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  • 2000-2004
  • 1990-1994  (128)
  • 1992  (128)
  • crystal structure  (128)
  • 1
    Electronic Resource
    Electronic Resource
    Reversible formation of an intramolecular agostic CH interaction in a dimanganese complex (1992)
    Springer
    Journal of cluster science 3 (1992), S. 103-108 
    Details
    ISSN: 1572-8862
    Keywords: Manganese ; agostic ; crystal structure ; CH activation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract Agostic interactions of CH bonds with metal atoms are currently of great interest. UV irradiation of Mn2(CO)8 (PMe2Ph)2 in the presence of the HC≡COEt yielded the new compound Mn2(CO)6(PMe2Ph)2 [μ-C(OEt)=C(H)C=C(H)C=O(OEt)],1 that contains a strong agostic interaction of an olefinic CH bond to one of the managanese atoms, Mn...C=2.349(5), Mn...H=2.01(4). This interaction can be removed (reversibly) by CO addition (25°C/1000 psi) to1 to yield the new complex Mn2(CO)7(PMe2Ph)2[μ-C(OEt)=C(H)C=C(H)C=O(OEt)],2.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00814614
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  • 2
    Electronic Resource
    Electronic Resource
    Further studies of M3(μ3-O)(μ-X)3(μ-O2CCH3)3L3 (M=Mo, W) type clusters with nine core electrons (1992)
    Springer
    Journal of cluster science 3 (1992), S. 123-144 
    Details
    ISSN: 1572-8862
    Keywords: Molybdenum ; tungsten ; crystal structure ; reduction ; acetate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract Four new compounds having nine cluster electrons and cores of the types Mo3OCl3, Mo3OBr3, and W3OCl3 are reported. Compound (1) prepared by reduction of [Bu4N][Mo3OCl6(OAc)3] in THF with metallic zinc, was shown by X-ray crystallography to be Mo3OCl4(OAc)3 (THF)2 (1). It forms crystals in space groupP21 with unit cell dimensionsa=9.472(2) Å,b=13.546(4) Å,c=9.652(2) Å, β=101.70(2)°,V=1201(1) Å3,Z=2. The [Mo3(μ3-O)(μ-Cl)3]4+ core is surrounded by three μ-O2CCH3 anions, one Cl−, and two THF and has Mo-Mo distances of 2.620(1) Å, 2.613(1) Å, and 2.530(1) Å, with the shortest bond between the two Mo atoms to which the THF molecules are coordinated. Compounds [Bu4N]2 [Mo3OBr6(O2CCH3)3] · Me2CO, (2) and [Mo3OBr3(O2CCH3)3(PMe3)3]3 · BF4, (3) are the first two nine-electron Mo3 species with a [Mo3(μ3-O) Br3]4+ core. Both were obtained by zinc reduction of [Mo3OBr6(O2CCH3)3]− in the presence of (NBu4) Br (2) or PMe3 and NaBF4 (3), and each was characterized crystallographically. Compound (2) crystallized in space group Cc with unit cell dimensionsa=25.037(5) Å,b=12.827(2) Å,c=21.484(4) Å, β=122.96(1)0,V=5790(3) Å3,Z=4. While the anion has no crystallographically required symmetry, its virtual symmetry is C3v . The Mo-Mo distances are 2.619(2) Å, 2.610(3) Å, 2.644(2) Å, with a mean value of 2.624[14] Å. Compound (3) crystallized in space groupP21/c with unit cell dimensionsa=10.846(2) Å,b=25.033(5) Å,c=12.641(5) Å, β=94.74(2)0,V=3420(2) Å3,Z=4. The cation occupies a general position but has virtual C3v symmetry, with Mo-Mo distances of 2.601(2) Å, 2.610(2) Å, 2.627(2) Å, with a mean value of 2.613[14] Å. Thus the anionic and cationic Mo3 clusters in (2) and (3), respectively, have average Mo-Mo distances that are equal within experimental error. Compound (4), [NEt4]2 [W3OCl6(O2CCH3)3] is the first 9-electron compound of this type containing tungsten. It was prepared by reduction of [Et4N][W3OCl6(OAc)3] in benzene with Na/Hg. It crystallized in space groupP212121 with unit cell dimensionsa=11.076(2) Å,b=14.345(2) Å,c=21.026(3) Å,V=3574(1) Å3,Z=4. The anion resides on a general position but has virtual C3v symmetry, with W-W distances of 2.577(1) Å, 2.612(1) Å, 2.584(1) Å and a mean value of 2.591[15] Å.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00702878
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  • 3
    Electronic Resource
    Electronic Resource
    Synthesis, structural characterization and bonding properties of heterometallic-heterobridging cubane-type tetranuclear cluster compounds [CuMo3OS3]·I·(μ-OAc)[S2P(OC2H5)2]3·L (L=py, DMF) (1992)
    Springer
    Journal of cluster science 3 (1992), S. 179-199 
    Details
    ISSN: 1572-8862
    Keywords: Heterometallic-heterobridging cubane-type tetranuclear cluster ; preparation ; crystal structure ; molecular orbital calculation ; quasi-aromaticity ; copper ; molybdenum
