol%) were prepared by the sol-gel procedure with and without 2-methyl-2, 4-pentanediol (MPD) as an organic ligand. The effect of MPD on the gel structure and the properties of the TiO2 crystals were studied by XRD and raman spectroscopy, and the effect of the sol standing time on the properties of the TiO2 crystals were also studied by XRD spectroscopy. In the gels with MPD, anatase of TiO2 appeared at approximately 580°C, and the crystal structures were similar despite the difference in the gel preparation procedure. The titania gels with MPD were presumed to be dispersed in the silica gel matrix without any Ti-O-Si bond. In the presence of MPD, the formation of titania gels is controlled and the specified TiO2 crystal is produced.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00490241
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  • 3
    Electronic Resource
    Electronic Resource
    A structural two-ring version of a tubular stack ofβ-rings in crystals of a cyclic D,L-hexapeptide (1994)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 18 (1994), S. 27-36 
    Details
    ISSN: 1573-1111
    Keywords: D,L-hexapeptide ; cyclic ; crystal structure ; stacks ; tubular ; β-rings ; channels
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract An X-ray analysis of single crystals (from MeOH) of cyclo(-D-Leu-L-MeLeu-D-Leu-L-MeLeu-D-Leu-L-MeLeu-) has been carried out. The analysis reveals that the molecules of the cyclopeptide occur in the crystals with two slightly different, almost hexagonal backbone conformations of the β-type, and that pairs of molecules with the same conformation interact through their nonmethylated face, forming dimeric units (units A and B) with six interannular H-bonds. This kind of pairing reproduces well that expected for a two-ring element in a stack of antiparalleβ-rings. The X-ray analysis has also revealed the presence in the A units of two water molecules, each at one of two equivalent sites located on the 3-fold axis of the units and equidistant from the center of gravity, and the presence in the B units of one water molecule at the center of the units. This provides experimental support for the idea that stacks ofβ-rings can serve as molecular channels.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00706936
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  • 4
    Electronic Resource
    Electronic Resource
    N(nPr)4[B5O6(OH)4][B(OH)3]2 and N(nBu)4[B5O6(OH)4][B(OH)3]2: Clathrates with a diamondoid arrangement of hydrogen-bonded pentaborate anions (1994)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 18 (1994), S. 161-175 
    Details
    ISSN: 1573-1111
    Keywords: Pentaborate ; boric acid ; clathrate ; diamond-related network ; hydrogen bonding ; tetrapropy-lammonium ; tetrabutylammonium ; crystal structure ; 11B MAS NMR ; 13C MAS NMR ; thermogravimetry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Single-crystal X-ray structure analyses of N(nPr)4[B5O6(OH)4][B(OH)3]2,1, and N(nBu)4 [B5O6(OH)4][B(OH)3]2,2, reveal that these materials are novel clathrates, the isotypic host structures of which are three-dimensional assemblies of hydrogen-bonded [B5O6(OH)4]− ionsand B(OH)3 molecules. The assembly of only the pentaborate anions is a distorted (i.e., along [102] elongated) fourconnected diamond-related network. The N(nPr) 4 + and N(nBu) 4 + ions are trapped within the complex three-dimensional channel systems of the host frameworks. Both1 and2 crystallize monoclinically with space groupP21/c andZ=4. The cell constants are:1:a=13.592(5),b=12.082(2),c=17.355(6) Å, β=106.60(2)° (298K);2:a=13.874(3),b=12.585(1),c=17.588(4) Å, β=107.04(1)° (238 K). The results obtained by both11B and13C MAS NMR spectroscopy are discussed. Thermogravimetric studies under a flowing inert-gas atmosphere suggest that water, stemming from polycondensation of the hydrous borate species, is released from the clathrates at ca. 443 K (1) and 398 K (2) before the decomposition of the organic cations starts at ca. 603 K (1) and 603 K (2).
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00705819
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  • 5
    Electronic Resource
    Electronic Resource
    12-Membered crown ethers. Lipophilic derivatives of benzo- and naphtho-12-crown-4 and their membrane electrode properties. Crystal structures of benzo-12-crown-4 NaI and KI complexes (1994)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 20 (1994), S. 335-351 
    Details
    ISSN: 1573-1111
    Keywords: 12-Membered crown ethers ; ion-selective membrane electrodes ; complexes ; crystal structure ; X-ray analysis ; conformation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Lipophilic derivatives of benzo-12-crown-4 and naphtho-12-crown-4 have been synthesized. The behavior of the parent compounds and their derivatives in membrane ion-selective electrodes have been studied. Selectivity changes have been observed with the rise in lipophilicity. Crystal structures of the NaI and KI complexes of benzo-12-crown-4 (1 and2) have been determined by X-ray analysis. The alkali metal and iodide ions are in direct contact in2 but not in1. Compound1 [Na(benzo-12-crown-4)2]·I is triclinic, witha=13.368(8),b=10.727(7),c=10.325(4) Å; α=73.56(4),β=77.73(4), γ=108.70(5)°;Z=2, space group is $$P\bar 1$$ . Compound2 [K(benzo-12-crown-4)2·I] is monoclinic, witha=15.807(8),b=12.043(4),c=15.601(6) Å,β=117.74(3)°;Z=4, space groupC2/c. In both compounds the cations interact with all oxygen atoms of two crown ether molecules. Correlation of the crystal structures and behavior of the crown ethers in ion-selective membrane electrodes is discussed.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00708878
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  • 6
    Electronic Resource
    Electronic Resource
    Inclusion complexes of the natural product gossypol. Recognition by gossypol of halogeno methanes. Structure of the dichloromethane complex of gossypol and single crystal conservation after decomposition (1994)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 17 (1994), S. 317-324 
    Details
    ISSN: 1573-1111
    Keywords: Gossypol ; complex ; crystal structure ; single crystal ; desolvation ; polymorph
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The structures of gossypol complexes are extremely sensitive to the halogenomethane present as the guest; e.g. changing the number of Cl atoms in chloromethane derivatives changes the structure of the gossypol complex. The crystals of C30H30O8·CH2Cl2 are monoclinic, space groupC2/c,a=21.320(4),b=19.199(6),c=15.765(2)Å, β=113.05(2)o,V=5916(2)Å3,Z=8,D x=1.35 g/cm3,T=295 K. The structure has been solved by direct methods and refined to the finalR value of 0.084 for 1828 reflections. In the structure H-bonded gossypol molecules form columns, generating channels in the structure which are filled by guest molecules. After decomposition (desolvation) monocrystals of the complexes are conserved without destruction, in which there are rather wide and empty channels though slightly smaller than in the complex. An attempt is made to explain some peculiarities of the behavior of the gossypol polymorph formed on the basis of its structure with empty channels.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00707127
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  • 7
    Electronic Resource
    Electronic Resource
    Crystal structure of the product of a condensation reaction of (±)-gossypol with (R)-(+)-1-phenylethylamine. Why do diastereoisomeric diaminogossypols cocrystallize? (1994)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 17 (1994), S. 365-376 
    Details
    ISSN: 1573-1111
    Keywords: Gossypol ; inclusion compounds ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structure of a compound obtained in a condensation reaction of (±)-gossypol with (R)-(+)-phenylethylamine has been determined by X-ray structure analysis. The crystals of C46H48O6N2·(C4H8O2)2 are monoclinic, space groupP21,a=21.243(3),b=8.666(1),c=28.651(4) Å, β=108.24(1)0,V=5009(3) β3,Z=4,D x=1.195 g cm−3, μ(CuK α)=0.66 mm−1,T=292 K. The structure has been solved by direct methods and refined to the finalR value of 0.091 for 4290 observed reflections and 1049 parameters. There are two diastereoisomeric molecules of the host and four solvent molecules in the asymmetric unit. The host molecules are H-bonded into chains with diastereoisomeric molecules alternating along the chain. The fact that the host prefers the association mode in which molecules with a different configuration of the 2,2′-binaphthyl moiety are H-bonded explains why separation of diastereoisomeric diaminogossypols by fractional crystallization has been unsuccessful. The 1,4-dioxane molecules are accommodated in infinite channels but only every second guest molecule in a channel is H-bonded to the host.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00707132
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  • 8
    Electronic Resource
    Electronic Resource
    X-ray crystallographic studies of tricarbonylchromium complexes of calix[4]arene conformers: On an unusual conformation which appears in cone conformers (1994)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 19 (1994), S. 227-236 
    Details
    ISSN: 1573-1111
    Keywords: Calixarenes ; arenetricarbonylchromium ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The structures of three arene-tricarbonylchromium complexes prepared from cone and 1,3-alternate-25, 26,27,28-tetrapropoxycalix[4]arene(1) and Cr(CO)6 were determined by single crystal X-ray studies. Crystal data for 1,3-alternate-1·Cr(CO)3 are space groupP21/a,a=19.496(3)Å,b=11.118(2)Å,c=19.121(2)Å, β=109.95°(1) andV=3895Å3. The structure was refined toRw=0.068. Crystal data for cone-1·Cr(CO)3 are space groupP21/a,a=21.457(4)Å,b=12.184(1)Å,c=14.816(2)Å, β=91.61°(1) andV=3872Å3. The structure was refined toRw=0.077. Crystal data for cone-1·2Cr(CO)3 are space groupP21/a,a=18.019(3)Å,b=41.347(4)Å,c=11.743(2)Å, β=97.39°(1) andV=8676Å3. The single crystal included two similar but slightly different structures but the data were successfully refined toRw=0.092. The structure of 1,3-alternate-1·Cr(CO)3 differs only slightly from that of the regular 1,3-alternate calix[4]arene. In contrast, cone-1·Cr(CO)3 and cone-1·2Cr(CO)3 show an unusual conformation with a pair of faced gablelike roofs, which is considerbly distorted from the regular cone calix[4]arene. The origin of this distortion is discussed in combination with the spectral studies.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00708984
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  • 9
    Electronic Resource
    Electronic Resource
    Dicyclohexylamides as ionophores for li-selective electrodes. Crystal structures of a triamide ligand and its complex with lithium ion (1994)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 20 (1994), S. 53-71 
    Details
    ISSN: 1573-1111
    Keywords: Lithium ionophores ; podand ; dicyclohexylamides ; Li-complex ; crystal structure ; X-ray analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The influence of structure and lipophilicity of dicyclohexylamides on the lithium selectivity in membrane electrodes is discussed. The crystal structures of the triamide podand1 and its complex with LiBr1b has been determined by X-ray analysis. Crystal data for ligand1: C48H83O6N3, triclinic,P1,a=10.749(2),b=12.097(3),c=19.123(6)Å, α=95.76(2),β=80.06(2), γ=100.27(2)0,V=2403(1) Ã3,Z=2. Crystal data for the lithium complex1b: C48H83O6N3·LiBr·x C2H5OH, monoclinic,P2 1/c,a=21.297(6),b=16.316(8),c=19.450(4) Å,β=110.87(2)0,V=6315(3) Å3,Z=4. In the complex the ligand adopts a conformation in which oxygen binding sites surrounding the Li+ cation form a slightly distorted trigonal prism.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00707612
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  • 10
    Electronic Resource
    Electronic Resource
    Effects of Configuration Around the Chiral Carbon Atoms on the Crystal Properties of Ephedrinium and Pseudoephedrinium Salicylates (1994)
    Springer
    Pharmaceutical research 11 (1994), S. 1549-1556 
    Details
    ISSN: 1573-904X
    Keywords: ephedrine ; pseudoephedrine ; salicylate ; chirality ; salt formation ; homochiral crystal ; racemic compound ; racemic conglomerate ; crystal structure ; conformation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The physicochemical properties and crystal structures of the crystalline salts formed by the interaction of an achiral anion, salicylate, with homochiral and racemic ephedrinium and pseudoephedrinium cations were determined. The interaction of ephedrinium or pseudoephedrinium with salicylate in aqueous solution yielded crystalline salts with the notable exception of homochiral ephedrinium. Evaporation of the solvent from solutions of homochiral ephedrine and salicyclic acid in various organic solvents, as well as grinding together solid homochiral ephedrine and solid salicylic acid, yielded viscous semisolids suggesting that homochiral ephedrinium salicylate has a low melting point and/or a high aqueous solubility. Mixing of the two viscous solids, obtained by grinding each of the opposite enantiomers of ephedrine with equimolar salicylic acid, resulted in the formation of racemic ephedrine and subsequently, upon heating, in the formation of racemic ephedrinium salicylate. While racemic ephedrinium salicylate exists as a crystalline compound (P21/n space group) with an equal number of opposite enantiomers in the unit cell, its diastereomer, racemic pseudoephedrinium salicylate, exists as a conglomerate, i.e. a physical mixture, of the homochiral crystals of the opposite enantiomers (each P21 space group). The inability of homochiral ephedrinium to exist as a crystalline salicylate salt at 20–25°C is attributed to its high energy conformation and/or to the poor packing of homochiral ephedrinium salicylate molecules in the crystal lattice.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1018945401484
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  • 11
    Electronic Resource
    Electronic Resource
    Studies of crystalline native celluloses using potential energy calculations (1994)
    Springer
    Cellulose 1 (1994), S. 161-168 
    Details
    ISSN: 1572-882X
    Keywords: cellulose I ; molecular mechanics ; crystal structure ; molecular ; modelling
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Abstract Energies for various trial packing arrangements of unit cells for the Iα and Iβ phases of native cellulose discovered by Sugiyamaet al. were evaluated. Both a rigid-ring method, PLMR, and the full-optimization, molecular mechanics program, MM3(90), were used. For both phases the models that had the lowest PLMR energy also had the lowest MM3 energy. Both calculated models have the chains packed ‘up’, O6s intg positions, and the same sheets of hydrogen-bonded chains. The Iβ structure model is essentially identical to that proposed previously for ramie cellulose by Woodcock and Sarko. It is also the same as the best parallel model previously proposed that was based on the X-ray data of Mann, Gonzalez and Wellard, once the various unit cell conventions are considered. Also, the energies from both methods for all three celluloses, Iα, Iβ and II, are in the order that rationalizes their relative stabilites.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00819665
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  • 12
    Electronic Resource
    Electronic Resource
    Superconductivity in the tetragonal phase of La1.9Bi0.1CuO4+δ annealed under high oxygen pressure (1994)
    Springer
    Journal of superconductivity 7 (1994), S. 37-38 
    Details
    ISSN: 1572-9605
    Keywords: High-Tc superconductivity ; La1.9Bi0.1CuO4+δ ; excess oxygen ; crystal structure ; superconducting transition temperature
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Physics
    Notes: Abstract We have investigated the relation between the crystal structure and superconductivity in La1.9Bi0.1CuO4+δ , in which the phase separation observed in La2CuO4+δ is suppressed. A phase diagram in theT−δ plane is given for La1.9Bi0.1CuO4+δ with excess oxygen. For very smallδ values, the crystal structure is orthorhombic, and an orthorhombic-tetragonal phase transition occurs markedly atδ ∼ 0.03 in the measured temperature range between 13 and 293 K. Superconductivity is observed in the range of 0.04〈δ〈0.11. This is clear evidence thathigh-T c superconductivity also appears in the tetragonal phase.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00730364
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  • 13
    Electronic Resource
    Electronic Resource
    X-ray structure and thermal analysis of a 1∶1 complex between sulfathiazole andβ-cyclodextrin (1994)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 17 (1994), S. 187-201 
    Details
    ISSN: 1573-1111
    Keywords: β-Cyclodextrin ; sulfathiazole ; inclusion complex ; crystal structure ; thermal analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract An inclusion complex with the formula (β-cyclodextrin) (sulfathiazole) 8.3 H2O has been crystallized and characterized by physicochemical methods including single crystal X-ray analysis. The complex crystallizes in the monoclinic system, space group P21, witha=15.264(4),b= 16.500(6),c=15.559(5) Å,β=117.29(3)o andZ=2. The structure was solved using published co-ordinates forβ-cyclodextrin in an isomorphous complex. Refinement by block-diagonal leastsquares yieldedR=0.061 for 4706 unique observed reflections. Inclusion of sulfathiazole produces a slight ellipticity in the host conformation, but the guest adopts a conformation similar to that observed in its polymorphs. The guest is held in the macrocyclic cavity predominantly by hydrophobic forces, with the phenyl ring near the host primary hydroxyl side and the thiazole ring near the secondary hydroxyl side. The complex packs in layers parallel to theac-plane. Layers are linked by hydrogen bonding to water molecules which are located outside the cyclodextrin cavity. An extensive network of hydrogen bonds mediated chiefly by water molecules stabilizes the crystal structure.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00711858
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  • 14
    Electronic Resource
    Electronic Resource
    Phase and X-ray study of clathrate formation in the tetraisoamylammonium fluoride-water system (1994)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 17 (1994), S. 137-148 
    Details
    ISSN: 1573-1111
    Keywords: Clathrate hydrate ; phase diagram ; crystal structure ; tetraisoamylammonium fluoride
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The phase diagram of the binary (i-C5H11)4NF-water system has been studied in the clathrate formation region. Three polyhydrates have been discovered, two of which (1∶38.9 and 1∶32.7) are the known orthorhombic and tetragonal phases:Pbmn,a=11.88,b=21.53,c=12.70 Å,ρ means=1.019 g cm-3 (0°C), m.p.=32.4°C andP42/m, a=23.729,c=12.466 Å,ρ means=1.062 g cm-3, (0°C), m.p.=31.2°C, respectively. A single crystal X-ray analysis of the novel clathrate hydrate (i-C5H11)4NF·27 H2O is reported. This new clathrate hydrate is tetragonal,I4I/a, witha=16.894(5),c=17.111(2) Å,Z=4, (−50°C), and m.p.=34.6°C. Each (i-C5H11)4N+ cation occupies a four-chamber cavity built of 15-hedra 71635942 (idealized description), with small vacant 5444 cavities filling the intervening space.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00711854
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  • 15
    Electronic Resource
    Electronic Resource
    Synthesis, characterization, and crystal structure of 1,3,7,9-tetramethylpyrido-[2,3-d∶6,5-d′]-dipyrimidine-2,4,6,8-tetrone (1994)
    Springer
    Journal of chemical crystallography 24 (1994), S. 465-468 
    Details
    ISSN: 1572-8854
    Keywords: Pyrimidine ; uracil ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract A new and easy method for the preparation of 1,3,7,9-tetramethylpyrido-[2,3-d∶6,5-d′]-dipyrimidine-2,4,6,8-tetrone is described. The structure of this compound has been solved by means of X-ray diffraction methods. The chemical characterization by spectral (mass, ultraviolet, infrared, and proton nuclear magnetic resonance) and thermal (thermogravimetry and differential scanning calorimetry) method is also reported. The compound is monoclinic, space groupP21/c,a=12.720(5),b=13.688(7),c=8.079(2) Å, β=107.06(4)°,Z=4. The structure consists of discrete tricyclic molecules, stacking playing an important role in crystal packing.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01666096
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  • 16
    Electronic Resource
    Electronic Resource
    The W2Cl4(NHCMe3)2(PR 3)2 molecules (R 3=Me3, Et3, Pr n 3, Me2Ph) I. Their isomeric forms, interconversion proeesses, crystalline forms, and detailed molecular structures (1994)
    Springer
    Journal of cluster science 5 (1994), S. 11-36 
    Details
    ISSN: 1572-8862
    Keywords: Tungsten ; isomeric forms ; crystal structure ; triple bonds ; interconversion
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract A thorough study of compounds with the formula W2Cl4(NHCMe3)2(PR3)2, withR 3=Me3, Et3, Prg n 3 Me2,Ph, is reported. In addition to the previously reported crystalline compounds, namely Ia,trans-W2Cl4(NHCMe3)2(PMe3)2 in space group Pmmn;3a,trans-W2Cl4(NHCM3)2(PEt3)2 in space group P21/a (or P21/c); and4,cis-W2Cl4(NHCMe3)2(PMe2Ph)2 in Pna21, we have obtained and structurally characterized the following new substances,1b,trans-W2Cl4,(NHCMe3)2(PMe2)2, space group P21/c,a= 12.233 (4) Å,b= 12.872 (4) Å,c=17.095 (5) Å,β=93.52 (2)°,Z=4,V=2687 (1) Å3 2,cis-W2Cl4(NHCMe3)2(PMe3)2, P21/c,a=9.673 (4) Å,b=17.249 (4) Å,c=16.244 (5) Å,β=99.63 (3),Z = 4 ,V=2669 (1) Å.3b,trans-W2Cl4(NHCMe3)2(PEt3)2, Pl,a=16.850 (3) Å,b=17.797 (3) Å,c= 11.459 (2)Å,α= 101.02 (1),β= 103.13°, y=84.23 (1)°,Z=4,V= 3279 (1) Å5,trans-W2Cl4(NHCM3)2(PMe2Ph)2, Fdd2,a=39.563 (8) Å at 20°C; 39.325 (10) Å at -6O°C,b = 57.543 (17) Å at 20°C; 57.186 (16) Å at -60°C,c= 8.810 (1) Å at 20°C; 8.770 (1) Å at - 60°C ,Z=24,V=20057 (7) Å3 (20°C), 19723 (8) Å3 ( - 60°C) .6,trans-W2Cl4(NHCMe3 2(PPrn 3)2, Pl,a= 17.287 (2) Å (20°C); 17.077 (5) Å (-60°C),b= 19.119 (2) Å (20°C); 18.952 (6) Å (-60°C),c= 12.713 (1) Å (20°C); 12.668 (4) Å (-60°C),Z=4,V= 3980 (1) Å3 (20°C), 3898 (2) ,Å3 ( - 60°C). In addition, the structure of3a was re-determined and refined so that the disorder ratio was a refined parameter, leading to a value of 0.520:0.480 instead of being arbitrarily fixed at 0.50:0.50. In all of the structures the molecules are held in eclipsed (but very distorted) rotational conformations and the W-W distances are all within the range of 2.305-2.330 Å. As will be shown in a later paper, for all phosphines, thecis andtrans isomers are of similar stability and an equilibrium mixture exists in solution. It is also shown that1a and3a do not contain unexpectedly short W-N bonds as previously reported.
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    URL: http://dx.doi.org/10.1007/BF01165490
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  • 17
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    Electronic Resource
    A new platinum-osmium alkyne complex from the reaction of Pt2Os4(CO)18 with PhC ≡ CPh: The synthesis, characterization, and crystal structure of Pt2Os4(CO)8 (μ3-PhC2Ph)3(μ4-PhC2Ph) (1994)
    Springer
    Journal of cluster science 5 (1994), S. 317-326 
    Details
    ISSN: 1572-8862
    Keywords: Mixed metal cluster ; alkyne ; diphenylacetylene ; platinum ; osmium ; 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 new platinum-osmium alkyne cluster complex Pt2Os4(CO)8(μ3-PhC2Ph)3 (μ 4-PhC2Ph),2, was obtained from the reaction of Pt2Os4(CO)18,1b, with PhC2Ph and was characterized by IR.1H NMR and single-crystal X-ray diffraction analyses. The cluster of compound2 consists of an osmium capped Pt2Os3 square pyramid. It aLso contains three triply bridging and one quadruply bridging diphenylacetylene ligands. Crystal data for2: space group PI,a = 12.530(2) Å,b = 21.565(4) Å,c = 11.284(2) Å,α = 100.31(2),β = 111.89(1),β = 76.78(2),Z = 2, 3879 reflections,R = 0.032.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01170715
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  • 18
    Electronic Resource
    Electronic Resource
    The synthesis and structural analysis of the new high nuclearity platinum-ruthenium cluster complex Pt2Ru8(CO)18(μ3−EtC2Et)2(μ4−EtC2Et) containing three alkyne ligands (1994)
    Springer
    Journal of cluster science 5 (1994), S. 551-564 
    Details
    ISSN: 1572-8862
    Keywords: Mixed metal ; platinum ; ruthenium ; alkyne ; 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: Abstarct The ten metal cluster complex Pt2Ru8(CO)23(µ3−H)2, 1 was found to react with EtC2Et to form a new ten metal tris-alkyne complex Pt2Ru8(CO)18(µ3−EtC2Et)2 (µ4−EtC2Et),2 in 35% yield. Complex 2 was characterized by IR,1H NMR , and single crystalx-ray diffraction analyses. The cluster can be viewed as a dodecahedron of eight metal atoms capped with two ruthenium carbonyl groups, two triply bridging EtC2Et ligands and one quadruply bridging EtC2Et ligand. Application of the standard electron counting procedures indicate that this is an unusual complex in which the 18 electron rule applies and the polyhedral skeletal electron pair theory does not. Crystal Data for 2 2.0.5 CH2CI2: space group = P21,a = 12.759(2) A,b=18.438(2)Å,c = 20.197(3) Å,β = 91.59(1)°, Z. = 4, 6394 reflections,R = 0.037.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01171385
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  • 19
    Electronic Resource
    Electronic Resource
    Crystal structure oftrans-carbonylchlorobis-(tricyclohexylphosphine)iridium(I),trans-Ir(CO)Cl-[P(cyclo-C6H11)3]2, a disordered species (1994)
    Springer
    Journal of chemical crystallography 24 (1994), S. 557-560 
    Details
    ISSN: 1572-8854
    Keywords: Centrosymmetric ; symmetry ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound crystallizes in the centrosymmetric triclinic space group $$P\bar 1$$ (C 1 l ; No.2) witha=9.9143(10) Å,b=10.2616(11) Å,c=10.7715(10) Å, α=113.887(8)°, β=109.197(8)°, γ=90.699(9)°,V=932.78(17) Å3 andZ=1. A total of 4869 data were collected and merged to a set of 2450 independent reflections; the structure was solved and refined toR=1.42% andwR=1.94%. The molecule lies on a site of $$\bar 1$$ symmetry and is disordered, with obvious scrambling of carbonyl and chloride ligands. Resulting bond lengths include Ir−P=2.339(1) Å, Ir−Cl=2.398(4) Å and Ir−CO=1.808(15) Å.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01666737
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  • 20
    Electronic Resource
    Electronic Resource
    The crystal and molecular structure of N-(methylsulfonyl)-N-(2,6)-(dimethylphenyl)methanesulfonamide (1994)
    Springer
    Journal of chemical crystallography 24 (1994), S. 759-762 
    Details
    ISSN: 1572-8854
    Keywords: Sulfonamide ; methanesulfonanilide ; crystal structure ; molecular structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound, crystallizes in the triclinic space group $$P\bar 1$$ witha=8.232(4),b=9.159(2),c=10.230(3)Å. α=74.07(3)°, β=72.50(4)°, γ=63.65(3)° andZ=2. The structure was solved by direct methods and refined by full matrix least squares methods toR=0.054 for 1817 observed reflections. The plane containing the nitrogen and sulfur atoms is perpendicular to the aromatic plane. One of the S−O bonds in each methanesulfonyl group is in nearly eclipsed conformation with the N−C bond.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01666966
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  • 21
    Electronic Resource
    Electronic Resource
    Synthesis, structure and IR characterization of disodium tetra(9,10-dihydro-9-oxo-10-acridineacetato)zincate(II) bis(ethanol) heptahydrate (1994)
    Springer
    Journal of chemical crystallography 24 (1994), S. 731-737 
    Details
    ISSN: 1572-8854
    Keywords: Synthesis ; crystal structure ; IR data
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The synthesis, crystal structure and IR data are reported for Na2[Zn(CMA)4]·2EtOH·7H2O, where CMA− is the 9,10-dihydro-9-oxo-10-acridinacetate ion. The complex crystallizes in the monoclinic space group P2/n, with cell dimensionsa=17.335(9),b=8.440(5),c=21.875(12) Å, β=91.94(5)°,Z=2. The structure was solved by direct methods and refined to a finalR value of 0.0363 for 3022 non-zero reflections. The Zn2+ ion occupies twofold axis and is coordinated to four carboxylate ligands, the ZnO4 tetrahedron is considerably distorted with Zn−O distances of 1.978(3) and 1.961(3)Å. Each Na+ cation interacts with two water, one ethanol, and three carboxylate O atoms comprising distorted octahedron. The Zn2+ and Na+ cations are linked through monooxygen and syn-syn carboxylate bridges forming a trinuclear, mixed-metal cluster. The Zn...Na separation is 3.267(2)Å and Na...Na distance equals 3.520(2)Å. All oxygen bonded H-atoms are utilized in hydrogen bonds. The acridone rings overlap in the crystal with the 3.5 Å interlayer separations. The compound has been characterized by IR spectroscopy.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01666961
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  • 22
    Electronic Resource
    Electronic Resource
    The crystal structure of calcium succinate monohydrate (1994)
    Springer
    Journal of chemical crystallography 24 (1994), S. 437-440 
    Details
    ISSN: 1572-8854
    Keywords: Ca(C4H4O4)·H2O ; pentagonal pyramid ; calcium succinate ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal structure of calcium succinate monohydrate, Ca(C4H4O4)·H2O, has been determined by single crystal X-ray diffraction. The crystals are monoclinic witha=11.952(2),b=9.691(2),c=11.606(2)Å, β=108.81(1)°, space group C2/c,Z=8,V=1272.49 Å3,d m =1.80, andd c =1.818 Mg m−3. The structure was refined by full-matrix least-squares techniques toR=0.027,R w =0.040, for 829 reflections with1≥3δ(I). Ca is coordinated to seven oxygen atoms, and the coordination polyhedron is best described as a pentagonal bipyramid. One carboxylate group in the succinate ion is bonded to three different Ca ions, forming a four-membered chelate ring with one Ca ion is bonded to three different Ca ions, forming a four-membered chelate ring with one Ca ion and unidentate bridge bonds to two other Ca ions. The other carboxylate group is bonded to two Ca ions through unidentate bonds. The structure is highly polymeric. The general structural features are nearly identical to those of calcium adipate monohydrate.
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    URL: http://dx.doi.org/10.1007/BF01666091
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  • 23
    Electronic Resource
    Electronic Resource
    Preparation and characterization of some metal(II) complexes of isocinchomeronic acid and X-ray crystal structure ofcis-diaquabis(hydrogen isocinchomeronato)manganese(II) (1994)
    Springer
    Structural chemistry 5 (1994), S. 165-170 
    Details
    ISSN: 1572-9001
    Keywords: Isocinchomeronic acid ; 2,5-pyridinedicarboxylic acid ; hydrogen isocinchomeronate ; manganese(II) complex ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The reactions between Mn(II), Co(II), Ni(II), and Zn(II) ions with isocinchomeronic acid (H2-isocin) afforded complexes of the general formula M(H-isocin)2-2H2O, whereas Fe(II) gives both red and deep red-brown products of the same formula. Various physical measurements suggest that the complexes of M = Co, Ni, Zn, and Fe (brown) are octahedrally coordinated by two aqua ligands and twotrans-N,O-bidentate H-isocin− anions with dimeric hydrogen bonding. Those for M = Mn and Fe (red) are the correspondingcis isomers. The structure of the manganese complex as determined by X-ray crystallography exhibitsC 2 molecular symmetry with Mn-N = 2.279(2), Mn-O(H-isocin)− = 2.196(2), and Mn-O(aqua) = 2.137(2) Å. Each aqua ligand forms two donor O-H ⋯ O hydrogen bonds with carboxy groups of different molecules in adjacent chains.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02262837
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  • 24
    Electronic Resource
    Electronic Resource
    Tris(pyrazol-1-yl)-s-triazine (TPT): X-ray crystallographic, computational, and gas-phase electron diffraction studies (1994)
    Springer
    Structural chemistry 5 (1994), S. 255-264 
    Details
    ISSN: 1572-9001
    Keywords: tris(pyrazol-1-yl)-s-triazine ; crystal structure ; electron diffraction ; AM1 semiempirical calculation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The conformation of the TPT molecule has been analyzed using experimental and computational techniques. The solid-state molecular structure shows similar conformational features to those in the 2-pyrimidine and phenyl derivatives although a different pattern of bond angles in the triazine ring was observed. The AM1 calculations predicted two conformations of comparable stability (ΔE=1.8 kcal/mol) differing in the orientation of one pyrazole ring. While the minimum energy conformation corresponds to a model displayingC 3h symmetry (φ 1=φ 2=φ 3=0°), the other minimum (φ 1=φ 2=0°,φ 3=180°) is close to that observed in the solid state. The electron diffraction results are consistent with a planar or nearly planar conformation in agreement with the preceding studies.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02275498
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  • 25
    Electronic Resource
    Electronic Resource
    A complex of buckminsterfullerene with sulfur, C60·2S8: synthesis and crystal structure (1994)
    Springer
    Russian chemical bulletin 43 (1994), S. 240-244 
    Details
    ISSN: 1573-9171
    Keywords: C60·2S8 ; fullerene complexes ; synthesis ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The C60·2S8 complex was prepared by reaction of buckminsterfullerene C60 with sulfur in trichloroethylene and its single-crystal X-ray structure was studied at room temperature. Crystals of this compound are monoclinic, space groupC 2/c, a=20.90(1),b=21.10(1),c=10.537(9) Å, β=111.29(7)°,Z=4,d calc=1.89 g·cm−3. The crystal structure of the C60·2S8 complex consists of packed fullerene molecules that form hexagonal channels along thec axis with eight-membered crown-shaped S8 cyclic molecules inside the channels. The distances between the centers of neighboring fullerene molecules are 10.036(7), 10.636(7), and 10.537(9) Å. Each C60 molecule is linked to eight S8 molecules with ten shortened intermolecular contacts C...S 3.41(1)–3.52(2) Å. The average values of the C=C and C-C bond lengths are 1.32(3) and 1.47(3) Å, which attest to a significant degree of localization of electron density in the c60 molecule.
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    URL: http://dx.doi.org/10.1007/BF00695818
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  • 26
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    Electronic Resource
    Synthesis and crystal structure of an organic semiconductor (ET)4[Hg2I6] (1994)
    Springer
    Russian chemical bulletin 43 (1994), S. 1175-1179 
    Details
    ISSN: 1573-9171
    Keywords: organic conductors ; ion-radical salts ; bis(ethylenedithio)tetrathiafulvalene ; mercury iodides ; crystal structure ; electrochemical synthesis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A new cation-radical salt (ET)4[Hg2I6] (1), where ET is bis(ethylenedithio)tetrathiafulvalene, has been synthesized in the system ET-HgI3 −-PhCl. An X-ray study of 1 (a=41.02(5),b=23.01(1),c=8.233(2) Å,V=7772(3) Å3, space groupPc21 b,Z=4,d calc=2.308 g cm−3) has established its composition, chemical formula, and the main structural features. The ET cation-radicals are packed in the conducting layer, the type of packing is α″; the [Hg2I6]2− anion has a dimeric structure. The temperature dependence of the conductivity of the (ET)4[Hg2I6] crystals (σ300=6 Ohm−1 cm−1) has a semiconducting character.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00698238
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  • 27
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    Electronic Resource
    Synthesis and crystal structure of cyclotris-(4,4′-thiodiphenylene ketone) (1994)
    Springer
    Russian chemical bulletin 43 (1994), S. 1384-1389 
    Details
    ISSN: 1573-9171
    Keywords: synthesis ; macrocyclic thiophenylene ketone ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The side reaction of macrocyclization that occurs during the synthesis of poly-(1,4-phenylenesulfide ketone) by polycondensation of a 4,4-dihalobenzophenone with sodium sulfide was studied. It was found that the major product of this reaction is a cyclic trimer, cyclotris-(4,4"-thiodiphenylene ketone) (1). Despite the fact that ketone bridges are more rigid than sulfide bridges, the yield of the macrocycle is rather high, as it is in the synthesis of poly-(1,4-phenylenesulfide), and reaches 20% under high dilution conditions. The structure of 1 was investigated by X-ray diffraction analysis (R = 0.069 on 3138 reflections). Macrocycle 1 is strongly flattened in the crystal; the conformation observed is determined by the packing, since stereochemical analysis indicates high flexibility of the macrocycle. The solvate acetone molecules incorporated in the crystal are disordered, nevertheless, they are strongly fixed in the cavities and channels of the crystal structure.
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    URL: http://dx.doi.org/10.1007/BF00703700
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  • 28
    Electronic Resource
    Electronic Resource
    Liquid crystalline main chain polymers with a poly(p-phenylene-terephthalate) backbone: 7. Thermal expansion of oriented films of the polyester with dodecyloxy side chains (1994)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 32 (1994), S. 851-857 
    Details
    ISSN: 0887-6266
    Keywords: rigid rod polymer ; thermotropic ; aromatic polyester ; oriented film ; thermal expansion ; crystal structure ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The linear thermal expansion coefficients of oriented films of poly(p-phenylene-2,5-didodecyloxy-terephthalate) in the three structures B, A, and Lf are reported. The results are interpreted in terms of a molecular laminate model in which the rigid main-chain layers are separated by the aliphatic side chains. In a film oriented unidirectionally the rigid mainchain layers provide a negative contribution to the thermal expansion coefficient, while the side chains supply a positive contribution. Therefore, the resulting expansion coefficient α depends on the details of the main- and side-chain packing and low-temperature values between α = +0.3 × 10-5 K-1 (A and Lf and α = -1.2 × 10-5 K-1 (B) are found in highly oriented films. Measurements on undrawn films are in accordance with the molecular laminate model. © 1994 John Wiley & Sons, Inc.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/polb.1994.090320508
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  • 29
    Electronic Resource
    Electronic Resource
    Crystal structure and in vitro antitumour activity of dibutylbis(5-chloro-2-hydroxybenzoato)tin(IV) (1994)
    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 8 (1994), S. 19-23 
    Details
    ISSN: 0268-2605
    Keywords: Diorganotin ; carboxylate ; crystal structure ; antitumour ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The crystal structure of the title compound, [nBu2Sn(5-Cl-2-OH-C6H3CO2)2], shows that in the monomeric species the six-coordinate Sn atom exists in a skew trapezoidal bipyramidal geometry in which the four O donor atoms, derived from two asymmetrically chelating carboxylate ligands, define the basal plane and the n-butyl substituents lie over the weaker Sn—O interactions defining a C—Sn—C angle of 147.6(2)°. An unusual feature of the structure is the presence of both intra- and inter-molecular hydrogen bonding contacts which serve to stabilize the structure. The in vitro antitumour activity of this compound against mammary and colon carcinoma cell lines is also reported.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/aoc.590080105
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  • 30
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    Electronic Resource
    Crystal structure and fungitoxicity of aquatributyltin N-phthaloylglycinateAtomic coordinates for this structure have been deposited with the Cambridge Crystallographic Data Centre. The coordinates can be obtained from the Cambridge Crystallographic Data Centre, University Chemical Laboratory, University of Cambridge, Lensfield Road, Cambridge CB2 1EW, UK. (1994)
    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 8 (1994), S. 37-42 
    Details
    ISSN: 0268-2605
    Keywords: Triorganotin ; carboxylate ; crystal structure ; fungitoxicity ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The [nBu3Sn(N-phthaloylglycinate)(OH2)] compound has been prepared and characterized. The crystal structure reveals the tin atom, in each of the two molecules comprising the asymmetric unit, to exist in a distorted trigonal bipyramidal geometry in which the trigonal plane is defined by the three organic substituents and the axial sites are occupied by an oxygen atom derived from a monodentate carboxylate ligand and a coordinated water molecule. The [nBu3Sn(N-phthaloylglycinate)(OH2)] compound and three other triorganotin derivatives of N-phthaloyl-protected amino acids display marked toxicity against several economically important plant pathogenic fungi.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/aoc.590080108
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  • 31
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    Electronic Resource
    Synthesis, spectroscopic characterization and fungicidal activity of triphenyltin derivatives of N,N-dimethylglycine: Crystal structure of [dimethyl(carboxylatomethyl)ammonium]-chlorotriphenylstannateAtomic coordinates for this structure have been deposited with the Cambridge Crystallographic Data Centre. The coordinates can be obtained from the Cambridge Crystallographic Data Centre, University Chemical Laboratory, University of Camhridgc. Lenslield Road. Cambridge CB2 1 EW. UK. (1994)
    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 8 (1994), S. 33-36 
    Details
    ISSN: 0268-2605
    Keywords: Organotin ; fungicidal ; crystal structure ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The new triorganotin complexes formulated as Me2HNCH2COO · Ph3SnX, X = Cl, NCS were prepared and spectroscopically characterized, and their fungicidal properties against Ceratocystis ulmi were determined. An X-ray structure for [dimethyl(carboxylatomethyl)ammonium] chlorotriphenylstannate is also reported.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/aoc.590080107
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  • 32
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    From crystalline boryl-substituted and boryl-coupled 2,2,4,4,6,6-hexamethyl-cyclotrisilazanes to β-SiC and BNFurther data are available from the Cambridge Crystallographic Data Centre, Cambridge, UK. (1994)
    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 8 (1994), S. 491-498 
    Details
    ISSN: 0268-2605
    Keywords: Cyclosilazane ; BF-coupled rings ; crystal structure ; pyrolysis ; β-SiC/BN composites ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: [Me2SiNBFN(SiMe3)2]3 (1) is synthesized in the reaction of trilithiated hexamethylcyclotrisilazane with F2BN(SiMe3)2. The mono- and dilithium derivatives of the six-membered ring (Me2SiNH)2 Me2SiNSiFMe2 react with the F2B-substituted cyclotrisilazane F2B(NSiMe2)3(SiFMe2)2 in the molar ratio 1:1 or 1:2 to give the BF-coupled rings 2 and 3. The crystal structure analysis of 1 and 3 and pyrolysis of 1 and 3 with formation of silicon boron carbonitride and its crystallisation to composite powders at very high temperatures are reported.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/aoc.590080509
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  • 33
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    Synthesis and characterization of diorganotin(IV) derivatives of 2-mercaptopyridine and crystal structure of diphenyl pyridine-2-thiolatochlorotin(IV) (1994)
    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 8 (1994), S. 397-407 
    Details
    ISSN: 0268-2605
    Keywords: Organotin ; 2-mercaptopyridine ; pyridine-2-thiolato complexes ; Mössbauer ; IR ; NMR ; crystal structure ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Diorganotin(IV) derivatives of 2-mercaptopyridine (HSPy), R2Sn(SPy)2, R2SnCl(SPy) (R = Me, iPr, nBu, tBu, Cy, Ph) and Cy2SnBr(SPy), were obtained from R2SnX2 (X = Cl, Br) and NaSPy.Ph2SnCl(SPy) crystals, as determined by singlecrystal X-ray diffraction, are monoclinic in the space group P21/n. Tin forms with the bidentate SPy ligand a four-membered chelate ring with a short NSnS bite angle of 64.8(1)° leading to a heavily distorted trigonal-bipyramidal environment about tin. Apical Cl-Sn-N angle = 156.1(1)° equatorial C-Sn-C angle = 121.9(2)°. From 119Sn Mössbauer and IR data, analogous structures are inferred for the other solid compounds R2SnX(SPy), and distorted octahedral molecular structures for the solid compounds R2Sn(SPy)2 with R in the trans position, and sulfur atoms and nitrogen-donor atoms each in cis positions. According to IR and 1H, 13C and 119Sn NMR data, the solid-state molecular structures are retained in chloroform solution.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/aoc.590080414
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  • 34
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    Electronic Resource
    N(B(NMe2)2)(Si(NMe2)3)(Ti(NMe2)3), [N(Si(NMe2)3)(Ti(NMe2)2)]2 und N(SiMe3)(Si(NMe2)3)(Ti(NMe2)3)  -  Synthese und Charakterisierung neuer molekularer Einkomponentenvorläufer für nitridische und carbonitridische Keramiken (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 366-370 
    Details
    ISSN: 0044-2313
    Keywords: Bis(dimethylamino)boryl-tris(dimethylamino)silyl-tris(dimethylamino)titanylamin ; N,N′-Bis(tris(dimethylamino)-silyl)-1,1,3,3-tetrakis(dimethylamino)cyclobistitanazan, Trimethylsilyl-tris(dimethylamino)silyl-tris(dimethylamino)titanylamin ; Trimethylsilyl-tris(dimethylamino)-silylamin ; synthesis ; nmr spectra ; mass spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: N(B(NMe2)2)(Si(NMe2)3) (Ti(NMe2)3), [N(Si(NMe2)3)(Ti(NMe2)2)]2 und N(SiMe3)(Si(NMe2)3)(Ti(NMe2)3)  -  Synthesis and Characterization of New Molecular Single-source Precursors for Nitride and Carbonitride CeramicsSynthesis and spectroscopic data of the title compounds are reported. [N(Si(NMe2)3)(Ti(NMe2)2)]2 crystallizes in the space group P1, a = 8.406(7), b = 10.673(8), c = 10.872(6) Å, α = 68.45(4)°, β = 71.72(4)°, γ = 78.11(7)°, 2 877 diffractometer data (Fo ≥ 2σFo), R = 0.051. The compound is characterized by a planar four-membered Ti2N2-ring with exocyclic tris(dimethylamino)silyl substituents attached to the nitrogen atoms of the ring.
    Notes: Darstellung, kernresonanz- und massenspektroskopische Daten der Titelverbindungen werden mitgeteilt. [N(Si(NMe2)3)(Ti(NMe2)2)]2 kristallisiert in der Raumgruppe P1 mit den Gitterkonstanten a = 8,406(7), b = 10,673(8), c = 10,872(6) Å, α = 68,45(4)°, β = 71,72(4)°, γ = 78,11(7)°. 2 877 Diffraktometerdaten (Fo ≥ 2σFo), R = 0,051. Die Verbindung besitzt einen planaren Ti2N2-Vierring mit exocyclischen Tris(dimethylamino)silylsubstituenten an den Stickstoffatomen des Rings.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200228
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  • 35
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    Electronic Resource
    Synthesis and Crystal Structure of Hg5Sb2I6 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 389-392 
    Details
    ISSN: 0044-2313
    Keywords: Mercury antinionide iodide, Hg5Sb2I6 ; Preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese und Kristallstruktur von Hg5Sb2I6Das Antimonid-Iodid von Quecksilber, Hg5Sb2I6, früher irrtümlich als Hg3Sb2I4 formuliert, wurde in Standardampullen synthetisiert. Einkristalle wurden mittels Transport über die Gasphase erhalten. Hg5Sb2I6: Raumgruppe Pc21n, Gitterparameter: a = 8,108(1), b = 10,702(1), c = 21,295(1) Å. Die Struktur (Einkristall) ist aus [HgSbI3]-Tetraedern und [HgSbI2]-Dreiecken aufgebaut. Alle Antimonatome sind paarweise zu Sb24--Hanteln verbunden. Die Struktur wird mit anderen Strukturen, die Sb24--Hanteln enthalten, verglichen.
    Notes: Mercury antimonide iodide, Hg5Sb2I6, previously and erroneously reported as Hg3Sb2I4 was synthesized using standard ampoule technique. A gas-phase transport reaction was applied for preparation of single crystals. Hg5Sb2I6 crystallizes in the space group Pc21n (No. 33) with unit cell dimensions: a = 8.108(1), b = 10.702(1), c = 21.295(1) Å. Crystal structure solved using single crystal X-ray data is built of [HgSbI3] tetrahedra and [HgSbI2] triangles. All antimony atoms are joined into Sb24- dumbbells. The structure is compared with ones containing similar Sb24- dumbbells.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200232
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  • 36
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    Electronic Resource
    Die Chloride Na3xM2-xCl6 (M = La—Sm) und NaM2Cl6 (M = Nd, Sm): Derivate des UCl3-Typs. Synthese, Kristallstruktur und Röntgenabsorptionsspektroskopie (XANES) (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 444-450 
    Details
    ISSN: 0044-2313
    Keywords: Chlorides ; lanthanides ; synthesis ; crystal structure ; X-ray absorption spectroscopy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Chlorides Na3xM2-xCl6 (M = La—Sm) and NaM2Cl6 (M = Nd, Sm): Derivatives of the UCl3-Type of Structure. Synthesis, Crystal Structure and X-Ray Absorption Spectroscopy (XANES)Single crystals of the derivatives of the UCl3-type structure Na3xM2-xCl6 (M = La/x = 0.364(4); Ce/0.349(5); Pr/0.318(8); Nd/0.305(5); Sm/0.246(4)) and NaSm2Cl6 were grown by different methods generally under reducing conditions. They are addition [Na(Sm2)Cl6] and addition/substitution variants [Na2x(NaxM2-x)Cl6] of the UCl3 structure type [□(U2)Cl6]. X-Ray Absorption Spectroscopy (XANES) at the LIII edge characterizes NaSm2Cl6 and NaNd2Cl6 as mixed-valence compounds with valences of +2 and +3 in statistical distribution (approximately 1:1) for Sm and Nd, respectively.