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract By the reaction of cluster [Mo3OS3](dtp)4(H2O) used as starting material with CuI using [3+1] mode, two novel heterometallic-heterobridging cubane-type tetranuclear cluster compounds [CuMo3OS3]·I·(μ-OAc)[S2P(OC2H5)2]3·L [(I)L=py, (II)L=DMF] [dtp=S2P(OC2H5)2; OAc=OOCCH3] containing [CuMo3OS3] core have been obtained. Compounds (I) and (II) have been characterized by IR, EPR, UV-VIS, electrochemistry and X-ray crystallography. By comparison of these two compounds with the analogous [CuMo3S4] series in the structure and molecular orbital calculation, the influence of mixed S/O bridging on the structure is discussed. It is demonstrated that the {Mo3S3} cluster ring in [Mo3OS3]4+ possesses a similar quasi-aromaticity to [Mo3S4]4+. Crystal data: for (I), space group= $$P\overline 1 $$ ,a=13.781(8)Å,b=14.523(6)Å,c=12.098(6)Å, α=98.37(4)°, β=109.41(5)°, γ=105.00(5)°,V=2133(2)Å3,Z=2,R=0.058; for (II), space group= $$P\overline 1 $$ ,a=13.215(4)Å,b=17.818(8)Å,c=9.873(4)Å, α=106.06(4)°, β=109.78(3)°, γ=82.00(3)°,V=2100(2)Å3,Z=2,R=0.045.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00702882
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  • 4
    Electronic Resource
    Electronic Resource
    Packing analysis and the crystal chemistry of 2,5-dibenzylidenecyclopent-3-ene-1-one. Rationale for a non-topochemical solid-state reaction (1992)
    Springer
    Molecular engineering 2 (1992), S. 103-116 
    Details
    ISSN: 1572-8951
    Keywords: Non-topochemical reaction ; crystal structure ; lattice energy calculations ; thermal motion analysis ; disorder
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The molecular and crystal structure of 2,5-dibenzylidenecyclopent-3-ene-1-one has been studied in detail to explain the formation of a non-topochemical pseudo-mirror-symmetric dimer upon photoirradiation. Packing energy calculations, analysis of the thermal motion, and lattice energy calculations are employed to analyse and understand the observed dimerization reaction, crystal structure, and crystal properties.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00999702
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  • 5
    Electronic Resource
    Electronic Resource
    The crystal and molecular structures of 1,1′-divinyl-2,2′-biimidazolyl (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 1076-1079 
    Details
    ISSN: 1573-9171
    Keywords: X-ray crystallographic analysis ; 1,1′-divinyl-2,2′-biimidazolyl ; crystal structure ; molecular structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal and molecular structures of 1,1′-divinyl-2,2′-biimidazolyl (L) were determined by x-ray crystallographic analysis. It was established that the molecule of L has crystallographic symmetry 2 and a cisoid conformation with an angle of rotation of 128° between the imidazole rings. The length of the C2-C2′ bond is increased to 1.485(11) Å compared with the length of the analogous bond in unsubstituted 2,2′-biimidazolyl (1.423 Å). Localization of the N=C multiple bond is observed [1.297(9) Å]. The other N-C bonds of the ring are almost equalized (1.374 Å) and are close to the standard values for bonds of the C sp 2-N type in imidazoles. The angle between the plane of the heterocycle and the plane passing through the atoms of the vinyl group amounts to 7°.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00866589
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  • 6
    Electronic Resource
    Electronic Resource
    Photo- and thermochromic mannich bases. 1. Mannich bases from 3,5-di-tert-butyl-4-hydroxybenzaldehyde and 2-naphthols (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 1875-1883 
    Details
    ISSN: 1573-9171
    Keywords: synthesis ; crystal structure ; UV spectra ; 2,6-di-tert-butyl-4-[α-(2-hydroxy-1-naphthyl)methyl]phenol ; 2,6-di-tert-butyl-4-[α-morpholino-α-(2-hydroxy-6-bromo-1-naphthyl)methyl]phenol ; 2,6-di-tert-butyl-4-α-(2-hydroxy-1-naphthyl)-1,4-methylenequinone ; 2,6-di-tert-butyl-4-α-(2-acetyloxy-1-naphthyl)-1,4-methylenequinone
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Mannich bases exhibiting photo- and thermochromic properties in solutions were synthesized from 3,5-di-tert-butyl-4-hydroxybenzaldehyde and 2-naphthols. An investigation of an acetyl derivative of methylenequinone, modeling a product of photo- and thermochromic transformations, proved that the color change of solutions of the Mannich bases is due to reversible dissociation into colored methylenequinones and morpholine. On the basis of data of x-ray diffraction analysis of one of the Mannich bases, characteristics of their molecular structure were determined, and reasons were stated for their effect on the dissociation mechanism.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00863826
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  • 7
    Electronic Resource
    Electronic Resource
    Synthesis and physicochemical investigation of LiMTif6 (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 1950-1956 
    Details
    ISSN: 1573-9171
    Keywords: hexafluorotitanates ; synthesis ; crystal structure ; 19F NMR ; IR spectroscopy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Mixed alkali hexafluorotitanates of the composition LiMTiF6 are synthesized, which crystallize with the orthorhombic symmetry. The lattice parameters of these materials are determined. It is shown that substitution of the Li+ cation in Li2TiF6 by Na+, K+, Rb+, and Cs+ leads to various degrees of distortion of the hexafluoroion. It is determined (19F NMR data) that the change in the dynamic state of the octahedral [TiF6]2− ions is related to their transition from the hindered-rotational to the isotropic state.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00863353
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  • 8
    Electronic Resource
    Electronic Resource
    Macrocyclic amidophosphoryl polyethers: Biological activity, molecular structure, and structure of the complex with calcium thiocyanate (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 2211-2216 
    Details
    ISSN: 1573-9171
    Keywords: macrocyclic polyethers ; crystal structure ; biological activity ; IR spectra ; complex with calcium thiocyanate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The antihypoxic and anticonvulsant activity of eight new amidophosphoryl derivatives of crown ethers was investigated. It was found that some of them exhibit pronounced antihypoxic activity. The results of an x-ray structural and IR spectroscopic study of dibenzo-N-phenylphosphonyl-14-crown-5 (a=9.818,b=16.062,c=15.925 Å; γ=124.90°;V=2072 Å3;M=417.2;d=1.33 g/cm3 forZ=4, 1955 independent reflections [I〉3σ(I)] in a DAR-UM inCuK α radiation,P2 1/b space group,R=5.2%) and dibenzo-N-adamantylphosphonyl-14-crown-5 compounds (a=11.077,b=15.936,c=16.771 Å; γ=56.05°;V=2456 Å3;M=486.3;d=1.31 g/cm3 forZ=4, 2164 independent reflections [I〉3σ(I)] in a DAR-UM inCuK α radiation,P21/b space group,R=5.1%) are reported. Some details of the structure of the dibenzo-N-phenylphosphonyl-14-crown-5-complex with calcium thiocyanate and water are discussed; a polyhedron with a coordination number of six was found for the first time for calcium complexes with macrocyclic ligands. The combined examination of the results of the biological, x-ray structural, and IR spectroscopic study of macrocyclic, 14-member ligands suggested that the nature of the substituents at phosphorus affect the conformational state of the macrocycle, which remains unchanged in complexation in the investigated conditions.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01150749
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  • 9
    Electronic Resource
    Electronic Resource
    Crystal and molecular structure of 1:1 molecular complexes of triphenyl-N-(4-methylpyridyl-2)phosphinimine and triphenyl-N-(3-methylpyridyl-2)phosphinimine with perchloric acid (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 495-499 
    Details
    ISSN: 1573-9171
    Keywords: crystal structure ; molecular complexes ; phosphinimines ; protonation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract X-ray diffraction analysis has been used to determine the crystal structures of the 1:1-composition products of protonation by perchloric acid of isomeric triphenyl-N-(4-methylpyridyl-2)phosphinimine (1) and triphenyl-N-(3-methylpyridyl-2)phosphinimine (2). The structures were refined toR=0.048 andR=0.052, respectively, using 2274 (1) and 2647 (2) reflections. The protonation centers are located at the sites of N atoms of the pyridine ring (1) and the phosphinimino group (2). The distribution of the bond lengths in the cations suggests that a significant contribution is made by a phosphonic structure with positive charges localized on the P atoms. N-H...O hydrogen bonds, with lengths of 2.890(4) and 3.020(3) Å, connect cations and anions in both structures.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00863071
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  • 10
    Electronic Resource
    Electronic Resource
    1,1,4,4-Tetranitrobutane-2,3-diol and its derivatives. 4. Study of the reaction of 1,1,4,4-tetranitrobutane-2,3-diol with N-(methoxymethyl)-2-fluoro-2,2-dinitroethylamine; synthesis and crystalline structure of 1,12-difluoro-1,1,3,5,5,8,8,10,12,12-decanitro-3,10-diazadodecane-6,7-diol dinitrate (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 528-530 
    Details
    ISSN: 1573-9171