    Notes: Einkristalle der Derivate des UCl3-Typs Na3xM2-xCl6 (M = La/x = 0,364(4); Ce/0,349(5); Pr/0,318(8); Nd/0,305(5); Sm/0,246(4)) sowie von NaSm2Cl6 wurden auf unterschiedlichen Wegen, im allgemeinen unter reduzierenden Bedingungen erhalten. Sie sind Additions- [Na(Sm2)Cl6] bzw. Additions- / Substitutionsvarianten [Na2x(NaxM2-x)Cl6] des UCl3-Strukturtyps [□(U2)Cl6]. Röntgenabsorptionsspektren (XANES) an der Lm-Kante charakterisieren NaSm2Cl6 und NaNd2Cl6 als gemischtvalente Verbindungen mit Valenzen von +2 und +3 in statistischer Verteilung (etwa 1:1) für Sm bzw. Nd.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200307
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  • 37
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    Electronic Resource
    Synthesis, structures and luminescence of two new Europium(II) Silicate-Chlorides, Eu2SiO3Cl2 and Eu5SiO4Cl6 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 451-456 
    Details
    ISSN: 0044-2313
    Keywords: Silicates ; crystal structure ; europium ; luminescence ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese, Strukturen und Lumineszenz von zwei neuen Europium(II)-silicat-chloriden, Eu2SiO3Cl2 und Eu5SiO4Cl6Eu2SiO3Cl2 und Eu5SiO4Cl6 wurden durch Erhitzen von EuCl2 mit EuSiO3 bzw. Eu2SiO4 gewonnen, Sr2SiO3Cl2:Eu2+ aus einem Gemenge von SrCO3, Eu2O3, SrCl2 · 6H2O und SiO2 unter reduzierenden Bedingungen. Die Kristallstrukturen von Eu2SiO3Cl2 [a = 1118,7(5), c = 952,6(1) pm, tetragonal, I4/m, Z = 8, R = 3,3, Rw = 3,0%] und Eu5SiO4Cl6 [a = 900,4(1), b = 1401,7(2), c = 1112,3(2) pm, β = 103,51(1)°, monoklin, C2/c, Z = 4, R = 3,6, Rw = 2,6%] wurden aus Einkristall-Vierkreisdiffraktometer-Daten bestimmt und mit verwandten Verbindungen verglichen. Die Lumineszenzeigenschaften wurden bei 300 K und bei 4,2 K untersucht; sämtliche Verbindungen zeigen eine intensive blaugrüne Photolumineszenz. Sr2SiO3Cl2:Eu2+ zeigt Thermolumineszenz.
    Notes: Eu2SiO3Cl2 and Eu5SiO4Cl6 were prepared by reaction of EuCl2 with EuSiO3 and Eu2SiO4, respectively, Sr2SiO3Cl2: Eu2+ from mixtures of SrCO3, Eu2O3, SrCl2 · 6H2O and SiO2 under reducing conditions. The crystal structures of Eu2SiO3Cl2 [a = 1118.7(5), c = 952.6(1) pm, tetragonal, I4/m, Z = 8, R = 3.3, Rw = 3.0%] and Eu5SiO4Cl6 [a = 900.4(1), b = 1401.7(2), c = 1112.3(2) pm, β = 103.51(1)°, monoclinic, C2/c, Z = 4, R = 3.6, Rw = 2.6%] were determined from four-circle diffractometer data and compared with related compounds. The luminescence properties were investigated at 300 K and at 4.2 K; all compounds show intense bluish-green photoluminescence. Sr2SiO3Cl2:Eu2+ shows thermoluminescence.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200308
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  • 38
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    Electronic Resource
    Synthetic and structural Studies on Organomolybdenum-Bismuth Halide Complexes (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 457-466 
    Details
    ISSN: 0044-2313
    Keywords: Organomolybdenum-bismuth halide complexes ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Untersuchungen zur Synthese und Struktur von Organomolybdän-Bismuthalogenid-KomplexenDie Reaktionen von BiBr2Ph mit Na/K[Mo(CO)3(η—C5H5)], von [BiPh{Mo(CO)3(η—C5H5)}2] mit BiBr2Ph oder BiBr3 und BiPh3 mit [Bi{Mo(CO)3(η—C5H5)}3] ergeben den Komplex [BiBrPh{Mo(CO)3(η—C5H5)}] 1, der röntgenographisch charakterisiert worden ist. Der Komplex 1 besteht aus einem Bismutzentrum mit einem Bromatom, einer Phenylgruppe und einer Mo(CO)3(η—C5H5)-Einheit. Eine intermolekulare Wechselwirkung besteht zum Bromatom eines benachbarten Moleküls, wodurch sich eine eindimensionale polymere Struktur ergibt. Bei der Umsetzung mit einer Bromidabgebenden Verbindung wird zunächst der anionische Komplex [BiBr2Ph{Mo(CO)3(η—C5H5)}2]- 3- und bei längerer Reaktion [BiBr2{Mo(CO)3(η—C5H5)}2]- 5- gebildet, das als [Ph4P]+-Salz röntgenographisch charakterisiert wurde. Der Komplex 5-, der am Bi zwei Br und zwei Mo(CO)3(η—C5H5)-Einheiten enthält, liegt in einer Struktur zwischen unvollständig trigonal-pyramidal und tetraedrisch vor. Der Komplex [PPN]2[Bi2Cl6{Mo(CO)3(η—C5H5)}2] 8 wurde ebenfalls dargestellt und röntgenographisch charakterisiert. Es liegt ein dimeres Anion vor, das aus zwei quadratischen Pyramiden mit einer gemeinsamen Kante besteht, in denen die Chloratome in der Basisebene und die zwei Mo(CO)3(η—C5H5)-Einheiten sich an den Spitzen in gegenüberliegenden Positionen befinden.
    Notes: The reactions between either BiBr2Ph and Na/K[Mo(CO)3(η—C5H5)], [BiPh{Mo(CO)3(η—C5H5)}2] and BiBr2Ph, or BiBr3 and BiPh3 and [Bi{Mo(CO)3(η—C5H5)}3] afford the complex [BiBrPh{Mo(CO)3(η—C5H5)}] 1 which has been characterised by X-ray crystallography. Complex 1 comprises a bismuth centre bonded to a bromine atom, a phenyl group and a Mo(CO)3(η—C5H5) fragment together with a longer secondary intermolecular interaction between a bromine from an adjacent molecule which results in a one-dimensional polymeric structure. Addition of a source of bromide anion to 1 affords the anionic complex [BiBr2Ph{Mo(CO)3(η—C5H5)}]- 3- although prolonged reaction results in the complex [BiBr2{Mo(CO)3(η—C5H5)}2]- 5- which was characterised by X-ray crystallography as its [Ph4P]+ salt. Complex 5- comprises a mononuclear bismuth centre bonded to two bromine atoms and two Mo(CO)3(η—C5H5) fragments in a geometry which lies between equatorially vacant trigonal bipyramidal and tetrahedral. The complex [PPN]2[Bi2Cl6{Mo(CO)3(η—C5H5)}2] 8 has also been synthesised and characterised by X-ray crystallography. A dimeric dianion is observed which can be viewed as two edge-shared square-based pyramids with chlorine atoms in the basal planes and Mo(CO)3(η—C5H5) fragments in the apical positions on opposite sides of the Bi2Cl6 plane.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200309
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  • 39
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    Electronic Resource
    The Molybdenum Stannide MoSn2In memoriam Konrad Schubert (1915-1992) (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 467-470 
    Details
    ISSN: 0044-2313
    Keywords: MoSn2 ; crystal structure ; Pauli paramagnetism ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Das Molybdän-Stannid MoSn2Die Titelverbindung wurde durch Tempern von Molybdän-Pulver mit einem Überschuß von Zinn hergestellt. Einkristalle wurden durch Auflösen der zinnreichen Matrix in Salzsäure erhalten. Sie sind Pauli-paramagnetisch. Die Kristallstruktur wurde aus Einkristall-Röntgen-Diffraktometer-Daten bestimmt: P6222, a = 548,8(1) pm, c = 1417,1(2) pm, Z = 6, R = 0,036 für 18 variable Parameter und 389 Strukturfaktoren. MoSn2 ist erst der zweite Vertreter der hexagonalen Mg2Ni-Struktur. Die Beziehung der Struktur zum CuAl2-Typ wird diskutiert.
    Notes: The title compound was prepared by annealing molybdenum powder with an excess of tin. Single-crystals were obtained by dissolving the tin-rich matrix in hydrochloric acid. They are Pauli paramagnetic. The crystal structure was determined from single-crystal X-ray diffractometer data: P6222, a = 548.8(1) pm, c = 1417.1(2) pm, Z = 6, R = 0.036 for 18 variable parameters and 389 structure factors. MoSn2 is only the second representative of the hexagonal Mg2Ni-type structure. The relation of the structure to the CuAl2-type is discussed.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200310
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  • 40
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    Electronic Resource
    Zur Kristallchemie der Kupfer-Lanthanoid-Oxowolframate: (I) triklin-α-CuTbW2O8, (II) monoklin-CuInW2O8 und (III) monoklin-CuYW2O8 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 642-646 
    Details
    ISSN: 0044-2313
    Keywords: Copper, rare earth, tungsten, oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Chemistry of Copper Rare-Earth Oxotungstates: (I): triclinic-α-CuTbW2O8, (II): monoclinic-CuInW2O8 and (III): monoclinic-CuYW2O8Single crystals of (I), (II) and (III) were prepared by recrystallisation in closed systems and examined by X-ray technique. (I): space group Cil—P1, a = 7.3080, b = 7.8945, c = 7.1476 Å, α = 115.23, β = 116.21, γ = 56.98°, Z = 2; (II): space group C2h6—C2/c, a = 9.6576, b = 11.6496, c = 4.9863 Å, β = 91.17°, Z = 4; (III): space group C2h4—P2/n, a = 10.0504, b = 5.8214, c = 5.0224 Å, β = 94.23°, Z = 2. The crystal structures are discussed with respect to calculations of the coulombterms of lattice energy and possible valence states of Cu2+ and Mo5+.
    Notes: Einkristalle von (I), (II) und (III) wurden durch Rekristallisation in geschlossenen Systemen dargestellt und röntgenographisch untersucht. Die kristallographischen Daten lauten: (I): Raumgruppe Cil—P1, a = 7,3080, b = 7,8945, c = 7,1476 Å, α = 115,23, β = 116,21, γ = 56,98°, Z = 2; (II): Raumgruppe C2h6—C2/c, a = 9,6576, b = 11,6496, c = 4,9863 Å, β = 91,17°, Z = 4; (III): Raumgruppe C2h4—P2/n, a = 10,0504, b = 5,8214, c = 5,0224 Å, β = 94,23°, Z = 2. Die Kristallstrukturen werden mit Blick auf Berechnungen der Coulombterme der Gitterenergie und mögliche Ladungen von Cu2+ und Mo5+ diskutiert.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200410
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  • 41
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    Zur Kenntnis eines Barium-Kupfer-Orthoarsenats: BaCu2(AsO4)2 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 651-654 
    Details
    ISSN: 0044-2313
    Keywords: Barium, copper, arsenic, 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 Barium-Copper-Orthoarsenate BaCu2(AsO4)2Single crystals of BaCu2(AsO4)2 were prepared above 1 000°C by CO2-LASER technique and investigated by X-ray structure determination. The light blue crystals show monoclinic symmetry, space group C2h5—P21/n, a = 4.752; b = 8.506; c = 8.945 Å; β = 93.49°, Z = 2. BaCu2(AsO4)2 represents a hitherto unknown structure type with Cu2+ in trigonal bipyramidal coordination. Ba2+ shows an 8 + 2 surrounding by O2- and As5+ is tetrahedrally coordinated. The crystal structure is discussed with respect to related orthophosphates and vanadates.
    Notes: Mit CO2-LASER-Technik wurden bei ca. 1 000°C Einkristalle der Verbindung BaCu2(AsO4)2 dargestellt und röntgenographisch untersucht. Die blaßblauen Kristalle haben monokline Symmetrie, Raumgruppe C2h5—P21/n, mit a = 4,752; b = 8,506; c = 8,945 Å; β = 93,49°, Z = 2. BaCu2(AsO4)2 repräsentiert einen neuen Strukturtyp, der Cu2+ in trigonal bipyramidaler Koordination zeigt. Ba2+ ist 8 + 2-fach und As5+ tetraedrisch von Sauerstoff umgeben. Die Kristallstruktur wird unter Bezug auf verwandte Orthophosphate und -vanadate diskutiert.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200412
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  • 42
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    Electronic Resource
    Li2H3IO6, eine neue Variante der Molybdänitstruktur (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 53-57 
    Details
    ISSN: 0044-2313
    Keywords: Dilithium trihydrogen orthoperiodate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Li2H3IO6, a New Variant of the Molybdenite StructureLi2H3IO6 crystallizes in P61 (a = 529.70(8), c = 2 759.6(5) pm; Z = 6). The crystals are twinned by merohedry, described by m ‖ [001] and 2 ⊥ [001]. According to the results of an X-ray structure determination (2 778 diffractometer data, Rw = 0.047), Li2H3IO6 exhibits a layer structure, with oxygen forming a distorted variant of the sulfur partial structure in molybdenite (MoS2), however, with iodine and lithium in the more (Li) or less (I) distorted octahedral holes. The Li2IO6 packages are connected via strong hydrogen bonds along the edges of distorted trigonal prisms.
    Notes: Li2H3IO6 kristallisiert in der Raumgruppe P61 (a = 529,70(8), c = 2 759,6(5) pm; Z = 6). Die Kristalle sind merohedrisch verviellingt, beschrieben durch m ‖ [001] und 2 ⊥ [001]. Nach der Röntgenstrukturanalyse (2 778 unabhängige Reflexe, Rw = 0,047) liegt eine Schichtstruktur vor, in der die Sauerstoffatome eine verzerrte Variante der Schwefelteilstruktur von Molybdänit (MoS2) ausbilden, die Kationen besetzen die mehr (Li) oder weniger (I) verzerrten Oktaederlücken. Die Li2IO6-Schichtpakete werden entlang der Kanten der verzerrten trigonalen Prismen durch Wasserstoffbrückenbindungen miteinander verknüpft.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200109
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  • 43
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    Zur Reaktion von 2,2′-Dilithiumbiphenyl mit SmBr3 Die Struktur von [(C24H16)SmBr(thf)2]2 · [C24H14] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 703-706 
    Details
    ISSN: 0044-2313
    Keywords: SmIII dimeric complex ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Reaction of Dilithiumbiphenyl with SmBr3. The Crystal Structure of [(C24H16)SmBr(thf)2]2 · [C24H14]In THF SmBr3 forms with [(biph)Li2] the dimeric complex [(quaph)SmBr(thf)2]2 · [C24H14]. The structure was characterized by X-ray single crystal structure analysis (space group P1 (No. 2), Z = 1, a = 943.3(6) pm, b = 1 350.3(1) pm, c = 1 599.9(9) pm, α = 64.99(5)°, β = 89.02(5)°, γ = 73.02(6)°). The Sm iones are bridged by two Br iones. Coordination by one quaph and THF ligands leads to distorded octahedra coordination of the Sm iones. Additionally crystallizes one molecule dibenzonaphthacene.
    Notes: SmBr3 reagiert mit [(biph)Li2] in THF zu dem zweikernigen Komplex [(quaph)SmBr(thf)2]2 · [C24H14]. Der Aufbau konnte durch eine Kristallstrukturanalyse geklärt werden (Raumgruppe P1 (Nr. 2), Z = 1, a = 943,3(6) pm, b = 1 350,3(1) pm, c = 1 599,9(9) pm, α = 64,99(5)°, β = 89,02(5)°, γ = 73,02(6)°). Die Sm-Ionen werden durch zwei Br-Ionen verbrückt. Durch zusätzliche Koordination eines quaph- und zweier THF-Liganden ist jedes Sm-Ion verzerrt oktaedrisch koordiniert. Zusätzlich kristallisiert ein Molekül Dibenzonaphthacen mit aus.
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    URL: http://dx.doi.org/10.1002/zaac.19946200420
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  • 44
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    Dimethylzinndithioquadratat: Die Kristallstruktur des Benzol-Solvats und des Dimethylsulfoxid-Addukts (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 723-729 
    Details
    ISSN: 0044-2313
    Keywords: Dimethyltin dithiosquarate benzene solvate ; Dimethyltin dithiosquarate-dimethylsulfoxide adduct ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Dimethyltin Dithiosquarate: The Crystal Structure of the Benzene Solvate and of the Dimethylsulfoxide Adduct(CH3)2SnS2C4O2 · 1/3 C6H6 (I) crystallizes in the orthorhombic space group Pnma. a = 14.393(2), b = 21.668(3), c = 10.424(1) Å, Z = 12.(CH3)2SnS2C4O2 · (CH3)2SO (II) is monoclinic, space group P21/n, a = 9.918(5), b = 12.028(6), c = 12.223(6) Å, β = 108.82(3)°, Z = 4.In I there are two independent dimethyltin dithiosquarate molecules. But in both molecules the Sn atoms display weak coordinative bonds to two O atoms of adjacent dithiosquarate groups. The distances amount 2.873 Å (2×), resp. 2.678 and 2.831 Å. The coordination number of tin becomes 6 and the structure gets connected in three dimensions.In II dimethylsulfoxide is bound with the O atom to Sn (2.345 Å) and the result is a distorted trigonal bipyramid. There a more distant O atom (2.944 Å) leads to a connection of the molecules to a ribbon. The changes of the geometrical parameters are described, which result from the progressive approach of the one O atom.
    Notes: (CH3)2SnS2C4O2 · 1/3 C6H6 (I) kristallisiert in der orthorhombischen Raumgruppe Pnma; a = 14,393(2); b = 21,668(3); c = 10,424(1) Å; Z = 12.(CH3)2SnS2C4O2 · (CH3)2SO (II) ist monoklin, Raumgruppe P21/n; a = 9,918(5); b = 12,028(6); c = 12,223(6) Å; β = 108,82(3)°; Z = 4.In I liegen zwei kristallographisch unabhängige Dimethyl-zinndithioquadratat-Moleküle vor. Bei beiden weisen jedoch die Sn-Atome schwache koordinative Bindungen zu zwei O-Atomen benachbarter Dithioquadratat-Gruppen auf. Die Abstände betragen 2,873 Å (2×) bzw. 2,678 und 2,831 Å. Dadurch erhält Zinn die Koordinationszahl 6, und es ergibt sich eine dreidimensional vernetzte Struktur.In II ist Dimethylsulfoxid über das O-Atom an Sn gebunden (2,345 Å), und es liegt eine verzerrte trigonale Bipyramide vor. Ein weiter entferntes O-Atom (2,944 Å) bewirkt hier die Vernetzung der Moleküle zu einem Band. Die Veränderungen der geometrischen Parameter als Folge der fortschreitenden Annäherung des einen O-Atoms werden beschrieben.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200423
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    Synthese und Kristallstruktur von Cu4[PhN3C6H4N3(H)Ph]4(μ2-O)2, einem vierkernigen Kupfer(II)-Komplex mit 1-Phenyltriazenido-2-phenyltriazenobenzol als Ligand (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 107-111 
    Details
    ISSN: 0044-2313
    Keywords: Tetrameric copper(II) complex ; μ2-oxo ligand ; 1-phenyltriazenido-2-phenyltriazeno benzene ligand ; synthesis ; 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 Cu4[PhN3C6H4N3(H)Ph]4(μ2-O)2, a Tetranuclear Copper(II) Complex with 1-Phenyltriazenido-2-phenyltriazeno-benzene as LigandCu4[PhN3C6H4N3(H)Ph]4(μ-O)2 (1) results from the reaction of an aqueous solution of [Cu(NH3)4]2+ with 1,2-bis(phenyltriazeno)benzene in ether. 1 crystallizes in the orthorhombic space group Pba2 with the lattice parameters a = 1661.5(5), b = 1914.7(7), c = 1269.2(5) pm; Z = 2. In the tetrameric complex with the symmetry C2 the Cu2+ cations form a tetrahedron (Cu—Cu: 298.3(1)-337.1(1) pm). The μ2-oxo ligands occupy the twofold axis and bridge two opposite edges of the Cu4 tetrahedron (Cu—O: 190.0(3) and 192.5(4) pm). The 1-phenyltriazenido-2-phenyltriazeno benzene anions bridge two Cu2+ ions chelating one metal ion and coordinating monodentate the neighbouring one (Cu—N: 191.0(5)-204.1(4) pm).
    Notes: Cu4[PhN3C6H4N3(H)Ph]4(μ-O)2 (1) entsteht bei der Umsetzung einer wäßrigen Lösung von [Cu(NH3)4]2+ mit 1,2-Bis(phenyltriazeno)benzol in Ether. 1 kristallisiert orthorhombisch in der Raumgruppe Pba2 mit den Gitterkonstanten a = 1661,5(5); b = 1914,7(7); c = 1269,2(5) pm; Z = 2. Im tetrameren Komplex mit der Symmetrie C2 bilden die Cu2+-Ionen ein Tetraeder (Cu—Cu: 298,3(1)-337,1(1) pm). Die μ2-Oxoliganden liegen auf der C2-Achse und überbrücken zwei gegenüberliegende Tetraederkanten (Cu—O: 190,0(3) und 192,5(4) pm). Die 1-Phenyltriazenido-2-phenyltriazeno-benzol-Anionen verbrücken benachbarte Cu2+-Ionen, die sie einerseits chelatisierend und andererseits einzähnig koordinieren (Cu—N: 191,0(5)-204,1(4) pm).
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200117
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  • 46
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    Zur Kenntnis des Natrium-tetrahydroxoaluminat-chlorids Na2[Al(OH)4]Cl (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 771-776 
    Details
    ISSN: 0044-2313
    Keywords: Tetrahydroxoaluminate chloride, Na2[Al(OH)4]Cl ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Sodium Tetrahydroxoaluminate Chloride Na2[Al(OH)4]ClThe hitherto unknown compound Na2[Al(OH)4]Cl was prepared by crystallisation from a NaCl containing sodium aluminate solution. According to the X-ray single crystal investigation (tetragonal, space group P4/nmm, a = 7.541 Å, c = 5.059 Å, Z = 2) the compound represents the first example of a crystalline hydroxoaluminate with monomeric [Al(OH)4]- anions. Cl- shows a quadratic anti prismatic coordination to 4 Na+ and over hydrogen bonds to 4 O2- while Na+ is octahedrally coordinated by 4 O2- and 2 Cl- (axial). The results of the crystal structure analysis are confirmed by 27Al and 23Na MAS NMR investigations. Na2[Al(OH)4]Cl decomposes at about 200°C without intermediates under formation of β-NaAlO2 and NaCl.
    Notes: Die bisher unbekannte Verbindung Na2[Al(OH)4]Cl wurde durch Kristallisation aus mit NaCl versetzter Natriumaluminatlösung erhalten. Entsprechend der Röntgenstrukturanalyse an einem Einkristall (tetragonal, Raumgruppe P4/nmm, a = 7,541 Å, c = 5,059 Å, Z = 2) liegt mit dieser Verbindung erstmals ein Beispiel für ein kristallines Hydroxoaluminat mit monomeren [Al(OH)4]--Anionen vor. Cl- ist quadratisch antiprismatisch mit 4 Na+ sowie über Wasserstoffbrückenbindungen mit 4 O2- koordiniert, während Na+ oktaedrisch von 4 O2- und 2 Cl- (axial) umgeben ist. Die Ergebnisse der Kristallstrukturanalyse werden durch 27Al- und 23Na-MAS-NMR-Messungen bestätigt. Na2[Al(OH)4]Cl zersetzt sich ohne Zwischenprodukte bei 200°C zu β-NaAlO2 und NaCl.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200432
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    Kristallstruktur von Hexamincyclotriphosphazen, P3N3(NH2)6Professor Friedo Huber zum 65. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 965-968 
    Details
    ISSN: 0044-2313
    Keywords: Hexamine cyclotriposphazene ; crystal growth ; crystal structure ; hydrogen-bonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of Hexamine Cyclotriphosphazene, P3N3(NH2)6In the presence of KNH2 hexamine cyclotriphosphazene semi ammoniate (molar ratio 12:1) in NH3 gives crystals of solvent free P3N3(NH2)6 within 5 d at 130°C and p(NH3) = 110 bar. The structure was solved by X-rax methods: P3N3(NH2)6: P21/c, Z = 4, a = 10.889(6) Å, b = 5.9531(6) Å, c = 13.744(8) Å, β = 97.83(3)°, Z(Fo) = 1 721 with (Fo)2 ≥ 3σ(Fo)2, Z(var.) = 157, R/Rw = 0,036/0,041The structure contains columns of molecules P3N3(NH2)6 all in the same orientation. The six-membered rings within one molecule have boat conformation. The columns are stacked together in a way that one is surrounded by four others shifted by half a lattice constant in direction [010]. Strong hydrogen bridge-bonds N—H…N connect molecules within the columns and between them.