    Keywords: synthesis ; crystal structure ; 1,12-difluoro-1,1,3,5,5,8,8,10,12,12-decanitro-3,10-diazadodecane-6,7-diol dinitrate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A two-step synthesis has been proposed to obtain 1,12-difluoro-1,1,3,5,5,8,8,10,12,12-decanitro-3,10-diazadodecane-6,7-diol dinitrate, starting from 1,1,4,4-tetranitrobutane-2,3-diol and N-(methoxymethyl)-2-fluoro-2,2-dinitroethyl-amine, followed by nitration of the Mannich base formed. An x-ray-diffraction investigation of the dinitrate obtained was carried out.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00863077
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  • 11
    Electronic Resource
    Electronic Resource
    X-ray structure of the organic conductor (ET)8[Hg2Br6·PhBr]2 (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 697-703 
    Details
    ISSN: 1573-9171
    Keywords: organic metals ; radical-cation salts ; bis(ethylenedithio)tetrathiafulvalene = ET ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The electrochemical oxidation of ET [bis(ethylenedithio)tetrathiafulvalene] in bromobenzene (electrolyte Bu 4 N[HgBr 3 ]) gave the radical-cation salt (ET) 8 [Hg 2 Br 6 ·PhBr] 2 (1), a new organic metal with a temperature range of 300–125 K. At 125 K a metal—dielectric transition is observed. Crystallographic data for (1):a=19.171(6),b=12.668(4),c=17.777(6) Å, α=118.03(3), β=89.45(2), γ=101.21(3)°, P $$\overline 1 $$ ,Z=1,d calc=2.30 g/cm 3 . The crystal structure of (1) is laminar. In the conducting organic layer the ET radical cations are linked into bands by shortened intermolecular S···S contacts of the “side-to-side” type. The anionic layer consists of centrosymmetric complexes [Hg 2 Br 6 ·C 6 H 5 Br] 2 4− . The Hg 1 and Hg 2 atoms are characterized by a trigonal configuration of the Hg-Br bond which is built up, on account of secondary Hg···Br interactions, into trigonal-bipyramidal for Hg 1 and trigonal-pyramidal (tetrahedral) for Hg 2 . Interaction between the anionic and cationic layers is effected through Br 6 ...S 8 contacts [3.491(7) Å)].
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01150895
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  • 12
    Electronic Resource
    Electronic Resource
    Crystal structure of the organic metal (ET)2[Hg(SCN)2Cl] withT M-D=50 K (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 704-709 
    Details
    ISSN: 1573-9171
    Keywords: organic metals ; bis(ethylenedithio)tetrathiafulvalene (ET) ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The composition and structure of the radical-ion salt (ET) 2 [Hg(SCN) 2 Cl], a new organic metal withT M-D=50 K, were established in an x-ray structure investigation. Principal crystallographic data:a=36.69(1),b=8.302(8),c=11.732(8) Å, β=90.02(6)°, space groupCc, Z=4,d calc=2.08 g/cm 3 ,R=0.067. The crystal structure of the salt consists of an alternation of organic (cationic) and inorganic (anionic) layers along the axisa. The anionic layer consists of the polymeric chains in which the [Hg(SCN) 2 Cl]− ions are linked together along the axisc through secondary Hg···N bonds with lengths of 2.75(3) and 2.98(8) Å. On account of these interactions the trigonal configuration of the bonds of the Hg atom is built up to trigonal-bipyramidal. In the organic layer with a structure of the κ type the ET cations form dimers with an interplanar distance of 3.53 Å. ET cations belonging to neighboring dimers are linked together through shortened intermolecular S...S contacts with lengths of 3.40–3.50(2) Å.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01150896
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  • 13
    Electronic Resource
    Electronic Resource
    Calixarenes as second-sphere ligands for transition metal ions. Synthesis and crystal structure of [(H2O)5 Ni(NC5H5)]2(Na)[calix[4]arene sulfonate] · 3.5 H2O and [(H2O)4Cu(NC5H5)2]-(H3O)3 [calix[4]arene sulfonate] · 10 H2O (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 14 (1992), S. 37-46 
    Details
    ISSN: 1573-1111
    Keywords: Calix[4]arene ; crystal structure ; second-sphere coordination ; nickel(II) ; copper(II) ; pyridine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The title compounds crystallize such that bilayers of calixarenes are separated by hydrophilic layers. In each case the transition metal has, in addition to a primary sphere of ligands, a second-sphere coordination by a calixarene. [(H2O)5Ni(NC5H5)]2(Na)[calix[4]arene sulfonate]·3.5 H2O,1, crystallizes in the triclinic space groupP $$\bar 1$$ witha = 12.487(4),b = 14.281(2),c = 15.055(5) Å, α = 85.66(2), β = 80.07(2), γ = 80.48(2)°, andD c = 1.64 g cm−3 forZ = 2. Refinement based on 2441 observed reflections led to a finalR value of 0.066. There are two different environments for the nickel-containing cations: one is positioned within the hydrophilic layer with the pyridine ligand intercalated into the hydrophobic calixarene bilayer and the other is also positioned within the hydrophilic layer, but the pyridine ligand is inserted into the hydrophobic cavity of the calix[4]arene. [(H2O)4Cu(NC5HS)2](H3O)3[calix[4]arene sulfonate]·10 H2O,2, crystallizes in the triclinic space groupP $$\bar 1$$ witha = 15.438(4),b = 15.727(6),c = 12.121(9) Å, α = 112.74(4), β = 102.02(4), γ = 85.34(4)°, andD c = 1.57 g cm−3 forZ = 2. Refinement based on 3925 observed reflections led to a finalR value of 0.107. The structure is similar to that of 1 except that the one copper-containing cation spans the hydrophilic layer and is intercalated into the bilayer of calixarenes on one side and positioned into the calixarene cavity on the other.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01041364
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  • 14
    Electronic Resource
    Electronic Resource
    Isomerization processes in inclusion compounds: Xylenes in deoxycholic acid (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 14 (1992), S. 55-64 
    Details
    ISSN: 1573-1111
    Keywords: Host-guest inclusion compound ; p-,m-,o-xylene ; deoxycholic acid ; symmetry factor ; energy transfer ; photophysical factor ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The isomerization processes induced by UV photons in inclusion compounds of the host-guest type are examined, with special attention to the photophysics of the energy transfer process between the host and the guest, as well as to the influence of the host molecular cavity symmetry and the guest molecular symmetry. In particular, the experimental study has been carried out on the isomerization processes ofp-,m-, ando-xylene inside the molecular cavities of deoxycholic acid. The results have been compared with those obtained by irradiating the xylenes in an inert solution of hexane. The main difference is the elimination of by-products when the photochemical process is carried out in the solid state inclusion compound; however, the high purity of the isomerization product corresponds to a decrease in its yield with respect to the reaction in solution, due to the energy transfer process from the host to the guest moiety.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01041366
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  • 15
    Electronic Resource
    Electronic Resource
    Crystal structure analysis of Y2Cu2O5 (1992)
    Springer
    Journal of superconductivity 5 (1992), S. 33-38 
    Details
    ISSN: 1572-9605
    Keywords: Yttrium ; copper ; X-ray ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Physics
    Notes: Abstract Single crystals of Y2Cu2O5 were obtained in the flux growth process by controlled heating of a mixture of Y2O3, BaO, and CuO in a molar ratio of 1∶8∶20. These crystals were analyzed by a single-crystal X-ray diffraction analysis. The crystal contains polymeric chains of Cu2O5 interspersed by yttrium ions surrounded by octahedral arrangements of oxygen atoms. Crystal data: space group=Pna21,a=10.799(2) Å,b=3.4990(5) Å,c=12.459(2) Å,Z=4, 380 reflections,R=0.026,R w=0.030.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00617994
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  • 16
    Electronic Resource
    Electronic Resource
    Three-dimensional structure of the quinoprotein methylamine dehydrogenase from Paracoccus denitrificans determined by molecular replacement at 2.8 Å resolution (1992)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 14 (1992), S. 288-299 
    Details
    ISSN: 0887-3585
    Keywords: amino acid-derived cofactor ; crystal structure ; methylamine dehydrogenase ; molecular replacement ; oxidoreductase ; Paracoccus denitrificans ; pyrroloquinoline quinone ; quinoprotein ; tryptophan tryptophylquinone ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The three-dimensional structure of the quinoprotein methylamine dehydrogenase from Paracoccus denitrificans (PD-MADH) has been determined at 2.8 Å resolution by the molecular replacement method combined with map averaging procedures, using data collected from an area detector. The structure of methylamine dehydrogenase from Thio-bacillus versutus, which contains an “X-ray” sequence, was used as the starting search model. MADH consists of 2 heavy (H) and 2 light (L) subunits related by a molecular 2-fold axis. The H subunit is