    Notes: Bei Umsetzungen von Hexamincyclotriphosphazensemiammoniakat mit KNH2 (Molverhältnis 1:12, 5 d, T = 130°C, P(NH3) = 110 bar) in NH3 wurden Kristalle von ammoniakfreiem P3N3(NH2)6 als Nebenprodukt erhalten. Die Struktur dieser Verbindung wurde röntgenographisch bestimmt: P3N3(NH2)6: P21/c, Z = 4, a = 10,889(6) Å, b = 5,9531(6) Å, c = 13,744(8) Å, β = 97,83(3)°, Z(Fo) = 1 721 für (Fo)2 ≥ 3σ(Fo)2, Z(Parameter) = 157, R/Rw = 0,036/0,041In der Struktur liegen Säulen deckungsgleich gestapelter Moleküle P3N3(NH2)6 mit wannenförmiger Konformation vor. In nächster Umgebung befinden sich vier weitere Säulen, die um eine halbe Gitterkonstante in Richtung [010] entlang der Staperlrichtung gegenüber einer Bezugssäule versetzt sind. Starke Wasserstoffbrückenbidungen N—H⋅⋅⋅N verknüpfen die Moleküle sowohl zwischen den Säulen als auch in Säulenrichtung.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200602
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    HgPb2O2Cl2, ein „perforiertes“ Blei(II)-oxidProfessor Friedo Huber zum 65. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 977-980 
    Details
    ISSN: 0044-2313
    Keywords: Mercury(II) lead(II) oxide chloride ; synthesis ; crystal structure ; structural comparison ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: HgPb2O2Cl2, a “Perforated” Lead(II) OxideSingle crystals of HgPb2O2Cl2 were grown in a HgCl2 flux by reaction of PbO with HgCl2. Crystal structure analysis by single crystal X-ray methods were carried out. HgPb2O2Cl2 crystallizes monoclinic with a = 11.788(2) Å, b = 3.910(1) Å, c = 7.749(2) Å, β = 122.64(3)°, space group C2/m (No. 12) and Z = 2. HgPb2O2Cl2 is the first member of a new structure type, closely related to the structure of PbO.
    Notes: Einkristalle von HgPb2O2Cl2 wurden durch Umsetzung von PbO und HgCl2 in HgCl2-Schmelzen gezüchtet. An ihnen wurde der Aufbau mittels Einkristallröntgenstrukturanalyse bestimmt. HgPb2O2Cl2 kristallisiert monoklin mit a = 11,788(2) Å, b = 3,910(1) Å, c = 7,749(2) Å, β = 122,64(3)°, Raumgruppe C2/m (Nr. 12) und Z = 2. HgPb2O2Cl2 ist der erste Vertreter eines neuen Strukturtyps, der kristallchemisch von der Struktur von PbO ableitbar ist.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200604
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    AuTa14S2  -  Zentrierte (Au,Ta)13-Ikosaeder organisiert nach dem Motiv einer kubisch dichten PackungProfessor Friedo Huber zum 65. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 969-976 
    Details
    ISSN: 0044-2313
    Keywords: AuTa14S2 ; tantalum sulfides ; crystal structure ; metal icosahedra ; tetrahedral close packed structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: AuTa14S2 - Centred (Au,Ta)13 Icosahedra Organized According to the Motif of a Cubic Close PackingThe tantalum-rich phases of composition AuxTa15-xS2 (0.4 〈 x 〈 1.1) were prepared by arc-melting of appropriate compressed mixtures (Au, Ta, Ta1.35S2) and subsequent annealing of the samples in sealed molydenum crucibles. Brittle crystals with silver lustre were grown in tantalum ampoules at 1 700 K within two days using iodine as a chemical transport agent.In contrast to Vegard's rule the lattice parameters of the rhombohedral phases which are isostructural with Pd15P2, shrink with increasing gold content. The structures were determined from Rietveld fits of powder X-ray diffraction spectra and confirmed by a crystal structure analysis of a merohedral twinned crystal of Au0.7Ta14.3S2: a = 747.7(2) pm, α = 59.84(2)°, R3, Z = 1, 760 reflections (F2 〉 2σ(F2)), 30 variables, R(F) = 0.048. The parts of the volumina of the domains with distinct orientations are 0.346(4) and 0.654.Topologically the structure corresponds to a cubic close packed arrangement of Ta12-icosahedra with all non-tetrahedral interstices being filled. Gold accumulates preferentially in the centres of the icosahedra. The remaining metal atoms - two per formula and site - populate the „octahedral sites“ which are encased in stretched polyhedra limited by 32 triangulated faces. The „tetrahedral sites“ are occupied by the sulfur atoms which themselves have a ninefold, triangulated tetrakaidecahedral coordination. The complete occupation of interstices together with the specific orientation of the gold stabilized icosahedral (Au,Ta)13-clusters ensure a tetrahedral close packing of all atoms. The distortions of the packing are quantitatively analysed in terms of dihedral angles and deviations of the tetrahedral edge lengths from the mean and are compared with those of other tcp structures.
    Notes: Die tantalreichen Phasen AuxTa15-xS2 (0,4 〈 x 〈 1,1) wurden durch Aufschmelzen entsprechender Gemenge von Ta1,35S2 und den Metallen und nachfolgendes Tempern der Reguli in zugeschweißten Molybdäntiegeln hergestellt. Silbern glänzende, spröde Kristalle der neuen Phase wurden mit Iod als chemischem Transportmittel in einer Tantalampulle bei 1 700 K in 2 Tagen gezüchtet.Die Gitterkonstanten der rhomboedrisch kristallisierenden, mit Pd15P2 isostrukturellen Phasen kontrahieren mit zunehmendem Goldgehalt. Die Struktur wurde über Rietveld-Anpassungen von Röntgen-Diffraktogrammen bestimmt und durch die Strukturverfeinerung eines meroedrisch verzwillingten Kristalls der Zusammensetzung Au0,7Ta14,3S2 bestätigt: a = 747,7(2) pm, α = 59,84(2)°, R3, Z = 1, 760 Reflexe (F2 〉 2σ(F2)), 30 Variable, R(F) = 0,048. Die Volumenanteile der unterschiedlich orientierten Domänen sind 0,346(4) und 0,654.Die Struktur entspricht topologisch einer kubisch dichten Packung von Ta12-Ikosaedern, in der alle, nicht von Tetraedern eingeschlossenen Hohlräume von Atomen besetzt sind: Gold reichert sich bevorzugt im Zentrum der Ikosaeder an, die verbleibenden zwei Metallatome, die sich im Innern eines gestreckten, von Dreiecken begrenzten 32-Flächners befinden, besetzen die „Oktaederlücken“. In den „Tetraederlücken“ befinden sich die Schwefelatome. Sie sind neunfach tetrakaidekaedrisch von Tantalatomen koordiniert. Die durch Gold stabilisierten (Au,Ta)13-Cluster sind so zueinander orientiert, daß sie zusammen mit den Atomen in den anderen Lücken eine tetraedrisch dicht gepackte (tcp-) Struktur bilden, deren Verzerrungsgrad über eine Analyse der Diederwinkel und Kantenlängen der Tetraeder quantifiziert und mit dem anderer tcp-Strukturen verglichen wird.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200603
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    Kationische und anionische kantenverknüpfte Dimere in [Dy2(Dibenzo-18-Krone-6)2Cl4][Dy2(CH3CN)2Cl8]. Synthese und Kristallstruktur (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1023-1027 
    Details
    ISSN: 0044-2313
    Keywords: Dysprosium halide complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cationic and Anionic Edge-Connected Dimers in [Dy2(dibenzo-18-crown-6)2Cl4][Dy2(CH3CN)2Cl8]. Synthesis and Crystal StructureColourless single crystals of 2 DyCl3 · dibenzo-18-crown-6 · CH3CN are obtained upon reaction of DyCl3 or KDy2Cl7 with dibenzo-18-crown-6-ether in acetonitrile. The crystal structure (triclinic, P1, Z = 2; a = 1 105.6(2); b = 1 144.5(3); c = 1 367.8(3); α = 93.46(1); β = 92.27(1); γ = 117.45(1); R = 0.046; Rw = 0.033) contains cationic and anionic edge-connected dimers according to [Dy2(dibenzo-18-crown-6)2Cl4]2+ [Dy2(CH3CN)2Cl8]2+ where Dy1 and Dy2 are coordinated by 3 and 5 chloride ions, respectively.
    Notes: Bei der Umsetzung von DyCl3 oder KDy2Cl7 mit Dibenzo-18-Krone-6-Ether in Acetonitril werden farblose Kristalle der Zusammensetzung 2 DyCl3 · Dibenzo-18-Krone-6 · CH3CN erhalten. Die Kristallstruktur (triklin, P1, Z = 2; a = 1 105,6(2); b = 1 144,5(3); c = 1 367,8(3); α = 93,46(1); β = 92,27(1); γ = 117,45(1); R = 0,046; Rw = 0,033) enthält kationische und anionische, jeweils kantenverknüpfte Dimere gemäß [Dy2(Dibenzo-18-Krone-6)2Cl4]2+ [Dy2(CH3CN)2Cl8]2+, in denen Dy1 und Dy2 gegenüber Cl- die Koordinationszahlen 3 bzw. 5 aufweisen.
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    URL: http://dx.doi.org/10.1002/zaac.19946200612
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    Alkaline Earth Transition Metal Antimonides AT4Sb12 (A = Ca, Sr, Ba; T = Fe, Ru, Os) with LaFe4P12-Structure (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1028-1032 
    Details
    ISSN: 0044-2313
    Keywords: Synthesis ; crystal structure ; CaFe4Sb12 ; SrRu4Sb12 ; BaRu4Sb12 ; polyantimonides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Erdalkali-Übergangsmetall-Antimonide AT4Sb12 (A = Ca, Sr, Ba; T = Fe, Ru, Os) mit LaFe4P12-StrukturDie Titelverbindungen wurden durch Reaktion von CaSb2, SrSb2 bzw. BaSb3 mit den Übergangsmetallen und Antimon in evakuierten Quarzglasröhrchen hergestellt. Sie kristallisieren in der kubischen LaFe4P12-Struktur, die aus Röntgen-Einkristall-Daten für CaFe4Sb12, SrRu4Sb12 und BaRu4Sb12 zu Restwerten von R = 0,014, 0,016 bzw. 0,014 verfeinert wurde. Die thermischen Parameter der Erdalkaliionen nehmen mit abnehmender Ionengröße zu. Die Sb—Sb-Abstände sind in der Eisen-Verbindung größer als in den beiden Ruthenium-Verbindungen, was sich auf eine stärkere Besetzung von antibindenen Sb—Sb-Zuständen bei der Eisen-Verbindung zurückführen läßt.
    Notes: The title compounds were prepared by reaction of CaSb2, SrSb2, or BaSb3 with the transition metals and antimony in sealed silica tubes. They crystallize with the cubic LaFe4P12-structure, which was refined from single-crystal X-ray data of CaFe4Sb12, SrRu4Sb12, and BaRu4Sb12 to residuals of R = 0.014, 0.016, and 0.014, respectively. The thermal parameters of the alkaline earth ions increase with decreasing ionic size. The Sb—Sb distances are greater in the iron compound than they are in the two ruthenium compounds. This is rationalized to be due to a larger portion of electrons in antibonding Sb—Sb states in the iron compound.
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    Eu3+ und Eu2+ in Oxometallaten der Zusammensetzung MBeLn2O5: SrBeEu2O5 und EuBeNd2O5 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1033-1036 
    Details
    ISSN: 0044-2313
    Keywords: Strontium, europium, beryllium, oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Eu3+ and Eu2+ in Oxides of the Composition MBeLn2O5: SrBeEu2O5 and EuBeNd2O5Single crystals of (I): SrBeEu2O5 and (II): EuBeNd2O5 were prepared by CO2-LASER (I) in air and plasma torch (II) technique in H2 atmosphere. X-ray investigations led to orthorhombic symmetry, space group D2h16-Pnma; (I): a = 9.488, b = 7.156, c = 6.495 Å; (II): a = 9.534, b = 7.225, c = 6.544 Å, Z = 4. Sr2+ and Eu3+ as well as Eu2+ and Nd3+ are in statistical distribution within a Kagomé framework. Both compounds are discussed with respect to the monoclinic form of MBeLn2O5.
    Notes: Einkristalle von (I): SrBeEu2O5 und (II): EuBeNd2O5 wurden mit CO2-LASER- bzw. Plasmabrennertechnik an Luft bzw. unter H2-Atmosphäre dargestellt. Die röntgenographische Untersuchung führte zu orthorhombischer Symmetrie, Raumgruppe D2h16-Pnma, mit (I): a = 9,488, b = 7,156, c = 6,495 Å; (II): a = 9,534, b = 7,225, c = 6,544 Å, Z = 4. Sr2+ und Eu3+ sowie Eu2+ und Nd3+ besetzen in einem Kagomégerüst die Metallpositionen statistisch. Beide Verbindungen werden mit Blick auf die monokline Form von MBeLn2O5 diskutiert.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200614
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    Ein neues Kupfercobaltboratoxid mit isolierten B2O5-Baugruppen: Cu2Co(B2O5)O (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1051-1055 
    Details
    ISSN: 0044-2313
    Keywords: Copper cobalt borate oxide, Cu2Co(B2O5)O ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On a New Copper Cobalt Borate Oxide with Isolated B2O5 Units: Cu2Co(B2O5)OSingle crystals of a new compound with the empirical formula Cu2CoB2O6 were obtained by using a B2O3 flux technique. X-ray single crystal technique led to a new structure type. Cu2CoB2O6 crystallizes monoclinic, space group C2h5-P21/c (No. 14); a = 3.2250(6); b = 14.847(1); c = 9.1171(6) Å; β = 93.67°; Z = 4. All metal sites are octahedrally coordinated and form a two dimensional framework consisting of edge sharing octahedra ribbons. In addition one observes isolated B2O5-units and oxygen which is not coordinated to boron. The far relation to the crystal structure of the mineral Warwickite is illustrated.
    Notes: Unter Verwendung einer B2O3-Schmelze gelang die Synthese von Einkristallen einer Substanz mit der Summenformel Cu2CoB2O6, die einen eigenständigen, neuartigen Strukturtyp bildet. Sie kristallisiert in der Raumgruppe C2h5-P21/c (No. 14), a = 3,2250(6); b = 14,847(1); c = 9,1171(6) Å; β = 93,67(2)°; Z = 4. Die Metallkationen sind verzerrt oktaedrisch koordiniert und bilden durch Kantenverknüpfungen der Polyeder in zwei Richtungen ein Netzwerk aus Oktaederbändern. Die Struktur weist isolierte B2O5-Baugruppen auf und zudem Sauerstoff, der nicht an Bor gebunden ist. Eine entfernte Verwandtschaft zur Kristallstruktur des Minerals Warwickit wird aufgezeigt.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200618
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    Darstellung, Kristallstruktur und elektronenmikroskopische Untersuchung von UNb6O16 - einem neuen niobreichen Oxid im System U/Nb/O (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1056-1065 
    Details
    ISSN: 0044-2313
    Keywords: UNb6O16 ; chemical transport ; crystal structure ; HRTEM ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation, Crystal Structure and Electron Microscopic Investigation of UNb6O16 - a New Niobium-rich Phase in the System U/Nb/OPowdery UNb6O16 was produced by heating (1 000°C or 1 100°C; evacuated silica tube) mixed powders of UO2, NbO2 and Nb2O5 (1:2:2). Single-crystals of UNb6O16 were obtained by chemical transport in a small temperature gradient (1 000°C → 990°C; transport agent NH4Cl). The lattice constants are a = 22 339(4) Å; b = 3.7750(6) Å; c = 7.249(3) Å; β = 97.61(3)° and Z = 2. The structure determination (space group C2) let to R = 0.026 (Rw = 0.026). Eight oxygen atoms surround U4+ like a trans-bis-capped octahedron, Nb4+ and Nb5+ are coordinated distorted octahedraly. The structure was checked and the occupation of the positions O8 and O9 was clarified with the program MAPLE4 [3]. A through focus series of high resolution transmission electron microscopic images was obtained which is in acceptable agreement with images calculated on the basis of the multi-slice method.
    Notes: Die Darstellung von pulverförmigem UNb6O16 gelingt durch Festkörperreaktion (1 000°C oder 1 100°C; evakuierte Quarzglasampulle) aus UO2, NbO2 und Nb2O5 (Gemenge 1:2:2). Schwarze Einkristalle sind durch chemischen Transport in einem geringen Temperaturgefälle (1 000°C→990°C; Transportmittel NH4Cl) zugänglich. UNb6O16 hat die Gitterkonstanten a = 22,339(4) Å; b = 3,7750(6) Å; c = 7,249(3) Å; β = 97,61(3)°; Z = 2. Die Strukturverfeinerung anhand von Einkristalldaten (RG C2) konvergierte bei R = 0,026 (Rw = 0,026). Die Metall-Sauerstoff-Koordinationspolyeder um Uran und Niob sind stark verzerrt. U4+ kann als dodekaedrisch bzw. trans-bis-bekappt oktaedrisch (CN = 8), Nb4+ und Nb5+ als oktaedrisch (CN = 6) koordiniert angesehen werden. Mit dem Programm MAPLE4 [3] konnte die Struktur überprüft, sowie die Halbbesetzung der Punktlagen O8 und O9 geklärt werden. Eine Defokusserie hochaufgelöster elektronenmikroskopischer Durchstrahlungsaufnahmen wurde mit rechnerischen Kontrastsimulationen verglichen.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200619
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    Preparation and crystal structure of potassium manganese cyclodecaphosphate octadecahydrate: K2Mn4P10O30 · 18 H2O (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 545-550 
    Details
    ISSN: 0044-2313
    Keywords: Dipotassium tetramanganese cyclodecaphosphate octadecahydrate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung und Kristallstruktur von Kaliummangancyclodecaphosphat-octadecahydrat: K2Mn4P10O30 · 18 H2ODie Titelverbindung, ein neues Cyclodecaphosphat, wurde durch Fällung aus wäßriger K10P10O30-Lösung hergestellt. Das in Wasser wenig lösliche Salz kristalliert monoklin in der Raumgruppe P21/a mit den Gitterkonstanten a = 14,546(10), b = 15,211(10), c = 9,860(6) Å, β = 105,12(4)°.Die Kristallstruktur wurde unter Verwendung von 6501 unabhängigen Reflexen gelöst, der R-Wert beträgt 0,044.Die zentrosymmetrischen Ringanionen sind relativ weit voneinander entfernt und in einer pseudotetragonalen Weise angeordnet, so daß parallel zur c-Achse große, die Wassermoleküle enthaltende Kanäle gebildet werden.
    Notes: The title compound, a new cyclodecaphosphate, was prepared by precipitation from an aqueous solution of K10P10O30. The sparingly soluble salt crystallizes monoclinic in the space group P21/a, with Z = 2, and the unit-cell dimensions a = 14.546(10), b = 15.211(10), c = 9.860(6) Å, β = 105.12(4)°.The crystal structure was solved using 6501 unique reflections with a final R-value of 0.044.The centrosymmetrical ring anions rather distant from each other and arranged in a pseudo-tetragonal way create, parallel to the c direction, large channels containing the water molecules.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200327
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    Er3Pd7P4  -  Kristallstrukturbestimmung und Extended Hückel Rechnungen (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 561-565 
    Details
    ISSN: 0044-2313
    Keywords: Ternary palladium phosphide ; erbium ; crystal structure ; band calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Er3Pd7P4  -  Crystal Structure Determination and Extended Hückel CalculationsEr3Pd7P4 was prepared by heating the elements (1050°C) and investigated by means of single-crystal X-ray methods. The compound crystallizes in a new structure (C2/m; a = 15.180(3) Å, b = 3.955(1) Å, c = 9.320(1) Å, β = 125,65(1)°; Z = 2) with a three-dimensional framework of Pd and P atoms and with Er atoms in the holes. The Pd atoms are surrounded tetrahedrally, trigonally or linearly by P atoms, which are coordinated by nine metal atoms in the form of a tricapped trigonal prism. Therefore the atomic arrangement of Er3Pd7P4 is related to the structures of ternary transition metal phosphides with a metal: phosphorus ratio of 2:1. Band calculations using the Extended Hückel method show strong covalent Pd—P bonds and weak bonding interactions between Pd atoms with Pd—Pd distances shorter than 2.9 Å.
    Notes: Er3Pd7P4 wurde durch Erhitzen der Elemente auf 1050°C dargestellt und röntgenographisch mit Einkristallmethoden untersucht. Die Verbindung kristallisiert monoklin (C2/m; a = 15,180(3) Å, b = 3,955(1) Å, c = 9,320(1) Å, β = 125,65(1)°; Z = 2) in einer neuen Struktur mit einem dreidimensionalen Gerüst aus Pd- und P-Atomen, in dessen Lücken sich die Er-Atome befinden. Die P-Umgebung der Pd-Atome ist tetraedrisch, trigonal oder linear. Die P-Atome ihrerseits werden von 9 Metallatomen in Form eines dreifach überkappten trigonalen Prismas koordiniert. Der Aufbau von Er3Pd7P4 ist dementsprechend verwandt mit den Strukturen ternärer Übergangsmetall-Phosphide mit einem Metall: Nichtmetallverhältnis von 2:1. Extended Hückel Rechnungen zeigen u. a. neben starken kovalenten Pd—P-Bindungen schwache bindende Wechselwirkungen zwischen denjenigen Pd-Atomen, deren Abstände voneinander kürzer als 2,9 Å sind.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200329
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    Zum Komplexbildungsverhalten der 5,6-Dihalogen-7-oxa-bicyclo[2.2.1]heptan-2,3-dicarbonsäure gegenüber 3d-Übergangsmetallen (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 574-580 
    Details
    ISSN: 0044-2313
    Keywords: Manganese ; cobalt ; nickel ; copper carboxylate complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Complex Formation of 5,6-Dihalogeno-7-oxa-bicyclo[2.2.1]heptane-2,3-dicarboxylic Acid with 3d Transition ElementsCarboxylate complexes of bivalent manganese, cobalt, nickel and copper with 5,6-dichloro- and 5,6-dibromo-7-oxa-bicyclo[2.2.1]heptane-2,3-dicarboxylic acid (3 and 4) have been prepared. For cobalt and nickel two types of complexes are formed: [ML3/4(H2O)3] · H2O and [ML3/4(H2O)2], the latter is thermodynamically more stable. Manganese and copper form only complexes [MnL3/4] and [CuL3/4(H2O)2], respectively. The stereochemical configuration of the compounds have been deduced from their spectroscopic and magnetic properties. The metal atoms have been found to be in an octahedral environment. The stability constants of the complexes have been determined by potentiometric measurements. The thermal decomposition of the complexes has been studied by thermogravimetry and differential thermal analysis. The complexes of 3 are thermally more stable than the corresponding ones of 4.The X-ray structure analysis of [CoL3(H2O)3] · H2O shows a monomeric structure of the complex within the crystal and an octahedral coordination of the metal ion. The dicarboxylate anion acts as a tridentate ligand, the other octahedral sites are occupied by three water molecules. The chlorine atoms are not involved in the network of hydrogen bonds within the crystal packing.