folded into seven four-stranded β-segments, forming a disk-shaped structure, arranged with pseudo-7-fold symmetry. A 31-residue elongated tail exists at the N-terminus of the H subunit in MADH from T. versutus but is partially digested in this crystal form of MADH from P. denitrificans, leaving the H subunit about 18 residues shorter. Each L subunit contains 127 residues arranged into 10 β-strands connected by turns. The active site of the enzyme is located in the L subunit and is accessible via a hydrophobic channel between the H and L subunits. The redox cofactor of MADH, tryptophan tryptophylquinone is highly unusual. It is formed from two co-valently linked tryptophan side chains at positions 57 and 107 of the L subunit, one of which contains an orthoquinone. © 1992 Wiley-Liss, Inc.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prot.340140214
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  • 17
    Electronic Resource
    Electronic Resource
    Physicochemical Properties of Salts of p-Aminosalicylic Acid. I. Correlation of Crystal Structure and Hydrate Stability (1992)
    Springer
    Pharmaceutical research 9 (1992), S. 1428-1435 
    Details
    ISSN: 1573-904X
    Keywords: pharmaceutical salt selection ; salts of p-aminosalicylic acid ; hydrates ; crystal structure ; thermal stability
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The potassium (K), sodium (NA), calcium (CA), and magnesium (MG) salts of p-aminosalicylic acid were obtained, and their thermal behavior was characterized by means of differential scanning calorimetry (DSC) and thermogravimetric analysis (TG). Their crystal and molecular structures were determined by single-crystal X-ray diffraction after powder patterns had shown them to be nonisomorphous. Different degrees of hydration were observed for the solid salts, and an assessment of hydrate stability to dehydration was made from thermogravimetric studies. The onset temperature of dehydration (T t) of each salt varied within the series and exhibited correlation with X-ray determined structure. The observed onset of dehydration of MG and CA was higher than that of NA and is consistent with stronger ion-dipole interactions for the divalent salts. Crystallographic determination of the bond lengths between the metal ion and the water oxygens were 2.4 and 2.9 Å for NA, between 2.0 and 2.1 Å for MG, and 2.4 Å for CA. The open nature and presence of a channel feature in the structure of the sodium salt may have facilitated escape of water molecules from the crystal. Particle presentation (e.g., size, crystallinity) was also shown to affect dehydration behavior.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1015806812349
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  • 18
    Electronic Resource
    Electronic Resource
    The Structure of Celiprolol (1992)
    Springer
    Pharmaceutical research 9 (1992), S. 365-371 
    Details
    ISSN: 1573-904X
    Keywords: celiprolol ; crystal structure ; two-dimensional nuclear magnetic resonance (2D NMR)
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structure and nuclear magnetic resonance (NMR) spectra and assignments of celiprolol, N′-[3-acetyl-4[3-[N-t-butylamino-2-hydroxypropoxy]phenyl]-N, N-diethylurea, are reported. Celiprolol crystallizes in the monoclinic space group, P2l/a, with a = 9.081(2), b = 13.800(4), and c = 17.471(5) Å and β = 95.04(2)°. Structure was solved by direct methods; structure refinement to R of 0.058. Intermolecular hydrogen-bonding in the crystal is discussed. The 1H, 13C, and two-dimensional (2D) NMR spectra of the hydrochloride have been obtained and definitive signal assignments made.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1015895019791
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  • 19
    Electronic Resource
    Electronic Resource
    Solid state structure of the hydrated potassium thiocyanate complex of benzodinaphthopyridino 21-crown-7, C37H31NO6·KSCN·H2O (1 : 1 : 1) (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 13 (1992), S. 29-36 
    Details
    ISSN: 1573-1111
    Keywords: Crown compound ; potassium thiocyanate ; crown cation complex ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Single crystal X-ray analysis of the hydrated KSCN complex of benzodinaphthopyridino-21-crown-7 (1) (1 : 1 : 1) is reported. Crystals of the complex are orthorhombic,Pnma, withα = 16.946(4),b = 22.298(4),c = 10.390(8) Å andD c = 1.184 g cm−1,Z = 4. The host macroring (1) has a mirror symmetry and exists in a so-called ‘dentists chair’ conformation. The cation (K−) is coordinated to all the six ether oxygen atoms and also weakly to the pyridine N atom. The SCN− anion group has a statistical type of disorder with opposite orientations of S and N such that nitrogen and sulphur are coordinated to K+. Packing of the host molecules is in columns to form quasi channels with K+, SCN−, and H2O being located inside the stacks.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01076668