    Notes: Es wurden Carboxylatkomplexe des zweiwertigen Mangans, Cobalts, Nickels und Kupfers mit der 5,6-Dichlor- und 5,6-Dibrom-7-oxa-bicyclo[2.2.1]heptan-2,3-dicarbonsäure (3 und 4) dargestellt. Dabei bilden sowohl Cobalt als auch Nickel zwei verschiedene Komplextypen [ML3/4(H2O)3] · H2O und [ML3/4(H2O)2] aus, wobei der letztere thermodynamisch stabiler ist. Für Mangan und Kupfer konnten dagegen nur Koordinationsverbindungen der Form [MnL3/4] bzw. [CuL3/4(H2O)2] erhalten werden. Die Ergebnisse spektroskopischer und magnetischer Messungen ließen in allen Fällen auf oktaedrische Koordinationsgeometrie schließen. Die Stabilitätskonstanten der Komplexe wurden durch potentiometrische Titration bestimmt. Die thermische Zersetzung der Verbindungen wurde mit TG-, DTG- und DTA-Methoden untersucht. Dabei erwiesen sich die Koordinationsverbindungen von 3 als thermisch stabiler als die entsprechenden von 4.Die Röntgenkristallstrukturanalyse von [CoL3(H2O)3] · H2O zeigt, daß der Komplex monomer im Kristall vorliegt und das Metallatom oktaedrisch koordiniert ist. Das Dicarboxylat-Anion fungiert als dreizähniger Chelatligand, die restlichen Oktaederplätze am Co-Atom werden von Wassermolekülen besetzt. Die Chloratome sind nicht am Wasserstoffbrückennetz im Kristallgitter beteiligt.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200332
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    Siliciumhaltige spirocyclische Phosphor(V)-Hydrazin-Heterocyclen (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 620-624 
    Details
    ISSN: 0044-2313
    Keywords: 3-Phenoxy-(1,2,4,5-tetraaza-3λ5-phospha-6-silacyclohexane)-6-spiro-1′-(silacyclohexane)-3-sulfide ; 1′,3′,5′,7′-tetraamino-2′,6′-diphenoxy-(silacyclohexane)-1-spiro-4′-(1′,3′,5′,7′-tetraaza-2′λ5,6′λ5-diphospha-4′,8′-disilacyclooctane)-8′-spiro-1″-(silacyclohexane)-2′,6′-disulfide ; NMR spectra ; crystal structure ; spirocycles ; inorganic heterocycles ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Silicon-Containing Spirocyclic Phosphorus(V) Hydrazine HeterocyclesIn the reaction of 1,1-dichlorosilacyclohexane with dihydrazido thiophosphoric acid O-phenylester in a 1:1 molar ratio in THF as solvent and in the presence of triethylamine mainly the expected spirocyclic system of inorganic and organic heterocycle is formed with the Si atom as spirocenter (ms, nmr). In addition and in low yield crystalls of a dimeric compound are isolated. A single crystall x-ray analysis reveals this compound to consist of a dispiro system with a central centrosymmetric eightmembered inorganic heterocycle connected with two silacyclohexanes via Si spirocenters.
    Notes: Bei der Umsetzung von 1,1-Dichlorsilacyclohexan mit Dihydrazidothiophosphorsäure-O-phenylester im Molverhältnis 1:1 in THF als Lösungsmittel und in Gegenwart von Triethylamin als Base entsteht überwiegend das gewünschte spiro-cyclische System aus anorganischem und organischem Sechsring mit dem Si-Atom als Spirozentrum (MS, NMR). Daneben kann in kristalliner Form in geringer Ausbeute auch eine dimere Verbindung isoliert werden, die nach einer Einkristall-Röntgenstrukturanalyse aus einem Dispiro-System mit zentralem, zentrosymmetrischem, anorganischem Achtring und zwei über Si-Atome spiro-verknüpften Silacyclohexanen besteht.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200406
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    Synthese und Kristallstruktur der molekularen Clusterverbindung W6Br14Professor Wilhelm Preetz zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1312-1320 
    Details
    ISSN: 0044-2313
    Keywords: Tungsten bromide cluster compound, W6Br14 ; synthesis ; 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 the Molecular Cluster Compound W6Br14Brownish-black crystals of W6Br14 are formed in the direct synthesis from W6Br12 and Br2 (400 K). The compound crystallizes cubically with neutral cluster molecules ([W6Br8i]Br6a): a = 13.458 Å; Pn3 (Nr. 201); d̄(W—W) = 2.653 Å; d̄(W—Bri) = 2.616 Å; d̄(W—Bra) = 2.569 Å. The W atoms are 0.03 Å outside of the Br8i cube faces. The molecules are arranged according to a cF point configuration, but each is rotated -23° about a threefold axis in order to avoid short inter cluster distances Bra—Bra. Nevertheless, via 12 short intermolecular distances per cluster of about d(Bri … Bra) = 3.487 Å the clusters are interconnected by forming two independent and interpenetrating 3D nets (Cu2O type). Although local distortion of the M6X8i cluster does not occur, as is expected for this system with 22 electrons per M6 octahedron, it is assumed that the Jahn-Teller theorem is fulfilled collectively via the low-symmetry nets of intermolecular interactions.
    Notes: W6Br14 wird bei der direkten Synthese aus W6Br12 und Br2 in Form braum-schwarzer Kristalle erhalten (400 K). Die Verbindung kristallisiert kubisch mit neutralen Clustermolekülen ([W6Br8i]Br6a): a = 13.458 Å; Pn3 (Nr. 201); d̄(W—W) = 2.653 Å; d̄(W—Bri) = 2.616 Å; d̄(W—Bra) = 2.569 Å. Die W-Atome liegen um 0.03 Å außerhalb der Br8i-Würfelflächen. Die Moleküle sind entsprechend einer cF-Konfiguration verteilt und dabei um jeweils eine der 3zähligen Achsen gedreht (-23°; Vermeidung kurzer inter-Clusterabstände Bra—Bra). Es resultieren aber pro Cluster 12 sehr kurze intermolekulare Abstände d(Bri … Bra) = 3.487 Å, über welche die Cluster zu zwei unabhängigen, sich durchdringenden 3D-Netzen miteinander verbunden sind (Cu2O-Typ). Die bei einem M6X8i-Cluster mit 22 Elektronen pro M6-Oktaeder erwartete lokale Verzerrung tritt nicht auf. Es wird angenommen, daß das Jahn-Teller-Theorem kollektiv über die niedersymmetrischen Netze intermolekularer Wechselwirkungen erfüllt wird.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200728
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    Na4[PbO4]  -  Darstellung neuer Plumbate(IV) durch Oxydation intermetallischer PhasenProfessor Hugo F. Franzen zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1346-1350 
    Details
    ISSN: 0044-2313
    Keywords: Sodium orthoplumbate ; preparation ; crystal structure ; MAPLE and CHARDI calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Na4[PbO4]  -  Preparation of new Plumbates(IV) by Oxidizing Intermetallic PhasesBy oxidizing NaPb with Na2O2 (molar ratio Na2O2:NaPb = 2.04:1; Ag-tubes; 600°C/50d) we obtained for the first time small orange coloured single crystals of Na4[PbO4]: Na4[SiO4]-type [2], P—1 (I.T. No. 2) with a = 898.5(3); b = 675.6(3); c = 592.2(2) pm; α = 124.75(1)°; β = 96.75(1)°; γ = 100.18(2)°; Z = 2; (four circle diffractometer data (MoKα-; 3 251 Io(hkl); R = 3.4%; Rw = 3.0%), parameters see text. Furthermore the Madelung part of lattice energy (MAPLE), effective coordination numbers (ECoN), mean fictive ionic radii (MEFIR) and the charge distribution (CHARDI) are being calculated.
    Notes: Durch Oxydation von NaPb mit Na2O2 (mol. Verhältnis Na2O2:NaPb = 2,04:1; Ag-Bömbchen; 600°C/50d) wurden erstmals orangefarbene, gedrungene Einkristalle von Na4[PbO4] erhalten: Na4[SiO4]-Typ [2], P—1 (I.T. No. 2) mit a = 898,5(3); b = 675,6(3); c = 592,2(2) pm; α = 124,75(1)°; β = 96,75(1)°; γ = 100,18(2)°; Z = 2; (Vierkreisdiffraktometerdaten; MoKα-; 3 251 Iohkl); R = 3,4%; Rw = 3,0%), Parameter siehe Text. Ferner werden der Madelunganteil der Gitterenergie (MAPLE), Effektive Koordinationszahlen (ECoN), Mittlere Fiktive Ionenradien (MEFIR) und die Ladungsverteilung (CHARDI) berechnet.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200803
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    Zur Existenz des Tetrahydrogenorthoperiodations Die Kristallstruktur von LiH4IO6 · H2O (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 805-808 
    Details
    ISSN: 0044-2313
    Keywords: Lithiumtetrahydrogenorthoperiodate monohydrate ; crystal structure ; tetrahydrogenorthoperiodate Ion ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Existence of the Tetrahydrogenorthoperiodate Ion. The Crystal Structure of LiH4IO6 · H2OThe crystal structure of LiH4IO6 · H2O has been determined (P1; a = 564.74(12), b = 574.41(13), c = 970.4(6) pm, α = 101.37(2), β = 96.37(2), γ = 114.72(2)°; Z = 2; 5 731 independent reflections; R = 0.038). All hydrogen-atoms were localized from difference fourier map and refined without applying constraints. Thus the existence of the tetrahydrogenorthoperiodate-ion in the solid state is proved, unambigously. The crystal structure is discussed and compared to other alkaliorthoperiodates.
    Notes: Die Kristallstruktur von LiH4IO6 · H2O wurde bestimmt (P1; a = 564,74(12), b = 574,41(13), c = 970,4(6) pm, α = 101,37(2), β = 96,37(2), γ = 114,72(2)°; Z = 2; 5 731 unabhängige Reflexe, R = 0,038). Alle Wasserstofflagen konnten aufgefunden und frei verfeinert werden und beweisen erstmals die Existenz des Tetrahydrogenorthoperiodations im Festkörper. Die Kristallstruktur wird diskutiert und mit denjenigen anderer Alkaliorthoperiodate verglichen.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200508
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    Hydrate schwacher und starker Basen. IX. Zur Wasserstoffbrückenbindung in CsNa2(OD)3 · 6D2O: Neutronenbeugung an einem Einkristall bei 120 KProfessor Heinz Dieter Lutz zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 809-813 
    Details
    ISSN: 0044-2313
    Keywords: Cesium disodium trihydroxide hexahydrate ; deuterated material ; neutron diffraction ; hydrogen bonding ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Hydrates of Weak and Strong Bases. IX. Hydrogen Bonding in CsNa2(OD)3 · 6D2O: A Single-Crystal Neutron-Diffraction Study at 120 KThe title compound is the first hydrate of a ternary alkali hydroxide reported. Its structure is related to the hexagonal perovskites and at the same time shaped by a complex system of hydrogen bonds. In a previous X-ray structure analysis at room temperature of the isotypic undeuterated material, these had been characterized only insufficiently. Therefore a complete structure determination has now been performed on a perdeuterated single crystal using low-temperature neutron-diffraction data (Pca21, Z = 4; a = 13.86, b = 6.070, c = 12.41 Å at 120 K; 1 655 observed independent reflections, R = 0.027).
    Notes: Die Titelverbindung ist das erste beschriebene Hydrat eines ternären Alkalihydroxids. Ihre Struktur ist verwandt mit der der hexagonalen Perowskite und zugleich durch ein komplexes System von Wasserstoffbrücken geprägt. Dieses war in einer vorangegangenen Röntgenstrukturanalyse bei Raumtemperatur an der isotypen nicht deuterierten Substanz nur unzureichend charakterisiert worden. Daher wurde nun eine vollständige Strukturbestimmung an einem perdeuterierten Einkristall mit Tieftemperatur-Neutronenbeugungsdaten durchgeführt (Pca21, Z = 4; a = 13,86, b = 6,070, c = 12,41 Å bei 120 K; 1 655 beobachtete unabhängige Reflexe, R = 0,027).
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200509
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    Diorganoindium-Kationen. Die Kristallstruktur von [Mes2In][BF4] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 847-850 
    Details
    ISSN: 0044-2313
    Keywords: Diorganoindium cations ; syntheses ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Diorganoindium Cations. The Crystal Structure of [Mes2In][BF4](PhCH3)2In and Mes3In react with BF3 · OEt2 in a ratio of 3:4 at 80°C in toluene to the corresponding salts [R2In][BF4] [R = PhCH2 (1), Mes (2)]. The same results could be obtained, when the diorganoindium fluorides (PhCH2)2InF and Mes2InF were treated with BF3 · OEt2 at 80°C in toluene. 1 und 2 were characterized by NMR-, IR- und MS-techniques. The arrangement of the ions in 2 could be established by an X-ray structure determination. The cations and anions of 2 are forming infinite chains. The metal centers are coordinated by two BF4--ions, so that every In atom possesses a distorted octahedral coordination sphere.
    Notes: (PhCH2)3In und Mes3In reagieren mit BF3 · OEt2 im Verhältnis 3:4 bei 80°C in Toluol zu den entsprechenden Salzen [R2In][BF4] [R = PhCH2 (1), Mes (2)]. Zum selben Ergebnis gelangt man, wenn die Diorganoindiumfluoride (PhCH2)2InF und Mes2InF mit BF3 · OEt2 bei 80°C in Toluol behandelt werden. 1 und 2 wurden mittels NMR- und IR-Spektroskopie sowie Massenspektrometrie charakterisiert. Die Anordnung der Ionen in 2 konnte durch eine Röntgenstrukturanalyse aufgeklärt werden. 2 bildet danach unendliche Ketten aus Kationen und Anionen, wobei durch eine chelatartige Anordnung zweier BF4--Ionen an jedes Metallzentrum eine verzerrt oktaedrische Koordinationssphäre der Indiumatome resultiert.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200516
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    CsNb3Br7S: Synthese, Struktur und Bindungsverhältnisse (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 863-866 
    Details
    ISSN: 0044-2313
    Keywords: CsNb3Br7S ; synthesis ; crystal structure ; bonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: CsNb3Br7S: Synthesis, Structure, and Bonding StatesThe reaction of NbBr5 with Nb, Cs and S in a sealed Nb container affords CsNb3Br7S at 800°C (3 days). Further on isotypic compounds of the general formula ANb3X7Ch with A = Rb, Cs; X = Cl, Br and Ch = S, Se are obtained. CsNb3Br7S crystallizes monoclinic (space group P21/a, Z = 2), with the lattice parameters a = 707.4(2), b = 1 888.4(4), c = 994.1(2) pm and β = 98.59(2)°. The crystal structure contains Nb3 clusters being linked by two additional Nb—Nb bonds to form infinite chains. Adjacent chains are bridged by Cs atoms in a cubeoctahedral coordination sphere of Br atoms. Similar with Nb3Br8 seven electrons occupy metal - metal bonding states.
    Notes: Bei der Reaktion von NbBr5 mit Nb, Cs und S bildet sich im verschweißten Niobrohr bei 800°C (3 Tage) CsNb3Br7S. Ferner wurden isotype Verbindungen der allgemeinen Zusammensetzung ANb3X7Ch mit A = Rb, Cs; X = Cl, Br und Ch = S, Se erhalten. CsNb3Br7S kristallisiert monoklin (Raumgruppe P21/a, Z = 2) mit den Gitterparametern a = 707,4(2), b = 1 888,4(4), c = 994,1(2) pm und β = 98,59(2)°. In der Kristallstruktur liegen Nb3-Cluster vor, die durch zwei zusätzliche Nb—Nb-Bindungen zu unendlichen Strängen verknüpft sind. Cs-Atome verbrücken benachbarte Stränge und besitzen eine kuboktaedrische Koordinationssphäre aus Br-Atomen. Wie in Nb3Br8 besetzen formal sieben Elektronen Metall - Metall-bindende Zustände.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200519
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  • 65
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    Verfeinerung der Kristallstruktur von SrO2 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 879-881 
    Details
    ISSN: 0044-2313
    Keywords: Strontium peroxide ; crystal structure ; composition ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Refinement of the Crystal Structure of SrO2Single crystals of SrO2 have been obtained after high pressure/high temperature reaction of a SrO/KClO3 mixture at 20 kbar, 1 400°C. The crystal structure was refined using 154 unique diffractometer data (I4/mmm; a = 3.5626(3), c = 6.6159(6) Å; Z = 2; R = 0.033, Rw = 0.022, S = 0.932). The O—O distance (1.493(4) Å) is significantly longer than the one previously assumed. From a refinement of the site occupation factor for oxygen a composition SrO1.95(2) has been found for the crystal investigated.
    Notes: Einkristalle von SrO2 wurden durch Hochdruck-Hochtemperatur-Reaktion eines SrO—KClO3-Gemisches bei 20 kbar, 1 400°C erhalten. Die Kristallstruktur wurde auf der Basis von Vierkreisdiffraktometerdaten (154 unabhängige Strukturfaktoren) verfeinert (I4/mmm; a = 3,5626(3), c = 6,6159(6) Å; Z = 2; R = 0,033, Rw = 0,022, S = 0,932). Der gefundene O—O-Abstand ist mit 1,493(4) Å deutlich größer als bisher angenommen. Eine Verfeinerung des Besetzungsfaktors von Sauerstoff ergab für den untersuchten Kristall eine Zusammensetzung SrO1,95(2).
    Additional Material: 2 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19946200521
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  • 66
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    Darstellung und Kristallstruktur von K6[Al2O6] und Rb6[Al2O6]Professor Heinz Dieter Lutz zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 882-887 
    Details
    ISSN: 0044-2313
    Keywords: K6[Al2O6], Rb6[Al2O6] ; preparation ; crystal structure ; MAPLE ; CHARDI ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of Crystal Structure of K6[Al2O6] and Rb6[Al2O6]Colourless single crystals of K6[Al2O6] have been prepared from intimate mixtures of KAlO2 and K2O (550°C, 90 d). The structure determination from four-circle diffractometer data (MoKα, 742 Io(hkl), R = 2.2%, Rw = 2.1%) confirms the space group C2/m with Z = 2; a = 698.25 pm, b = 1 103.54 pm, c = 646.49 pm, β = 102.49°.Colourless single crystals of hitherto unknown Rb6[Al2O6] have been prepared from intimate mixtures of RbAlO2 and Rb2O (520°C, 120 d). The structure determination from four-circle diffractometer data (MoKα, 1 240 Io(hkl)) results in the residual values R = 7.2%, Rw = 4.9%; space group C2/m; a = 725.92 pm, b = 1 143.33 pm, c = 678.06 pm, β = 104.05°; Z = 2.K6[Al2O6] and Rb6[Al2O6] are isostructural with K6[Fe2O6]. A characteristic structure unit is the anion [Al2O6]6- consisting of two edge-sharing [AlO4] tetrahedra.Effective Coordination Numbers (ECoN), Mean Fictive Ionic Radii (MEFIR), the Madelung Part of Lattice Energy (MAPLE) and the Charge Distribution (CHARDI) are calculated and discussed.
    Notes: Farblose Einkristalle von K6[Al2O6] wurden aus innigen Gemengen von KAlO2 und K2O erhalten (550°C, 90 d). Die Strukturaufklärung (Vierkreisdiffraktometer, MoKα, 742 Io(hkl), R = 2,2%, Rw = 2,1%) bestätigt die Raumgruppe C2/m mit Z = 2; a = 698,25 pm, b = 1 103,54 pm, c = 646,49 pm, β = 102,49°.Analog erhielten wir erstmals Rb6[Al2O6] aus RbAlO2 und Rb2O in Form farbloser Einkristalle (520°C, 120 d). Die Strukturaufklärung (Vierkreisdiffraktometer, MoKα, 1 240 Io(hkl)) ergab in C2/m die Residualwerte R = 7,2%, Rw = 4,9%; a = 725,92 pm, b = 1 143,33 pm, c = 678,06 pm, β = 104,05°.K6[Al2O6] und Rb6[Al2O6] sind mit K6[Fe2O6] isotyp; charakteristische Strukturelemente sind die Anionen [Al2O6]6-, die aus zwei kantenverknüpften [AlO4]-Tetraedern bestehen.Effektive Koordinationszahlen (ECoN), Mittlere Fiktive Ionenradien (MEFIR), der Madelunganteil der Gitterenergie (MAPLE) sowie die Ladungsverteilung (CHARDI) werden berechnet und diskutiert.
    Additional Material: 9 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200522
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    Pb3Al2F12: Crystal structure of a cyclo-fluoroaluminate related to Ba3Al2F12 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1449-1454 
    Details
    ISSN: 0044-2313
    Keywords: Lead fluoroaluminate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Pb3Al2F12: Kristallstruktur eines mit zu Ba3Al2F12 verwandten cyclo-FluoroaluminatDas Fluoroaluminat Pb3Al2F12 wurde in Form von Einkristallen durch Hydrothermal-Synthese erhalten und kristallisiert monoklin in P 21/n mit a = 9,435(6) Å, b = 9,610(5) Å, c = 10,100(9) Å, β = 90,59(5)°, V = 915,7(2) Å3, Z = 4, MoKα, λ = 0,71073 Å, R = 0,0463, Rw = 0,0465, 3 044 symmetrieunabhängige gemessene Reflexe. Die Struktur zeigt tetramere, isolierte, von einem Unternetzwerk unabhängiger Fluoridpolyeder eingeschlossene Oktaeder und ist mit Ba3Al2F12 verwandt. Existenz und Struktur der A3M2F12-Verbindungen werden diskutiert.
    Notes: Pb3Al2F12 is a fluorometalate obtained in single-crystal form by hydrothermal synthesis. It crystallizes in the monoclinic system, space group P 21/n, with a = 9.435(6) Å, b = 9.610(5) Å, c = 10.100(9) Å, β = 90.59(5)°, V = 915.7(2) Å3, Z = 4. The structure was solved from single crystal using 3 044 unique reflections (MoKα, λ = 0.71073 Å), R = 0.0463, Rw = 0.0465. The structure exhibits isolated tetrameric groups of octahedra encaged in a subnetwork of independent fluoride polyhedra and is related to that of Ba3Al2F12. A discussion about the existence and the structure of A3M2F12 compounds is given.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200822
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  • 68
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    Ein Beitrag über Ba3Pt4HgO11: Das erste Erdkalimetall-Oxoplatinat(II,V)/Oxomercurat (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1471-1475 
    Details
    ISSN: 0044-2313
    Keywords: Barium, mercury, platinum, oxide ; crystal structure ; high pressure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Contribution on Ba3Pt4HgO11: The First Alkaline-Earth Oxoplatinate(II,V)/OxomercurateSingle crystals of Ba3Pt4HgO11 were prepared by oxygen high pressure technique (4 200-3 600 bar) and investigated by X-ray methods. It crystallizes with hexagonal symmetry, space group D3h4—P62c, a = 6.021, c = 17.374 Å, Z = 2. Ba3Pt4HgO11 represents a new structure type, showing structural relationships to Ba2Hg3Pd7O14 and to the precious metal 6L-perovskites. The Hg2+ ions show dumb-bell like coordination, Pt2+ a square-planar surrounding and Pt5+ face shared double octahedra.
    Notes: Ba3Pt4HgO11 wurde unter hohem Sauerstoffdruck (4 200-3 600 bar) einkristallin dargestllt und röntgenographisch untersucht. Die Verbindung kristallisiert hexagonal, Raumgruppe D3h4—P62c mit a = 6,021; c = 17,374 Å; Z = 2. Ba3Pt4HgO11 bildet einen neuen Strukturtyp, der kristallchemische Verwandtschaft zu Ba2Hg3Pd7O14 und den Edelmetall-6L-Perowskiten zeigt. Die Hg2+-Ionen weisen eine hantelförmige, Pt2+ eine quadratisch-planare Koordination auf. Pt5+ bildet mit O2- flächenverknüpfte Doppeloktaeder.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200825
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    Synthesis of cis-Tetrabromobispyridinemolybdates(III) and the crystal structure of cis-(NH4)[MoBr4py2] · ⅓3 H2O (py = pyridine) (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 950-954 
    Details
    ISSN: 0044-2313
    Keywords: Tetrabromobispyridinemolybdates ; preparation ; isomerisation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung von cis-tetrabromobispyridinemolybdaten(III) und die Kristallstruktur von cis-(NH4)[MoBr4py2] · ⅓ H2O (py = Pyridin)(NH4)2[MoBr5 · H2O] reagiert mit Pyridin im Acetonitril (CH3CN) bei Zimmertemperatur. Das Produkt ist ein Gemenge von cis- und trans-(pyH)[MoBr4py2], das auf Grund der Löslichkeitsunterschiede aufgetrennt werden kann. cis-M[MoBr4py2] · ⅓ H2O (M = NH4+, Rb+, Cs+), cis-(bipyH)[MoBr4py2] (bipy = 2,2′-Bipyridyl) und cis-(PPh4)[MoBr4py2] wurden aus cis-(pyH)[MoBr4py2] dargestellt.In siedendem Acetonitril (82°C) erfolgt irreversible cis-trans-Isomerisierung. Brom oxidiert das cis-Diastereoisomere zu trans-MoBr4py2.Die Verbindungen wurden durch chemische Analyse, Infrarot-, UV-VIS-Spektroskopie, Konduktometrie und Röntgen-Pulveraufnahmen charakterisiert.Die Kristallstruktur von cis-(NH4)[MoBr4py2] · ⅓ H2O wurde bestimmt: rhomboedrisch, R3c, (No. 161), a = 15,809(3) Å, β = 112,79(2)°, Z = 6, Dröntg. = 2,29, Dgemess. = 2,27(3) g/cm3, V = 2 601(1) Å3, R1 = 0,046, Rw = 0,068. Die mittleren Mo—Br und Mo—N(Pyridin)-Abstände sind 2,58(2) bzw. 2,20(2) Å. cis-Rb[MoBr4py2] · ⅓ H2O und cis-Cs[MoBr4py2] · ⅓ H2O sind isostrukturell mit cis-(NH4)[MoBr4py2] · ⅓ H2O.