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  • 20
    Electronic Resource
    Electronic Resource
    Complexation with hydroxy host compounds, part 5. Structures and thermal analyses of 1,2,3,4,5-pentaphenylcyclopenta-2,4-dien-1-ol and its inclusion compounds with water and dimethylsulphoxide (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 13 (1992), S. 301-310 
    Details
    ISSN: 1573-1111
    Keywords: Inclusion compound ; hydroxy compound ; crystal structure ; thermal analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal and molecular structures of the title host compound (I), C35H26O, and its inclusion complexes with water (II), C35H26O·H2O and dimethylsulphoxide (III), C35H26O·C2H6OS are reported. (I) is monoclinicC2/c,a = 9.725(1),b = 20.031(3),c = 26.545(3) Å, β = 90.60(1)0,V = 5170 Å3,Z = 8; (II) is triclinic, $$P\bar 1$$ ,a = 10.206(1),b = 10.324(2),c = 14.425(2) Å, α = 101.68(1), β = 89.92(2), γ = 116.34(1)0,V = 1327 Å3,Z = 2; (III) is monoclinicP21/n,a = 17.832(5),b = 10.109(3),c = 17.901(5) Å, β = 111.93(2)0,V = 2993 Å3,Z =4. The structures were solved by direct methods and refined to final residuals of 0.045, 0.048, and 0.071, respectively. Thermal analysis of the complexes corroborates the crystallographic results.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01133229
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  • 21
    Electronic Resource
    Electronic Resource
    X-ray structural study of a zinc(II) inclusion complex of a phenolate-pendant cyclam (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 12 (1992), S. 377-387 
    Details
    ISSN: 1573-1111
    Keywords: Charles Pedersen ; crown ethers ; phenol-pendant cyclam-zinc(II) complex ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The molecular structure of phenol-pendant cyclam-zinc(II) complex,4a, has been determined by X-ray structure analysis. Crystals of4a · ClO4 · CH3OH (C16H27N4OZn · ClO4 · CH3OH) are monoclinic, space groupP21/nn, with four molecules in the unit cell of dimensionsa=31.198(2) Å,b=8.426(1) Å,c=8.214(1) Å, andβ=93.96(1)°. The structure was solved by the heavy atom method and refined anisotropically toR=0.044,R w=0.062 for 1551 independent reflections. The complex assumes a five-coordinate, square pyramidal geometry, where zinc(II) is surrounded by the cyclam moiety in a planar fashion with the pendant phenolate anion occupying an axial position. An extremely short Zn-O(phenolate) bond distance of 1.983(5) Å, in conjunction with the 0.288 Å displacement of Zn(II) above the cyclam N4 plane toward the phenolate, accounts for the extremely low pK a value of 5.8 for the pendant phenol. These facts about4a, in comparison with the previous findings for the Ni(II) (4b) and Cu(II) complexes (4c) with the same ligand, illustrate well the characteristics of zinc(II) ion coordination properties.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01053875
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  • 22
    Electronic Resource
    Electronic Resource
    Synthesis and crystal structure of a new paramagnetic complex salt of diprotonated dioxocyclam with PtCl 2− 4 and water (1:1:1) (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 13 (1992), S. 195-202 
    Details
    ISSN: 1573-1111
    Keywords: Dioxocyclam ; 5,7-dioxo-1,4,8,11-tetra-azacyclotetradecane ; platinum tetrachloride ; crystal structure ; paramagnetic properties of ionic stacked structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The paramagnetic complex salt of diprotonated dioxocyclam (1,11-dihydro-5,7-dioxo-1,4,8,11tetra-azacyclotetradecane), Pt(II) tetrachloride and water has been synthesized in strongly acidic medium and identified by X-ray structure analysis. The crystals of [(C10H22N4O2)2+(PtCl4)2−]·H2O are monoclinic, space groupP21 c,M r=585.23,a=9.516(1) Å,b=11.926(1) Å,c=16.622(2) Å,β=102.88(2)°,V=1839(1)Å3,Z=4,D x=2.114 g cm−3, λ(MoK α)=0.70930 Å,μ=83.1 cm−1,F(000)=1128,T=292 K,R=0.019 for 2808 observed reflections withI 〉 3δ(I). Alternating moieties of diprotonated dioxocyclam and a PtCl 2− 4 anion form columns running down the c axis. Water molecules are localized in the intercolumnar space and contribute to the extensive hydrogen bond network. The macrocycle conformation is characterized by two sequences of torsional angles, corresponding to two different subunits. The shorter sequence idealized as (-sc, ap, -ac, + ac, ap, +sc) [sc( ±60°), ac( ±120°), ap(180°)], describing the C pseudosymmetric part of the molecule, is centered on a -CH2 group between the two peptide O-C-N-H fragments. The opposite C pseudosymmetric subunit has a nearly (-sc, ac, -SC, ap)2 conformation. Pt is square planar coordinated by four Cl atoms, Pt-Clαve = 2.306(8) Å. The shortest Pt ... Pt distance is 7.200(1) Å.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01053643