    Notes: The reaction between (NH4)[MoBr5 · H2O] and pyridine in acetonitrile (CH3CN) at room temperature results in the mixture of cis- and trans-(pyH)[MoBr4py2] which can be separated on the basis of solubility. cis-M[MoBr4py2] · ⅓ H2O (M = NH4+, Rb+, Cs+), cis-(bipyH)[MoBr4py2] (bipy = 2,2′-bipyridil) and cis-(PPh4)[MoBr4py2], were prepared from cis-(pyH)[MoBr4py2].At the temperature of boiling acetonitrile irreversible cis to trans isomerisation takes place. Bromine oxydizes cis isomers at room temperature to trans-MoBr4py2.The compounds were characterised by chemical analysis, infrared, UV-VIS spectroscopy, conductivity measurements and powder diffraction.The crystal structure of cis-(NH4)[MoBr4py2] · ⅓ H2O has been determined: rhombohedral, R3c, (No. 161), a = 15.809(3) Å, β = 112.79(2)°, Z = 6, DC = 2.29, DO = 2.27(3) g/cm3, V = 2 601(1) Å3, R1 = 0.046, Rw = 0.068. Average Mo—Br and Mo—N(pyridine) distances within the anion are 2.58(2) and 2.20(2) Å. cis-Rb[MoBr4py2] · ⅓ H2O and cis-Cs[MoBr4py2] · ⅓ H2O are isostructural with cis-(NH4)[MoBr4py2] · ⅓ H2O.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200534
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    Synthese und Struktur von [(Ph3C6H2)Te]2, [(Ph3C6H2)Te(AuPPh3)2]PF6 und [(Ph3C6H2)TeAuI2]2Professor Ekkehard Lindner zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1678-1685 
    Details
    ISSN: 0044-2313
    Keywords: Ditelluride ; [(2,4,6-Ph3C6H2)Te]2 ; Bis(triphenylphosphanegold(I))tellurolate ; [(2,4,6-Ph3C6H2)Te(AuPPh3)2]PF6 ; Diiodinegold(III) tellurolate ; [(2,4,6-Ph3C6H2)TeAuI2]2 ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of [(Ph3C6H2)Te]2, [(Ph3C6H2)Te(AuPPh3)2]PF6 and [(Ph3C6H2)TeAuI2]2[(2,4,6-Ph3C6H2)Te]2 reacts with Ph3PAu+ to yield [2,4,6-Ph3C6H2TeAuPPh32]PF6 which can be oxidized by I2 to form the gold(III) complex [(2,4,6-Ph3C6H2)TeAuI2]2. [(2,4,6-Ph3C6H2)Te]2 crystallizes in the monoclinic space group P21/c with a = 810.6(2); b = 2026.5(5); c = 2260.6(7) pm; β = 99.23(3)° and Z = 4. In the crystal structure the ditelluride exhibits a dihedral angle C11—Te1—Te2—C21 of 66.1(2)°. The distance Te1—Te2 is 269.45(6) pm. In the cation of the triclinic complex [(2,4,6-Ph3C6H2)Te(AuPPh3)2]PF6 (space group P1; a = 1197.4(3); b = 1457.2(4); c = 1680.0(6) pm; α = 84.69(3)°; β = 85.11(3)°; γ = 75.54(3)°; Z = 2) a pyramidal skeleton RTeAu2 with distances Te—Au = 259.2(1) and 257.8(2) pm and Au—Au = 295.3(1) pm is present. [(2,4,6-Ph3C6H2)TeAuI2]2 crystallizes in the triclinic space group P1 with a = 1086.3(3); b = 1462.9(6); c = 1654.2(2) pm; α = 85.25(2)°; β = 87.44(1)°; γ = 80.90(3)°; Z = 2. In the centrosymmetrical dinuclear complex [(2,4,6-Ph3C6H2)TeAuI2]2 the Au atoms exhibit a square-planar coordination by two iodine atoms and two tellurolate ligands. The tellurolate ligands form symmetrical bridges with distances Te—Au = 260.0 pm. The distances Au—I are in the range of 260.3(1) and 263.7(1) pm.
    Notes: [(2,4,6-Ph3C6H2)Te]2 reagiert mit Ph3PAu+ unter Bildung von [2,4,6-Ph3C6H2)Te(AuPPh3)2]+, das von I2 zu der Gold(III)-Verbindung [(2,4,6-Ph3C6H2)TeAuI2]2 oxidiert werden kann. [(2,4,6-Ph3C6H2)Te]2 kristallisiert monoklin in der Raumgruppe P21/c mit a = 810,6(2); b = 2026,5(5); c = 2260,6(7) pm; β = 99,23(3)° und Z = 4. In der Kristallstruktur bildet das Ditellurid einen Diederwinkel C11—Te1—Te2—C21 von 66,1(2)°. Der Abstand Te1—Te2 beträgt 269,45(6) pm. Im Kation der triklinen Verbindung [(2,4,6-Ph3C6H2)Te(AuPPh3)2]PF6 (Raumgruppe P1; a = 1197,4(3); b = 1457,2(4); c = 1680,0(6) pm; α = 84,69(3)°; β = 85,11(3)°; γ = 75,54(3)°; Z = (2) liegt ein pyramidales RTeAu2-Gerüst mit Abständen Te—Au = 259,2(1) und 257,8(2) pm und Au—Au = 295,3(1) pm vor. [(2,4,6-Ph3C6H2)TeAuI2]2 kristallisiert in der triklinen Raumgruppe P1 mit a = 1086,3(3); b = 1462,9(6); c = 1654,2(2) pm; α = 85,25(2)°; β = 87,44(1)°; γ = 80,90(3)°; Z = 2. Im zentrosymmetrischen Zweikernkomplex [(2,4,6-Ph3C6H2)TeAuI2]2 sind die Au-Atome quadratisch planar von zwei Iod-und zwei Tellurolatoliganden koordiniert. Die Tellurolatoliganden bilden symmetrische Brücken mit Au—Te-Abständen von 260,0 pm. Die Au—I-Abstände liegen zwischen 260,3(1) und 263,7(1) pm.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201003
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    Neue ternäre Selenide der Lanthanide durch Reduktion der SesquiselenideProfessor Reinhard Schmutzler zum 60. Geburtstag gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1698-1701 
    Details
    ISSN: 0044-2313
    Keywords: Ternary selenides of lanthanides ; preparation ; crystal structure ; electronic structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Ternary Selenides of Lanthanoides by Reduction of SesquiselenidesThe compounds MLn2Se3 (M = Na; Ln = La—Sm) and MLn8Se12 (M = Na, Ca; Ln = La—Sm) were prepared by reduction of the corresponding lanthanide sesquiselenides with sodium and calcium, respectively, for the first time. Further-more MLa8Se12 (M = Sr, Eu) could be obtained in an analogous way. All compounds were characterized by chemical analysis and X-ray powder diffraction. The electronic structures of these compounds were investigated by band structure calculations and magnetic measurements.
    Notes: Die Verbindungen MLn2Se3 (M = Na, Ln = La—Sm) und MLn8Se12 (M = Na, Ca; Ln = La—Sm) wurden durch Reduktion der entsprechenden Lanthanidsesquiselenide mit Natrium bzw. Calcium erstmals dargestellt. Weitere Selenide MLa8Se12 (M = Sr, Eu) konnten analog erhalten werden. Die dargestellten Verbindungen wurden analytisch und röntgenographisch charakterisiert. Zur Bestimmung der elektronischen Struktur dieser Verbindungen wurden Bandstrukturrechnungen und magnetische Messungen durchgeführt.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201006
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    TlCu(OH)CO3  -  Ein neues basisches Thallium-Kupfer-Carbonat (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1707-1713 
    Details
    ISSN: 0044-2313
    Keywords: Thallium-μ-carbonato-μ-hydroxo-copper(II) ; synthesis ; crystal structure ; thermal decomposition ; IR-spectroscopy ; magnetic properties ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: TlCu(OH)CO3  -  a New Basic Thallium Copper CarbonateTlCu(OH)CO3 was prepared from carbonate solutions. Its crystal structure was determined (hexagonal, P63/m (Nr. 176), a = 1084.9(1), b = 611.8(1) pm, VEZ = 623.6(1) X 106 pm3, Z = 6, R = 0.036, Rw = 0.020). Structural features are Cu—O chains bridged by carbonate groups and tunnels parallel [0 0 1]. The thermal behaviour of the new carbonat was examined with TG/DTA- and Simon-Guinier-techniques. The decomposition occurs in two steps to the products Tl2O and CuO. Magnetic measurements show Curie-paramagnetism with θCurie = 2.7 K. A ferromagnetic arrangement of the Cu2+-moments was detected below 4.8 K. An IR-spectrometric characterisation in comparision with other copper-carbonato complexes will be discussed.
    Notes: TlCu(OH)CO3 wurde aus wäßrigen Carbonatlösungen dargestellt. Es kristallisiert hexagonal, in der RG P63/m (Nr. 176), mit a = 1084,(1), b = 611,8(1) pm, VEZ = 623,6(1) · 106 pm3, Z = 6, R = 0,036, Rw = 0,020. Struktur-bestimmende Merkmale sind über Carbonatgruppen verbrückte Cu—O-Ketten und parallel [0 0 1] verlaufende kanalartige Hohlräume. Das thermische Verhalten wurde mittels TG/DTA-Untersuchungen und Simon-Guinier-Aufnahmen untersucht. Die Zersetzung erfolgt in zwei Schritten zu Tl2O und CuO als Endprodukte. Magnetische Messungen ergeben einen reinen Curie-Paramagnetismus mit θCurie = 2,7 K. Unterhalb 4,8 K wird eine ferromagnetische Ordnung der Cu2+ -Momente festgestellt. Das IR-Spektrum wird im Vergleich mit Spektren anderer Kupfer(II)-carbonato-Komplexe diskutiert.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201008
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    Einkristallstudien zur Temperaturabhängigkeit der Kristallstruktur von α-Na3HgProfessor H. D. Lutz zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1736-1740 
    Details
    ISSN: 0044-2313
    Keywords: Sodium amalgam, Na3Hg ; α - β phase change ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Temperature Dependent Single Crystal Investigations of α-Na3HgIn contrast to β-Na3Hg (rhomboedrally distorted Li3Bi-type) α-Na3Hg crystallizes in a hitherto poorly understood variant of the Na3As-type. Based on temperature dependent measurements of poly- and single crystalline samples (-100°C 〈 T 〈 +35°C) we show, that in particular the sodium atoms (Na1) located in the region of the octahedral Hg6-holes show a pronounced temperature dependent dynamical behaviour. To a lesser extend this is also true for the tetrahedrally coordinated Na-atoms (Na2). With increasing temperature the former ones more and more approach the centers of the opposite triangular faces of mercury atoms, limiting the Hg6-octahedra along [001]. Occupation of the latter positions by sodium atoms would lead to unusual short interatomic distances dNa—Hg. However before reaching this unreasonable situation α-Na3Hg decomposes under formation of β-Na3Hg.
    Notes: Im Unterschied zu β-Na3Hg (rhomboedr. verzerrter Li3Bi-Typ) kristallisiert α-Na3Hg in einer bislang unverstandenen Variante des hexagonalen Na3As-Typs (Tu(α β) = + 36°C). Ausgehend von temperaturabhängigen Messungen an mikro- und einkristallinen Proben (-100°C 〈 T 〈 +35°C) können wir klar zeigen, daß insbesondere die Na-Atome (Na1) im „Einzugsbereich“ der Hg6-Oktaederlücken eine ausgeprägte, temperaturabhängige Dynamik zeigen. Dies gilt in geringem Maße auch für die tetraedrisch durch Hg koordinierten Na-Atome (Na2). Erstere entfernen sich mit zunehmender Temperatur von den Oktaederzentren und „tauchen“ mehr und mehr in die längs [001] gegenüberliegenden, die Hg6-Oktaeder begrenzenden Dreiecksflächen ein. Vor Erreichen des Mittelpunktes der Dreiecksflächen, einer Atomposition, die zwar dem idealen Na3As-Typ entspricht, deren Besetzung aber im vorliegenden Fall zu unakzeptabel kurzen interatomaren Abständen dNa—Hg führen würde, findet jedoch die Phasenumwandlung α-→β-Na3Hg statt.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201013
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    SnCl2 als Brückenligand in [{(CO)5M}2Sn(Cl)2]2- (M = Cr, Mo, W)  -  Synthese, Struktur und ReaktivitätProfessor Wilhelm Preetz zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1760-1767 
    Details
    ISSN: 0044-2313
    Keywords: SnCl2 bridging ligand ; pentacarbonylmetal derivatives ; organometallic protection ; Sn—O-cage compound ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: SnCl2 as a Bridging Ligand in [{(CO)5M}2Sn(Cl)2]2- (M = Cr, Mo, W)  -  Synthesis, Structure, and Reactivity[{(CO)5Cr}2Sn(Cl)2]2-, 1, may be obtained from [(CO)5Cr]2- or [(CO)5CrSnCl2 · THF] in fair yields. Alternatively, 1 is accessible by the reaction of [Cr2(CO)10]2- with SnCl2. This procedure may be extended to the synthesis of [{(CO)5M}2Sn(Cl)2]2- (M = Mo, 2; M = W, 3). The compounds 1-3 are crystallized as their alkalimetal (12-crown-4)2 or [2,2,2]cryptand salts. X-ray analyses demonstrate bridging SnCl2-moieties with M—Sn—M-angles close to 130° in each case. The relation of the bonding situation in 1-3 to the ones observed for stannylene or „inidene“ complexes, respectively, is discussed. The transformation of 1 into the rhombododecahedral (X-ray analysis) Sn—O-cage compound [{(CO)5CrSn}6(μ3-O)4(μ3-OH)4], 4, demonstrates the reactivity of the dianions 1-3.
    Notes: [{(CO)5Cr}2Sn(Cl)2]2, 1, kann aus [(CO)5Cr]2- oder [(CO)5CrSnCl2 · THF] in guten Ausbeuten dargestellt werden. Alternativ ist 1 aus [Cr2(CO)10]2- und SnCl2 zugänglich. Dieses Verfahren kann auf die Synthese von [{(CO)5M}2Sn(Cl)2]2- (M = Mo, 2; M = W, 3) übertragen werden. Die Dianionen 1-3 werden als Alkalimetall-(12-Krone-4)2 oder -[2,2,2]Kryptand-Salze kristallisiert. Einkristallröntgenstrukturanalysen zeigen jeweils die Verbrückung durch die SnCl2-Einheit mit M—Sn—M-Winkeln nahe bei 130°. Die Beziehung der Bindungsverhältnisse in 1-3 zu denen, die in Stannylen- oder „Iniden“-Komplexen beobachtet werden, wird diskutiert.Die Umwandlung von 1 in die rhombendo-dekaedrische (Röntgenstrukturanalyse) Käfigverbindung [{(CO)5CrSn}6(μ3-O)4(μ3-OH)4], 4, belegt die Reaktivität der Dianionen 1-3.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201017
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    Ba[CoN]: Ein niedervalentes Nitridocobaltat mit gewinkelten Ketten ∞1[CoN2/22-] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1781-1785 
    Details
    ISSN: 0044-2313
    Keywords: Nitridocobaltate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ba[CoN]: A Low-Valency Nitridocobaltate with Angled Chains ∞1[CoN2/22-]Ba[CoN] is prepared by reaction of barium and cobalt (molar ratio Ba : Co = 1 : 2.5) in tantalum crucibles at 870°C with flowing nitrogen (1 atm) within a period of 96 h. After cooling down to room temperature (24°C/h) black single crystals of the ternary phase with a platy habit are obtained (orthorhombic, Pnma; a = 959.9(2) pm, b = 2 351.0(3) pm, c = 547.6(2) pm; Z = 20). The crystal structure of Ba[CoN] contains angled (planar) chains ∞1[CoN2/22-] which run along the [010]-direction (N—Co—N[°]: 178.5(5), 179.6(6), 180.0; Co—N—Co[°]: 82.9(6), 84.2(5), 177.1(8); Co—N[pm]: 174.6(12), 177.2(12), 181.9(13), 184.3(13), 187.1(12)). Nitrogen is in an octahedral coordination (N Ba4Co2) and is arranged in a distorted cubic close packing. Barium occupies one half of the tetrahedral holes (Ba—N[pm]: 274.8(16) - 308.2(12)). The cis-positions of the Co-atoms at the nitrogen coordination-octahedra cause short Co—Co contacts within the chains ∞1[CoN2/22-]. Through this, Co2-units (Co—Co[pm]: 247.8(4); bridged by nitrogen) and linear Co3-groups (Co—Co [pm]: 245.5(2); Co—Co—Co[°]: 180.0; bridged by nitrogen) alternate along the chains.The crystal structure of Ba[CoN] is closely related to the Ba[NiN] type structure.
    Notes: Ba[CoN] wird durch Umsetzung von Barium und Cobalt im molaren Verhältnis Ba: Co = 1 : 2,5 bei 870°C im Tantaltiegel mit strömendem Stickstoff (1 atm) dargestellt. Die Reaktionszeit beträgt 96 h. Nach Abkühlen auf Raumtemperatur (24°C/h) liegt die ternäre Phase in Form schwarzer Einkristalle mit plattigem Habitus vor (orthorhombisch, Pnma; a = 959,9(2) pm, b = 2 351,0(3) pm, c = 547,6(2) pm; Z = 20). Die Kristallstruktur von Ba[CoN] enthält gewinkelte (ebene) Ketten ∞1[CoN2/22-], die entlang [010] verlaufen (N—Co—N[°]: 178,5(5), 179,6(6), 180,0; Co—N—Co[°]: 82,9(6), 84,2(5), 177,1(8); Co—N[pm]: 174,6(12), 177,2(12) 181,9(13), 184,3(13), 187,1(12)). Stickstoff ist oktaedrisch koordiniert (N Ba4Co2) und bildet das Motiv einer verzerrt kubisch dichtesten Packung. Barium besetzt eine Hälfte der Tetraederlücken (Ba—N[pm]: 274,8(16) - 308,2(12)). Die cis-Positionierung der Co-Atome an den Stickstoff-Koordinationsoktaedern bedingt kurze Co—Co-Abstände innerhalb der Ketten ∞1[CoN2/22-], so daß von Stickstoff überbrückte Co2-Einheiten (Co—Co[pm]: 247,8(4)) und gestreckte, von Stickstoff überbrückte Co3-Gruppen (Co—Co[pm]: 245,5(2); Co—Co—Co[°]: 180,0) in Kettenrichtung alternierend aufeinanderfolgen.Die Kristallstruktur von Ba[CoN] zeigt enge Verwandtschaft zum Ba[NiN]-Typ.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201020
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    Nitrido-Sodalithe. I Synthese, Struktur und Eigenschaften von Zn7-xH2x[P12N24]Cl2 mit 0 ≤ x ≤ 3 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 2014-2019 
    Details
    ISSN: 0044-2313
    Keywords: Phosphorus nitrides ; nitrido sodalites ; synthesis ; crystal structure ; i.r. data ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Nitrido Sodalites. I Synthesis, Crystal Structure, and Properties of Zn7-xH2x [P12N24]Cl2 with 0 ≤ x ≤ 3The nitrido sodalites Zn7-xH2x[P12N24]Cl2 with 0 ≤ x ≤ 3 are obtained by heterogeneous pressure-ammonolysis of P3N5 at presence of ZnCl2 (T = 650°C). These compounds are available too by reaction of ZnCl2, (PNCl2)3, and NH4Cl at 700°C. The crystal structures of four representatives of the above mentioned compounds have been refined by the Rietveld full-profile technique using X-ray powder diffractometer data (I43m, a = 821.61(4) to 824.21(1) pm, Z = 1). In the solid a three-dimensional framework of corner-sharing PN4-tetrahedra occurs (P—N: 163.6 pm, P—N—P: 125.6°, mean values) which is isosteric with the sodalite type of structure. In the center of the β-cages Cl- ions have been found, which are tetrahedrally coordinated by Zn2+ ions. The Zn2+ ions are statistically disordered. According to the phase-width observed (0 ≤ x ≤ 3) the Zn2+ ions may be partially replaced each by two hydrogen atoms which on the other hand are covalently bonded to nitrogen atoms of the P—N framework. The IR-spectra of these compounds show characteristic vibrations.
    Notes: Die Nitrido-Sodalithe Zn7-xH2x[P12N24]Cl2 mit 0 ≤ x ≤ 3 wurden durch heterogene Druckammonolyse von P3N5 in Gegenwart von ZnCl2 (T = 650°C) dargestellt. Die Verbindungen sind auch zugänglich durch Umsetzung von ZnCl2, (PNCl2)3 und NH4Cl bei 700°C. Die Kristallstrukturen von vier ausgewählten Vertretern der obigen Verbindungsreihe wurden auf der Basis von Röntgen-Pulverdiffraktometerdaten mit Hilfe der Rietveld-Methode verfeinert (I43m, a = 821,61(4) bis 824,21(1) pm, Z = 1). Im Festkörper liegt eine dreidimensionale Gerüststruktur allseitig eckenverknüpfter PN4-Tetraeder vor (P—N: 163,6 pm, P—N—P: 125,6°, Mittelwerte), die dem Sodalith-Typ entspricht. Im Zentrum der β-Käfige befinden sich Cl--Ionen, die ihrerseits tetraedrisch durch Zn2+-Ionen umgeben sind. Die Zn2+-Positionen sind statistisch besetzt und gemäß der angegebenen Phasenbreite (0 ≤ x ≤ 3) kann ein Teil der Zn2+-Ionen durch jeweils zwei H-Atome ersetzt werden, die ihrerseits kovalent an Stickstoffatome des P—N-Gerüstes gebunden sind. Im IR-Spektrum der Verbindungen werden charakteristische Schwingungsbanden beobachtet.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201130
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    Li10Si2PbIIO10 = Li20[(SiO4)4(OPbO2PbO)]  -  Das erste „gemischte“ Silicat-Plumbat(II)Professor Kurt Issleib in memoriam (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 2026-2032 
    Details
    ISSN: 0044-2313
    Keywords: Lithium silicate plumbate ; preparation ; crystal structure ; MAPLE and CHARDI calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Li10Si2PbIIO10 = Li20[(SiO4)4(OPbO2PbO)]  -  The first „mixed“ Silicate-Plumbate(II)Colourless crystals of Li10Si2PbO10 were obtained by heating a well-ground mixture of LiPb, Li2O2 and „SiO2“ (deriving from Duran glas) in Ag-tubes (650°C; 60 d). The crystal structure was determined (four-circle diffractometer data, Mo—Kα-, 1 474 Io(hkl), R = 4.2%, Rw = 2.8%, parameters see text). The silicate-plumbate crystallizes monoclinic (space group C2/m; I. T. No. 12) with a = 2985.1(4); b = 610.6(6); c = 512.8(1) pm, β = 99.70(9)° (four-circle data), Z = 4.Further the Madelung Part of Lattice Energy (MAPLE), Effective Coordination Numbers (ECoN), the Mean Fictive Ionic Radii (MEFIR) and the Charge Distribution (CHARDI) are being calculated.
    Notes: Farblose Kristalle von Li10Si2PbO10 entstanden beim Tempern inniger Gemenge von LiPb, Li2O2 und „SiO2“ (aus Duranglas) in Ag-Bömbchen (650°C; 60 d). Die Kristallstruktur wurde aufgeklärt (Vierkreisdiffraktometerdaten, Mo—Kα-, 1 474 Io(hkl), R = 4,2%, Rw = 2,8%, Parameter siehe Text). Das Silicat-Plumbat kristallisiert monoklin (Raumgruppe C2/m; I. T. No. 12) mit a = 2 985,1(4); b = 610,6(1); c = 512,8(1) pm; β = 99,70(9) (Vierkreisdaten), Z = 4.Ferner werden der Madelunganteil der Gitterenergie (MAPLE), Effektive Koordinationszahlen (ECoN), die Mittleren Fiktiven Ionenradien (MEFIR) sowie die Ladungsverteilung (CHARDI) berechnet.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201203
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    Hydrate schwacher und starker Basen. XI. Die Kristallstrukturen von NaOH · 3,5H2O und NaOH · 7 H2O. Eine PräzisierungProfessor Horst Sabrowsky zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1509-1513 
    Details
    ISSN: 0044-2313
    Keywords: Sodium hydroxide hydrates ; crystal structure ; hydrogen bonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Hydrates of Weak and Strong Bases. XI. The Crystal Structures of NaOH · 3,5H2O and NaOH · 7 H2O. A RefinementThe crystal structures of the hydrates NaOH · 3,5 H2O (space group P21/c, Z = 8 formula units per unit cell; lattice parameters: a = 6.481, b = 12.460, c = 11.681 Å, β = 104.12° at -100°C) and NaOH · 7 H2O (P21/c, Z = 4; a = 7.344, b = 16.356, c = 6.897 Å, β = 92.91° at -150°C) have been redetermined using MoKα diffractometer data. The obtained refinement of the structures, including the localization also of the H atoms for the first time, has led to new findings with respect to the H bonds. In particular, in both hydrates there is one such interaction of the rare type OH- … OH2, from an OH- ion to an H2O molecule, i. e. with the OH- ion as the proton donor.
    Notes: Die Kristallstrukturen der Hydrate NaOH · 3,5H2O (Raumgruppe P21/c, Z = 8 Formeleinheiten pro Elementarzelle; Gitterkonstanten a = 6,481, b = 12,460, c = 11,681 Å, β = 104,12° bei -100°C) und NaOH · 7 H2O (P21/c, Z = 4; a = 7,344, b = 16,356, c = 6,897 Å, β = 92,91° bei -150°C) wurden mit MoKα-Diffraktometerdaten einer Zweitbestimmung unterzogen. Die erreichte Präzisierung der Strukturen, einschließlich der erstmaligen Lokalisierung auch der H-Atome, führte zu neuen Erkenntnissen bezüglich der H-Brücken. Insbesondere gibt es in beiden Hydraten eine solche Wechselwirkung vom seltenen Typ OH- · OH2, von einem OH--Ion zu einem H2O-Molekül, also mit dem OH--Ion als Protondonor.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200903
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    Neue Silicate mit „Stuffed Pyrgoms“: CsKNaLi9{Li[SiO4]}4, CsKNa2Li8{Li[SiO4]}4, RbNa3Li8{Li[SiO4]}4 [1] und RbNaLi4{Li[SiO4]}2 [2]Professor Horst Sabrowsky zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1495-1508 
    Details
    ISSN: 0044-2313
    Keywords: New Lithosilicates ; preparation ; crystal structure ; MAPLE and CHARDI calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: More Silicates with „Stuffed Pyrgoms“: CsKNaLi9{Li[SiO4]}4, CsKNa2Li8{Li[SiO4]}4, RbNa3Li8{Li[SiO4]}4 [1] and RbNaLi4{Li[SiO4]}2 [2]Single crystals of the new silicates CsKNaLi9{Li[SiO4]}4, CsKNa2Li8{Li[SiO4]}4, RbNa3Li8{Li[SiO4]}4 and RbNaLi4{Li[SiO4]}2 as well as powder (Rb-containing compounds only) were obtained for the first time. The samples were prepared by heating well ground mixtures of the binary oxides in Ni and Ag tubes, respectively. The structure determination was carried out by four-circle diffractometer data (MoKα radiation; Siemens AED 2):CsKNaLi9{Li[SiO4]}4: tetragonally prismatic crystals, light yellow; 726 I0(hkl), R = 4.4%, Rw = 2.8%; a = 1 102.0(6), c = 637.9(5) pm; Z = 2; space group I4/m; 2 CsO0.55 + Li4TlO4 + glas (560°C, 15 d).CsKNa2Li8{Li[SiO4]}4: tetragonally prismatic crystals, light yellow; 727 I0(hkl), R = 4.4%, Rw = 2.6%; a = 1 103.5(7), c = 637.7(4) pm; Z = 2; space group I4/m; 1.1 CsO0.61 + 1.1 KO0.55 + 1.4 NaO0.52 + 6.5 Li2O + 4 SiO2 (600°C, 60 d).RbNa3Li8{Li[SiO4]}4: tetragonally prismatic crystals, colourless; 600 I0(hkl), R = 2.3%, Rw = 2.0%; a = 1 092.08(6), c = 632.76(4) pm; Z = 2; space group I4/m; 4 RbO0.57 + 3 NaO0.52 + 6.5 Li2O + 4 SiO2 (650°C, 63 d).RbNaLi4{Li[SiO4]}2: monoclinic, ball-shaped, colourless; 1 224 I0(hkl), R = 3.1%, Rw = 3.1%; a = 1 573.10(13), b = 630.48(5), c = 781.25(8) pm, b = 90.566(8)°; Z = 4; space group C2/m; 1.1 RbO0.52 + 1.2 NaO0.45 + 5 Li2O + 4 SiO2 (700°C, 40 d).
    Notes: Einkristalle der neuen Silicate CsKNaLi9{Li[SiO4]}4, CsKNa2Li8{Li[SiO4]}4, RbNa3Li8{Li[SiO4]}4 und RbNaLi4{Li[SiO4]}2, sowie Pulver der Rb-haltigen Verbindungen wurden dargstellt. Die Proben entstanden durch Tempern inniger Gemenge binärer Oxide in geschlossenen Ni- bzw. Ag-Bömbchen. Die Strukturaufklärung erfolgte jeweils durch Vierkreisdiffraktometerdaten (MoKα-Strahlung; Siemens AED 2):CsKNaLi9{Li[SiO4]}4: tetragonale Prismen, hellgelb; 726 I0(hkl), R = 4,4%, Rw = 2,8%; a = 1 102,0(6), c = 637,9(5) pm; Z = 2; Raumgruppe I4/m; 2 CsO0,55 + LiTlO4 + Duran-Glas (560°C, 15 d).CsKNa2Li8{Li[SiO4]}4: tetragonale Prismen, hellgelb; 727 I0(hkl), R = 4,4%, Rw = 2,6%; a = 1 103,5(7), c = 637,7(4) pm; Z = 2; Raumgruppe I4/m; 1,1 CsO0,61 + 1,1 KO0,55 + 1,4 NaO0,52 + 6,5 Li2O + 4 SiO2 (600°C, 60 d).RbNa3Li8{Li[SiO4]}4: tetragonale Prismen, farblos; 600 I0(hkl), R = 2,3%, Rw = 2,0%; a = 1 092,08(6), c = 632,76(4) pm; Z = 2; Raumgruppe I4/m; 4 RbO0,57 + 3 NaO0,52 + 6,5 Li2O + 4 SiO2 (650°C, 63 d).RbNaLi4{Li[SiO4]}2: monoklin, kugelförmig, farblos; 1 224 I0(hkl), R = 3,1%, Rw = 3,1%; a = 1 573,10(13), b = 630,48(5), c = 781,25(8) pm, b = 90,566(8)°; Z = 4; Raumgruppe C2/m; 1,1 RbO0,52 + 1,2 NaO0,45 + 5 Li2O + 4 SiO2 (700°C, 40 d)
    Additional Material: 17 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200902
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    Cs[Er10(C2)2]I18 und [Er10(C2)2]Br18: zwei neue Beispiele für „reduzierte“ Halogenide der Lanthanide mit isolierten [M10(C2)2]-Clustern (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1532-1536 
    Details
    ISSN: 0044-2313
    Keywords: Erbium Clusters, [Er10(C2)2] ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cs[Er10(C2)2]I18 and [Er10(C2)2]Br18: Two New Examples for Reduced Halides of the Lanthanides with Isolated [M10(C2)2] ClustersCs[Er10(C2)2]I18 is obtained from the reaction of ErI3 with caesium and carbon in sealed tantalum containers at 700°C and [Er10(C2)2]Br18 through the metallothermic reduction of ErBr3 with rubidium in the presence of carbon at 750°C in sealed niobium containers. The crystal structures {Cs[Er10(C2)2]I18: triclinic, P1; a = 1 105.2(8) pm, b = 1 112.0(7) pm; c = 1 122.9(8) pm; α = 66.91(3)°, β = 87.14(3)°; γ = 60.80(3)°; Z = 1; R = 0.049, Rw = 0.043; [Er10(C2)2]Br18: monoclinic, P21/n, a = 971.8(6) pm, b = 1 623.4(9) pm, c = 1 163.8(6) pm, β = 104.00(6)°; Z = 2; R = 0.077, Rw = 0.057} contain isolated dimeric [Er10(C2)2] clusters. Due to the inclusion of C2 units, the octahedra are elongated in the direction of the pseudo C4 axis. The connecting edges of the two octahedra are exceptionally short (316.7 pm and 314.8 pm respectively). The dimeric units are connected via Xi-a and Xa-i (X = Br, I) bridges according to [Er10(C2)2X10iX8/2i-a]X8/2a-i. Cs+ is surrounded by a cuboctahedron of iodide ions in Cs[Er10(C2)2]I18.
    Notes: Cs[Er10(C2)2]I18 entsteht bei der Umsetzung von Erl3 mit Caesium und Kohlenstoff in verschweißten Tantalampullen bei 700°C, [Er10(C2)2]Br18 bei der metallothermischen Reduktion von ErBr3 mit Rubidium in Gegenwart von Kohlenstoff bei 750°C in verschweißten Niobampullen. Die Kristallstrukturen {Cs[Er10(C2)2]I18: triklin, P1; a = 1 105,2(8) pm; b = 1 112,0(7) pm; c = 1 122,9(7) pm; α = 66,91(3)°; β = 87,14(3)°; γ = 60,80(3)°; Z = 1; R = 0,049, Rw = 0,043; [Er10(C2)2]Br18: monoklin, P21/n; a = 971,8(6); b = 1 623,4(9); c = 1 163,8(6); β = 104,00(6)°; Z = 2; R = 0,077, Rw = 0,057} beinhalten isolierte dimere [Er10(C2)2]-Cluster. Wegen des Einbaus der C2-Hantel sind die Oktaeder entlang ihrer pseudovierzähligen Achse gestreckt. Die verknüpfenden Oktaederkanten weisen einen besonders kurzen Metall-Metall-Abstand auf (316,7 bzw. 314,8 pm). Die dimeren Einheiten sind über Xi-a bzw. Xa-i-Brücken (X = Br, I) miteinander verknüpft, gemäß [Er10(C2)2X10iX8/2i-a]X8/2a-i. Cs+ ist in Cs[Er10(C2)2]I18 kuboktaederisch von Iodidionen umgeben.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200907
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  • 81
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    Ein weiteres Alkali-Erdalkalimetall-Oxoniccolat mit Perowskitstruktur: Sr12NaNi7O23 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1565-1568 
    Details
    ISSN: 0044-2313
    Keywords: Strontium, sodium, nickel, oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Another Alkaline Alkaline-Earth Oxoniccolate of Perovskite Type Structure: Sr12NaNi7O23Single Crystals of Sr12NaNi7O23 were prepared in closed system by Na2O2 flux reaction. X-ray single crystal work show hexagonal symmetry, space group D32-P321, a = 9.429, c = 7.896 Å, Z = 1. Sr12NaNi7O23 is strongly related to the stackered perovskites containing consequently face shared Ni2O9 double octahedra and Na+ inside a trigonal prismatic coordination by oxygen. One underoccupied oxygen point position decreases the coordination number of one Ni3+ of the Ni2O9 groups and a second surrounded by trigonal prisms to corner connected Ni2O7 double tetrahedra. The crystal chemistry will be discussed with respect to compounds of the same structure.
    Notes: Einkristalle von Sr12NaNi7O23 wurden im geschlossenen System mit Na2O2 als Schmelzmittel dargestellt. Röntgenographische Untersuchungen zeigen hexagonale Symmetrie, Raumgruppe D32-P321; a = 9,429; c = 7,896 Å, Z = 1. Sr12NaNi7O23 ist eng mit den Stapelvarianten der Perowskite verwandt und zeigt flächenverknüpfte Ni2O9-Oktaederdoppel sowie Na+ in einer trigonal prismatischen Koordination von Sauerstoff. Eine unterbesetzte Sauerstofflage erniedrigt die Koordinationszahl von einem Ni3+-Ion in den Ni2O9-Gruppen und von einem weiteren in trigonal prismatischer Koordination. Es entstehen eckenverknüpfte Ni2O7- Doppeltetraeder. Die Kristallchemie wird mit Blick auf Verbindungen vom gleichen Strukturtyp diskutiert.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200912
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  • 82
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    Ein neues Kupferzinnboratoxid mit isolierten BO3-Baugruppen: Cu5Sn(BO3)2O4 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1578-1582 
    Details
    ISSN: 0044-2313
    Keywords: Copper, tin, borate, oxide ; synthesis ; crystal structure ; X-ray diffraction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On a New Copper Tin Borate Oxide with Isolated BO3 Units: Cu5Sn(BO3)2O4Single Crystals of the new compound Cu5Sn(BO3)2O4 were obtained by a B2O3 fluxtechnique. They crystallize in a monoclinic distorted variant of a Ludwigite structure with a partly ordered metal distribution. X-ray investigations on single crystals led to the space group C2h5-P21/c (No. 14); a = 6.3526(7); b = 9.502(1); c = 12.100(9) Å; β = 93.30(3)°; Z = 4. All metal-sites are distorted octahedraly coordinated by oxygen-ions. The structure contains BO3-units and oxygen which is not coordinated to boron.
    Notes: Aus einer B2O3-Schmelze gelang die Synthese von Einkristallen der Substanz Cu5Sn(BO3)2O4, die in einer monoklin verzerrten Strukturvariante eines Ludwigites mit weitgehend geordneter Metallverteilung kristallisiert. Röntgenographische Untersuchungen an Einkristallen ergeben die Raumgruppe C2h5-P21/c (Nr. 14); a = 6,3526(7); b = 9,502(1); c = 12,100(9) Å; β = 93,30(3)°; Z = 4. Die Metallkationen sind verzerrt oktaedrisch von Sauerstoffionen koordiniert. Die Struktur weist sowohl isolierte, planare BO3-Baugruppen als auch nicht an Bor gebundenen Sauerstoff auf.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200914
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  • 83
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    Metall-Koordinationsverbindungen aus Essigsäure. I Chlorometallate(III) des Eisens, Chroms und VanadiumsProfessor Heinrich Oppermann zum 60. Geburtstag gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1943-1946 
    Details
    ISSN: 0044-2313
    Keywords: Ternary chlorometalates(III) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Metal Coordination Compounds Prepared in Acetic Acid. I. Chlorometalates(III) of Iron, Chromium, and VanadiumTernary chloride-hydrates A2MCl5 · H2O (A = Cs, Rb, (K)) can be precipitated with HCl from solutions of MCl3 · 6 H2O, (M = Fe, Cr, V) and alkali metal acetates in acetic acid. Under special conditions also compounds of the composition Cs3MCl6 · H2O can be obtained. After dehydration of the solutions with acetyl chloride, anhydrous compounds are formed: Cs3Fe2Cl9; A3CrCl6 and A3Cr2Cl9 with A = Cs, Rb; Cs3VCl6 and Cs3V2Cl9. VIII is partially oxidized to VIV by an excess of acetyl chloride. Compounds A2VCl6 with A = Cs, Rb can be obtained more conveniently by the reaction of VOCl2 · H2O in acetic acid with acetyl chloride.The lattice parameters of some compounds were determined from powder patterns in analogy to known structure families.
    Notes: Aus Lösungen der Chloridhydrate MCl3 · 6 H2O (M = Fe, Cr, V) in Eisessig lassen sich nach Zugabe von Alkalimetallacetaten mit HCl ternäre Chloridhydrate A2MCl5 · H2O (A = Cs, Rb, z. T. K), unter speziellen Bedingungen auch Verbindungen der Zusammensetzung Cs3MCl6 · H2O fällen. Werden die Ausgangslösungen mit Acetylchlorid dehydratisiert, so entstehen wasserfreie Chlorometallate(III): Cs3Fe2Cl9; A3CrCl6 und A3Cr2Cl9 mit A = Cs, Rb; Cs3VCl6 und Cs3V2Cl9. Vanadium(III) kann teilweise zu VIV oxidiert werden. Chlorovanadate A2VCl6 mit A = Cs, Rb lassen sich aber günstiger aus Lösungen von VOCl2 · 2 H2O in Eisessig mit Acetylchlorid erhalten.Von einigen strukturell noch nicht untersuchten Verbindungen sind durch Analogindizierungen von Pulveraufnahmen die Gitterparameter bestimmt worden.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19946201118
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  • 84
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    Synthese und Struktur von Li3RhH6, einem ternären Hydrid mit isolierten [RhH6]3--OktaedernProfessor Heinrich Oppermann zum 60. Geburtstag gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1983-1985 
    Details
    ISSN: 0044-2313
    Keywords: Metal hydrides ; rhodium ; lithium ; crystal structure ; neutron diffraction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of Li3RhH6  -  a Ternary Hydride with Isolated [RhH6]3- OctahedraThe ternary rhodium hydride Li3RhH6 was synthesized by the reaction of lithium hydride with rhodium under a hydrogen pressure of 80 bar. X-ray investigations on powdered samples and an elastic neutron diffraction experiment on the deuterated compound led to the complete structure determination (space group: Pnma, Z = 4). The atomic arrangement is isotypic to the Na3RhH6 structure type. The crystal structure contains isolated [RhH6]3- octahedra, which are separated by the lithium ions.
    Notes: Die Synthese von Li3RhH6 gelingt durch Umsetzung von Lithiumhydrid mit feinverteiltem Rhodium unter einem Wasserstoffdruck von 80 bar. Röntgenographische Untersuchungen an pulverförmigen Proben und ein elastisches Neutronenbeugungsexperiment an der deuterierten Verbindung führten zur Strukturaufklärung (Raumgruppe: Pnma, Z = 4). Die Verbindung ist isotyp zu der von Na3RhH6 und enthält isolierte [RhH6]3--Oktaeder, die durch die Lithiumionen separiert werden.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201124
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  • 85
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    Structural investigations and luminescence of In2Ge2O7 and In2Si2O7Dedicated to Professor Heinrich Oppermann on his 60th Birthday (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1965-1970 
    Details
    ISSN: 0044-2313
    Keywords: Indium digermanate ; indium disilicate ; crystal structure ; indium luminescence ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Strukturuntersuchungen und Lumineszenz von In2Ge2O7 und In2Si2O7Eine Rietveld-Pulverdiagramm-Methode erlaubt die Bestimmung der genauen Strukturen von Thortveitit verwandten In2Ge2O7 und In2Si2O7 Oxyden (Raumgrupe C2/m, Z = 2). Die Verbindungen wurden unter normalem Druck hergestellt. Die Lumineszenz unter 160 und 200 K sollte die Messung der Umwelt Neutrinobestrahlung erlauben. Sie scheint die Folge eines inneren Ladungstransfers in den Indium Sauerstoff Polyedern zu sein. Die optischen Resultate wurden an Hand der bestimmten Strukturen und der chemischen Bindungen diskutiert und mit Werten für andere Indiumoxyde verglichen.
    Notes: The crystal structures of the ordinary pressure forms of indium digermanate In2Ge2O7 and disilicate In2Si2O7 have been studied from X-ray powder diffraction data by Rietveld refinement. They are closely related to that of the thortveitite which crystallizes in the monoclinic system with the space group C2/m and Z = 2. They show luminescence properties below 160 K and 200 K respectively. The luminescence is discussed in terms of crystal structure and compared to that of some other luminescent indium oxides.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201121
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  • 86
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    Tellur-Polykationen stabilisiert durch Nioboxidhalogenide: Synthese und Kristallstrukturen von Te7NbOBr5 und Te7NbOCl5Professor Heinrich Oppermann zum 60. Geburtstag gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1971-1975 
    Details
    ISSN: 0044-2313
    Keywords: Tellurium ; niobium oxytrihalides ; poly(heptatellurium(2+)) ; tetrachlorooxoniobate (1-) ; tetrabromooxoniobate (1-) ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tellurium Cations stabilized by Niobium Oxytrihalides: Synthesis and Crystal Structure of Te7NbOBr5 and Te7NbOCl5The reaction of Te2Br with NbOBr3 in a sealed evacuated glass ampoule at 225°C yields Te7NbOBr5 in form of bright black needles. Te7NbOCl5 is obtained from tellurium, TeCl4 and NbOCl3 at 220°C. Both compounds crystallize orthorhombic in the space group Pcca (Te7NbOBr5: a = 2 651,9(4) pm, b = 836.6(1) pm, c = 794.6(1) pm; Te7NbOCl5: a = 2 597.7(5) pm, b = 805.1(1) pm, c = 791.2(1) pm). The crystal structure determinations show that Te7NbOBr5 and Te7NbOCl5 are built of one-dimensional polymeric tellurium cations, one-dimensional associated pyramidal NbOX4 groups (X = Cl, Br) and isolated halide anions. Magnetic properties of Te7NbOX5 were determined and confirm the expected diamagnetism. Te7NbOX5 can thus be formulated as ∞1[Te72+] ∞1[NbOX4-] (X-). The charge distribution in the structure type Te7MOX5 (M = W, Nb; X = Cl, Br) became clear by synthesis and characterisation of the two niobium containing compounds.
    Notes: Durch Reaktion von Te2Br mit NbOBr3 in einer evakuierten Glasampulle bei 225°C entsteht Te7NbOBr5 in Form von schwarzglänzenden, stäbchenförmigen Kristallen. Te7NbOCl5 wird aus Te, TeCl4 und NbOCl3 bei 220°C erhalten. Beide Verbindungen kristallisieren im orthorhombischen Kristallsystem in der Raumgruppe Pcca (Te7NbOBr5: a = 2 651,9(4) pm, b = 836,6(1) pm, c = 794,6(1) pm; Te7NbOCl5: a = 2 597,7(5) pm, b = 805,1(1) pm, c = 791,2(1) pm). Die Kristallstrukturanalysen zeigen, daß Te7NbOBr5 und Te7NbOCl5 aus eindimensionalen polymeren Tellur-Kationen, eindimensionalen Strängen von pyramidalen, über O-Atome assoziierten NbOX4-Einheiten und aus isolierten Halogenidionen aufgebaut sind. Magnetische Messungen bestätigen den erwarteten Diamagnetismus und zeigen, daß Nb in der formalen Oxidationsstufe + V vorliegt. Die ionische Schreibweise lautet daher ∞1[Te72+] ∞1[NbOX4-] (X-). Die Synthese und Charakterisierung der beiden niobhaltigen Vertreter klärt die Ladungsverteilung im Strukturtyp Te7MOX5 (M = W, Nb; X = Cl, Br).
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201122
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  • 87
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    Structure of trichosanthin at 1.88 Å resolution (1994)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 19 (1994), S. 4-13 
    Details
    ISSN: 0887-3585
    Keywords: trichosanthin ; ribosome-inactivating proteins ; crystal structure ; orthorhombic ; molecular replacement ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Trichosanthin (TCS) is one of the single chain ribosome-inactivating proteins (RIPs). The crystals of the orthorhombic form of trichosanthin have been obtained from a citrate buffer (pH 5.4) with KC1 as the precipitant. The crystal belongs to the space group P212121 with a = 38.31, b = 76.22, c = 79.21 Å. The structure was solved by molecular replacement method and refined using the programs XPLOR and PROLSQ to an R-factor of 0.191 for the reflections within the 6-1.88 Å resolution range. The bond length and bond angle in the protein molecule have root-mean-square deviations from ideal value of 0.013 Å and 3.3°, respectively. The refined model includes 247 residues and 197 water molecules. The TCS molecule consists of two structural domains. The large domain contains six α-helices, a six stranded sheet, and an antiparallel β-sheet. The small domain has a largest α-helix, which shows a distinct bend. The possible active site of the molecule located on the cleft between two domains was proposed. In the active site Arg-163 and Glu-160, Glu-189 and Arg-122 form two ion pairs, Glu-189 and Gln-156 are hydrogen bonded to each other. Three water molecules are bonded to the residues in the active site region. The structures of TCS molecule and ricin A-chain (RTA) superimpose quite well, showing that the structures of the two protein molecules are homologous. Comparison of the structures of the TCS molecule in this orthorhombic crystal with that in the monoclinic crystal indicates that there are no essential differences of the structures between the two protein crystals. © 1994 Wiley-Liss, Inc.
    Additional Material: 10 Ill.
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    URL: http://dx.doi.org/10.1002/prot.340190103
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  • 88
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    Cold adaption of enzymes: Structural comparison between salmon and bovine trypsins (1994)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 20 (1994), S. 149-166 
    Details
    ISSN: 0887-3585
    Keywords: crystal structure ; cold adaption ; catalytic efficiency ; protein stability ; anionic ; ectotherm ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The crystal structure of an anionic form of salmon trypsin has been determined at 1.82 Å resolution. We report the first structure of a trypsin from a phoikilothermic organism in a detailed comparison to mammalian trypsins in order to look for structural rationalizations for the cold-adaption features of salmon trypsin. This form of salmon trypsin (T II) comprises 222 residues, and is homologous to bovine trypsin (BT) in about 65% of the primary structure. The tertiary structures are similar, with an overall displacement in main chain atomic positions between salmon trypsin and various crystal structures of bovine trypsin of about 0.8 Å. Intramolecular hydrogen bonds and hydrophobic interactions are compared and discussed in order to estimate possible differences in molecular flexibility which might explain the higher catalytic efficiency and lower thermostability of salmon trypsin compared to bovine trypsin. No overall differences in intramolecular interactions are detected between the two structures, but there are differences in certain regions of the structures which may explain some of the observed differences in physical properties. The distribution of charged residues is different in the two trypsins, and the impact this might have on substrate affinity has been discussed. © 1994 Wiley-Liss, Inc.
    Additional Material: 10 Ill.
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    URL: http://dx.doi.org/10.1002/prot.340200205
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  • 89
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    Analysis of structure and properties of poly(ethylene terephthalate) fibers (1994)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 32 (1994), S. 2289-2306 
    Details
    ISSN: 0887-6266
    Keywords: poly(ethylene terephthalate) ; fiber ; x-ray diffraction ; crystal structure ; three-phase model ; modulus ; tenecity ; shrinkage ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The structure of four semicrystalline poly(ethylene terephthalate) fibers were analyzed with full-pattern (two-dimensional Rietveld) x-ray diffraction refinement, small-angle x-ray scattering, and thermal mechanical analysis, and compared to some of their known mechanical properties. The classical two-phase model of crystal and amorphous phases were unable to correlate structure and properties. We found that there must be a third phase, an oriented, intermediate phase, located mainly between the fibrils. About 1/3 of the intensity of fiber diffraction of the analyzed samples was contributed from such intermediate phase. For some fiber properties the intermediate phase plays a similar role as proposed for “taut tie molecules.” A simple model for the description of structure-insensitive properties of PET fibers was developed, based on this quantitaitve separation into three phases. The oriented intermediate phase changes the definition and calculation of the basic parameters of the fiber structure, such as crystallinity and orientation. Based on small-angle x-ray evidence, the crystallites are assumed to be separated by layers of largely amorphous material, both surrounded by the intermediate phase. The initial modulus of the fiber is determined mainly by the amount and orientation of the intermediate phase which has a maximum modulus of about 500 g/d on full orientation instead of the earlier predicted 150 g/d for fully oriented semicrystalline fibers. Based on the relationship between tenactity and average orientation function, the maximum tenacity for PET fibers of a structure like the ones analyzed may reach 20-45 g/d instead of earlier predictions of 10 g/d. The additional information needed to understand the structure-sensitive property of shrinkage is discussed. Presently easily accessible parameters have no quantitative predictive capabilities. © 1994 John Wiley & Sons, Inc.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/polb.1994.090321316
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  • 90
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    Surface studies of tetraalkylammonium bromides and iodides using atomic force microscopy (1994)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 32 (1994), S. 2653-2659 
    Details
    ISSN: 0887-6266
    Keywords: tetraalkylammonium halide ; atomic force microscopy ; crystal structure ; surface structure ; hextriacontane ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The surface structures of two series of tetra-n-alkylammonium halides, N(CxH2×+1)4I and N(CxH2x+1)4 Br have been investigated with atomic force microscopy (AFM) and compared to hexatriacontane (C36H74). The surfaces could be imaged with atomic resolution. The observed primitive, square surface-patterns of tetra-n-butyl chloride and bromide are in good accord with x-ray single-crystal structure. For n 〉 4, x-ray powder diffraction showed that increasing the alkyl chain-length leads mainly to an appropriate increase of the unit cell along the c-axis, which suggests similar layer structures for all long-chain salts beyond the butyl homologue. Within the centers of the molecular layers of these crystals reside the halide anions and the quaternary nitrogens. The surfaces accessible for AFM consist of methyl end-groups. As the number of carbon atoms increases beyond four, the surface symmetry changes to the face-centered square patterns characteristic of many paraffins. The chains of the tetraalkyl ammonium salts pack, however, less dense than paraffins. © 1994 John Wiley & Sons, Inc.
    Additional Material: 9 Ill.
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    URL: http://dx.doi.org/10.1002/polb.1994.090321611
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  • 91
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    Synthese und Strukturbestimmung von (i-Pr)2NB(t-BuP)3 und (i-Pr)2NB(t-BuP)4Professor Ernst-Otto Fischer zum 75. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 8-15 
    Details
    ISSN: 0044-2313
    Keywords: P3B and P4B ring systems ; NMR data ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure Analysis of (i-Pr)2NB(t-BuP)3 and (i-Pr)2NB(t-BuP)4The diphosphide K(t-Bu)P-(t-BuP)2-P(t-Bu)K obtained by the cleavage reaction of the 3-membered ring system (i-Pr)2BN(t-BuP)2 with potassium reacts with t-BuPCl2 at -78°C under ring expansion to form the P3B ring system (i-Pr)2NB(t-BuP)3 - 1,2,3-tri-t-butyl-tri-phospha-4-diisopropyl-aminoboretane (1). - The 5-membered P4B ring system (i-Pr)2NB(t-BuP)4 - 1,2,3,4-tetra-t-butyl-tetraphospha-5-diisopropylaminoborolidine, (2) - is formed from K(t-Bu)P—(t-BuP)2—P(t-Bu)K and (i-Pr)2NBCl2 analogous to the above reaction. 1 and 2 could be obtained in a pure form and characterized NMR spectroscopically and by X-ray structure analysis. 1 shows at 200 K two conformation isomers; for 2 31P-10,11B-isotopic shifts could be identified.
    Notes: Das bei der Spaltung des Dreiringes (i-Pr)2BN(t-BuP)2 mit Kalium gebildete Diphosphid K(t-Bu)P—BN(i-Pr)2—P(t-Bu)K reagiert bei -78°C mit t-BuPCl2 unter Ringerweiterung zu (i-Pr)2NB(t-BuP)3-1,2,3-Tri-t-butyl-triphospha-diisopropyl-aminoboretan, (1) - mit einem P3B-Ringgerüst. In analoger Weise entsteht bei der Reaktion zwischen K(t-Bu)P—(t-BuP) - (t-BuP)2—P(t-Bu)K und (i-Pr)2NBCl2 das P4B-Ringsystem (i-Pr)2NB(t-BuP)4 - 1,2,3,4-Tetra-t-butyl-tetraphospha-5-diiso-propylaminoborolidin, (2) -, 1 und 2 konnten in reiner Form isoliert, NMR-spektroskopisch und durch Röntgenstrukturanalysen charakterisiert werden. 1 zeigt bei 200 K zwei Konformationsisomere; bei 2 konnten 31P-10,11B-Isotopieverschiebungen nachgewiesen werden.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200104
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  • 92
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    Electronic Resource
    Darstellung und Kristallstruktur von NaBi2AuO5 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 48-52 
    Details
    ISSN: 0044-2313
    Keywords: Alkali bismuth gold oxide ; preparation ; 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 NaBi2AuO5NaBi2AuO5 was obtained by hydrothermal reaction of ‘Bi2O5’, Au2O3 · 2H2O and saturated aqueous NaOH solution at temperatures from 300 to 600°C and oxygen pressure from 3 × 108 to 6 × 108 Pa for the first time. The crystal structure (P4b2; a = 1 220.02(6) pm; b = 386.68(3) pm; Z = 4; Rw = 0.022) consists of bisphenoidic distorted AuO4 groups, which are stacked in c-direction. They are connected by square pyramidal BiO5 units. Sodium is occupying holes within the Au/Bi/O framework thus formed.
    Notes: NaBi2AuO5 wurde durch Hydrothermalreaktion aus ‘Bi2O5’, Au2O3 · 2H2O und ges. wäßriger NaOH bei Temperaturen von 300 bis 600°C und Sauerstoffdrucken von 3 · 108 bis 6 · 108 Pa erstmals dargestellt. Nach den Ergebnissen der Röntgenstrukturanalyse (P4b2, a = 1 220,02(6); b = 386,68(3) pm; Z = 4; Rw = 0,022) liegen bisphenoidisch verzerrte AuO4-Gruppen vor, die in c-Richtung gestapelt sind. Die Verknüpfung erfolgt über quadratisch pyramidale BiO5-Baueinheiten. In dieser Raumnetzstruktur besetzt Natrium die vorhandenen Lücken.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200108
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  • 93
    Electronic Resource
    Electronic Resource
    Neue Rheniumkomplexe mit Trichalkogenido- und Tetrachalkogenido-Chelatliganden (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 299-303 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium complexes ; rhenium trichalcogenido, -tetrachalcogenido complexes ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Rhenium Complexes Containing Trichalcogenido and Tetrachalcogenido Chelate LigandsThe reactions of Cp*ReCl4 with polychalcogenide salts such as Na2S4 or (NEt4)2Se6 lead initially to the violet trichalcogenido chelate complexes Cp*ReCl2(E3) (E = S (3a), Se (3b)) which, due to their functional chloro ligands, can be used as intermediates for further reactions. Upon hydrolysis in moist solvents or aminolysis with tert. butylamine 3a, b are converted into the tetrachalcogenido chelate complexes Cp*Re(O)(E4) (E = S (4a), Se (4b)) and Cp*Re(NtBu)(E4) (E = S (5a), Se (5b)), respectively. X-Ray structure analyses were carried out for the three mononuclear cyclo-oligoselenido compounds 3b-5b. It appears that the size of the Se2-n chelate ring (n = 3 or 4) essentially depends on steric factors within the coordination sphere of rhenium.
    Notes: Die Reaktionen von Cp*ReCl4 mit Polychalkogenid-Salzen wie Na2S4 oder (NEt4)2Se6 führen zunächst zu den violetten Trichalkogenido-Chelatkomplexen Cp*ReCl2(E3) (E = S (3a), Se (3a), die aufgrund der funktionellen Chloroliganden als Zwischenstufen bei weiteren Reaktionen verwendet werden können. Bei Hydrolyse in feuchten Solvenzien oder Aminolyse mit tert. Butylamin werden 3a, b in die Tetrachalkogenido-Chelatkomplexe Cp*Re(O)(E4) (E = S (4a), Se (4b) bzw. Cp*Re(NtBu)(E4) (E = S (5a), Se (5b) umgewandelt. Für die drei einkernigen cyclo-Oligoselenido-Verbindungen 3b-5b wurden Röntgenstrukturanalysen durchgeführt. Es scheint, daß die Größe des Se2-n-Chelatrings (n = 3 oder 4) im wesentlichen von sterischen Faktoren innerhalb der Koordinationssphäre des Rheniums abhängt.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200214
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  • 94
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstruktur von Ba25Cu142+Cu43+Zn4O49 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 313-318 
    Details
    ISSN: 0044-2313
    Keywords: Barium, copper, zinc, 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 Ba25Cu142+Cu43+Zn4O49Single crystals of Ba25Cu142+Cu43+Zn4O49 were prepared with solid state and flux reactions. X-ray investigations show tetragonal symmetry, space group D74th-P4/nmm, a = 18.2146, c = 9.3230 Å, Z = 2. The hitherto unknown structure type shows copper in square pyramids and planar polygones, connected to six member rings or Cu5O20 groups. Slightly bent Cu5O12 groups produced by edge connection of five CuO4 polygones are connected with ZnO4 tetrahedra forming Cu5Zn4O20 units. The complicated structure is shown step by step.
    Notes: Einkristalle von Ba25Cu142+Cu43+Zn4O49 wurden mit einer Kombination von Feststoff- und Schmelzmittel-reaktionen dargestellt. Diese Substanz kristallisiert tetragonal, Raumgruppe D74th-P4/nmm mit a = 18,2146, c = 9,3230 Å, Z = 2. Der bisher unbekannte Strukturtyp zeigt Kupfer in tetragonal pyramidaler und planarer Koordination. Diese Polygone sind zu Sechsringen oder Cu5O20-Baugruppen verknüpft. Schwach gebogene Cu5O12-Baugruppen, die durch Kantenverknüpfung von fünf planaren CuO4-Polygonen gebildet werden, sind mit ZnO4-Tetraedern verknüpft und bilden Cu5Zn4O20-Baueinheiten aus. Die komplizierte Kristallstruktur wird schrittweise aufgebaut.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200217
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  • 95
    Electronic Resource
    Electronic Resource
    Crystal Structure of a New Acentric Oxide Fluoride of VIV: BaVOF4 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 309-312 
    Details
    ISSN: 0044-2313
    Keywords: Barium vanadium oxide fluoride ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kristallstruktur eines neuen azentrischen Oxidfluorids des VIV: BaVOF4Die Struktur von BaVOF4, erhalten durch hydrothermale Synthese, wurde röntgendiffraktometrisch aus Einkristalldaten bestimmt: Raumgruppe Fdd2 (azentrisch), Z = 16, a = 7,920(1), b = 27,608(2), c = 7,375(1) Å mit R = 0,0262, Rw = 0,0273 für 1 508 unabhängige Reflexe und 64 Parameter. Das Gitter wird von cis-verknüpften VOF5-Oktaedern aus gewinkelten unendlichen Ketten entlang [101] und [101] gebildet, die über Barium-Kationen verbunden sind. Die Lage der O2- und F- wird mittels Valenzband-Rechnungen diskutiert. Wie für BaTiOF4 und einige Verbindungen aus der Reihe AIIMIIIF5 (A = Ba, Sr und M = Ga, Al, Mn) kann die Struktur durch quasi-hexagonal dichteste Ebenen aus Stapeln von Ba2+, O2-- und F--Ionen beschrieben werden.
    Notes: The structure of BaVOF4 has been determined by X-ray diffraction data from a single crystal obtained by hydrothermal synthesis: S.G. Fdd2 (acentric), Z = 16, a = 7.920(1), b = 27.608(2) and c = 7.375(1) Å with R = 0.0262 and Rw = 0.0273 for 1 508 independent reflections and 64 parameters. The network is built up from cis-linked VOF5 octahedra forming infinite kinked chains running along the [101] and [101] directions, connected by barium cations. The location of O2- and F- ions is discussed using bond valence calculations. As for BaTiOF4 and some compounds in the series AIIMIIIF5 (A = Ba, Sr and M = Ga, Al, Mn), the structure can be described in terms of a quasi hexagonal compact planes stacking of Ba2+, O2- and F- ions.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200216
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  • 96
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    Electronic Resource
    Ein Beitrag über ein cobaltreiches Oxoarsenat/-vanadat: Co5AsVO10 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 319-322 
    Details
    ISSN: 0044-2313
    Keywords: Cobalt, arsenic, nickel, oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Contribution about a New Cobalt-rich Oxoarsenate/-vanadate: Co5AsVO10Single crystals of Co5AsVO10 were prepared by solid state reactions and investigated by X-ray structure determination. It crystallizes with monoclinic symmetry, space group C2h3-C2/m, a = 19.134, b = 6.095, c = 17.482 Å, β = 133.37°; Z = 8. The new structure type is characterized by layers of CoO6- and AsO6-octahedra with partly alternating occupation. The layers are connected by Co2+ within tetrahedral oxygen coordination and tetrahedra around statistically occupied point positions of V5+ /As5+.
    Notes: Einkristalle von Co5AsVO10 wurden durch Feststoffreaktionen erhalten und röntgenographisch untersucht. Diese Verbindung kristallisiert mit monokliner Symmetrie, Raumgruppe C2h3-C2/m; a = 19,134; b = 6,095; c = 17,482 Å; β = 133,37°; Z = 8. Der neue Strukturtyp ist durch CoO6- und AsO6-Oktaederschichten ausgezeichnet, die teilweise alternierend mit Co2+ und As5+ besetzt sind. Die Oktaederschichten werden durch Co2+ in tetraedrischer Koordination und statistisch mit V5+ und As5+ besetzte Punktlagen verknüpft.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200218
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  • 97
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    Electronic Resource
    Einkristall-Röntgenstrukturanalyse von Sr3TiGa10O20 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 323-325 
    Details
    ISSN: 0044-2313
    Keywords: Strontium, titanium, gallium, oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Single Crystal X-Ray Analysis of Sr3TiGa10O20Single crystals of Sr3TiGa10O20 were prepared by recrystallisation of a molten oxide mixture and investigated by X-Ray technique. It crystallizes with monoclinic symmetry, space group C2h3-C2/m, a = 15.451, b = 11.579, c = 5.051 Å, β = 108.57°, Z = 2. Sr3TiGa10O20 belongs to the Pb3GeAl10O20 type, showing Ga3+ in tetrahedral and octahedral coordination. The octahedral coordinated point positions are occupied by Ga3+ and Ti4+ statistically.
    Notes: Einkristalle von Sr3TiGa10O20 wurden durch Rekristallisation aus Schmelzen erhalten und röntgenographisch untersucht. Diese Verbindung kristallisiert mit monokliner Symmetrie, Raumgruppe C2h3-C2/m, a = 15,451; b = 11,579; c = 5,051 Å; β = 108,57°; Z = 2. Sr3TiGa10O20 gehört zum Pb3GeAl10O20-Typ und zeigt Ga3+ in tetraedrischer und oktaedrischer Koordination. Die oktaedrisch koordinierten Punktlagen sind mit Ga3+ und Ti4+ statistisch besetzt.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200219
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  • 98
    Electronic Resource
    Electronic Resource
    On the Crystal Structure of LaCaCuGaO5 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 326-328 
    Details
    ISSN: 0044-2313
    Keywords: Lanthanum calcium copper gallate ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zur Kristallstruktur von LaCaCuGaO5Die Kristallstruktur von LaCaCuGaO5 wurde röntgenographisch an Einkristallen untersucht. Es kristallisiert orthorhombisch in der Raumgruppe C2v22-Ima2 mit a = 15,8467, b = 5,5077, c = 5,3188 Å, Z = 4. LaCaCuGaO5 gehört zum Brownmillerit-Typ und zeigt somit Schichten von eckenverknüpften CuO6-Oktaedern, die über GaO4-Tetraeder vernetzt sind. Die La3+- bzw. Ca2+-Ionen besetzen eine Punktlage statistisch.
    Notes: The crystal structure of LaCaCuGaO5 has been investigated by single crystal X-ray analysis. It crystallizes with orthorhombic symmetry, space group C2v22-Ima2, a = 15.8467, b = 5,5077, c = 5.3188 Å, Z = 4. LaCaCuGaO5 belongs to the mineral Brownmillerite showing layers of corner connected CuO6 octahedra linked by GaO4 tetrahedra. The La3+ and Ca2+ ions are distributed statistically over one crystallographic point position.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200220
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  • 99
    Electronic Resource
    Electronic Resource
    Darstellung und Struktur von Tetraethylcyclotetraarsoxan-Komplexen von Kupfer(I)-Halogeniden (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 334-342 
    Details
    ISSN: 0044-2313
    Keywords: Copper(I) halide complexes ; tetraethylcyclotetraarsoxane copper(I) complexes ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Structure of Tetraethylcyclotetraarsoxane Complexes of Copper(I) HalidesThe polymeric complexes [Cu4Cl4{cyclo-(C2H5AsO)4}3]n (1), [Cu3Br3{cyclo-(C2H5AsO)4}2]n (2) and [Cu6I6{cyclo-(C2H5AsO)4}3]n (3) were prepared by the reaction of (C2H5AsO)n and CuX (X = Cl, Br, I) in acetonitrile and characterised by X-ray analysis. All three complexes contain only tetramers (C2H5AsO)4 as ligands, in which the As4O4 ring systems coordinate between two and four Cu-atoms. In each case one As4O4 ring with a crown-shaped conformation is observed, which coordinates either four (in 1) or three (in 2 and 3) axially sited Cu-atoms. In addition there are further (C2H5AsO)4 ligands, which display either a boat-chair- (in 1) or a twist-chair-conformation (in 1-3). The individual building units are connected to one another via Cu—X—Cu bridges (in 2 and 3) and/or centrosymmetric As4O4 ring systems (in 1-3) into chain (1) or layer structures (2 und 3).
    Notes: Die polymeren Komplexe [Cu4Cl4{cyclo-(C2H5AsO)4}3]n (1), [Cu3Br3{cyclo-(C2H5AsO)4}2]n (2) und [Cu6I6{cyclo-(C2H5AsO)4}3]n (3) wurden durch die Umsetzung von (C2H5AsO)n und CuX (X = Cl, Br, I) in Acetonitril dargestellt und durch Röntgenstrukturanalyse charakterisiert. Alle drei Komplexe enthalten lediglich Tetramere (C2H5AsO)4 als Liganden, wobei die As4O4-Ringsysteme zwischen zwei und vier Cu-Atomen koordinieren. Es wird jeweils ein As4O4-Ring mit Kronenkonformation beobachtet, der entweder vier (in 1) oder drei (in 2 und 3) Cu-Atome axial koordiniert. Außerdem liegen weitere (C2H5AsO)4-Liganden in boat-chair- (in 1) oder twist-chair-Konformation (in 1-3) vor. Die einzelnen Baueinheiten werden über Cu—X—Cu-Brücken (in 2 und 3) und/oder zentrosymmetrische As4O4-Ringsysteme (in 1-3) zu Ketten-(1) oder Schichtstrukturen (2 und 3) verknüpft.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200222
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  • 100
    Electronic Resource
    Electronic Resource
    Über die Reaktion von Cp2TiCl2 mit [C(NMe2)3][(CO)4FeC(O)NMe2] - Kristallstruktur von [C(NMe2)3]2[FeCl4] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 343-345 
    Details
    ISSN: 0044-2313
    Keywords: Hexamethyl guanidinium cation ; tetrachloro iron(II) anion ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Concerning the Reaction of Cp2TiCl2 with [C(NMe2)3][(CO)4FeC(O)NMe2] - Crystal Structure of [C(NMe2)3]2[FeCl4]The title compound forms by the reaction of Cp2TiCl2 with [C(NMe2)3][(CO)4FeC(O)NMe2] in THF solution. It crystallizes in the space group Pbcn with a = 1 566.6(3); b = 976.4(2); c = 1 580.4(4) pm; Z = 4; R = 3.8%. Each [FeCl4]2- in is surrounded by eight cations. Two cations each are connected with one Cl atom by relatively short H … Cl contacts leading to a distortion of the tetrahedral geometry of the anion.
    Notes: Die Titelverbindung entsteht bei der Umsetzung von Cp2TiCl2 mit [C(NMe2)3][(CO)4FeC(O)NMe2] in THF-Lösung. Sie kristallisiert in der Raumgruppe Pbcn mit a = 1 566,6(3); b = 976,4(2); c = 1 580,4(4) pm; Z = 4; R = 3,8%. Jedes [FeCl4]2- Ion ist von acht Kationen umgeben. Je zwei Kationen sind über relativ kurze H … Cl Kontakte mit einem Cl-Atom verbunden, was zu einer Verzerrung der Tetraedergeometrie des Anions führt.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200223
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