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  • 23
    Electronic Resource
    Electronic Resource
    A hydrogen bond between a calixarene (as host and its guest: Crystal and molecular structure of thep-t-butyldihomooxacalix[4]arene : Triethylamine (1 : 2) complex/clathrate (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 14 (1992), S. 247-256 
    Details
    ISSN: 1573-1111
    Keywords: Inclusion compounds ; calixarene ; crystal structure ; hydrogen bonding ; amines
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The structure of thep-t-butyldihomooxacalix[4]arene triethylamine (1 : 2 complex has been determined by X-ray crystallography. Crystals are monoclinic, space groupCc,a = 22.821(3),b = 15.257(3),c = 16.365(2) Å,β = 97.44(1)°,V = 5650(1) Å3,Z = 4,D calc = 1.03 g cm−3. One triethylamine (Et3N) molecule has one of its ethyl groups pointing inside the cavity of a calixarene molecule; its nitrogen atom is directed exo to this calixarene molecule and is involved in a hydrogen bond with one of the hydroxy groups of a neighbouring calixarene molecule. This scheme leads to columns of alternating host and guest molecules. The other Et3N molecule is in the interhost space. This feature allows us to define the title compound as a complex/clathrate hybrid.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01045984
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  • 24
    Electronic Resource
    Electronic Resource
    The crystal structure of the syn-proximal-5,11,17,23-tetra-tert-butyl-25,26-bis[(2-pyridylmethyl)oxy]-27,28-dihydroxy-calix[4]arene ethanol 1 : 1 Inclusion Complex (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 14 (1992), S. 349-356 
    Details
    ISSN: 1573-1111
    Keywords: 1,2-Dialkylated calix[4]arene ; crystal structure ; ethanol inclusion complex ; intramolecular hydrogen bonding patterns
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structure of the title compound (1 · C2H5OH) has been determined by single-crystal X-ray analysis and refined to anR-value of 0.074 for 2732 observed reflections [I 〉 2.0σ(I)]. Crystals are triclinic, space group P $$\bar 1$$ , witha = 13.6150(18),b = 13.7195(11),c = 16.5497(16) Å, α = 73.132(7),β = 66.165(9), γ = 65.580(8)° andZ = 2. Calix[4]arene (1) adopts a relatively open distorted cone conformation in the solid state, with two pendantsyn-proximal O-CH2-Py groups. The major conformation determining features in (1 · C2H5OH) are the presence of (a) an intramolecular O-H...O hydrogen bond between adjacent proximal phenolic oxygens, O...O 2.719(7) Å and (b) an intramolecular O-H...N hydrogen bond between a phenolic oxygen and a proximal pyridinyl nitrogen, O...N 2.810(8) Å. The intramolecular hydrogen bonding and the interplanar angles of 65.1(3) and 50.7(3)° between opposite aromatic rings facilitate the inclusion of an ethanol molecule within the calixarene cup.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01045993
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  • 25
    Electronic Resource
    Electronic Resource
    Tribracchial lariat ethers: Syntheses, binding, and formation of an intramolecular macroring-sidearm complex in the absence of any cation (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 12 (1992), S. 187-197 
    Details
    ISSN: 1573-1111
    Keywords: Cation binding ; crown ether ; crystal structure ; lariat ether ; synthesis ; triaza-18-crown-6
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Details of a new synthetic approach to 4,10,16-triaza-18-crown-6 (‘triaza-18-crown-6’) are reported, along with the preparation and binding properties of the following derivatives having the indicated sidearms: CH2C≡CH, CH2CH2OH, CH2CH2OCH3, COCH2OCH3,CH2COOCH2CH3, CH2C6H5, and CH2C6H4−2−NO2. A key intermediate in the synthesis of triaza-18-crown-6 is 4-N-toluenesulfonyl-1,7,13-trioxa-4,10,16-triazacyclooctadecane-9,17-dione. This compound is found by solid state structure analysis to fold to form an intramolecular, doubly-hydrogen bonded complex in which the two N-H protons interact with the two tosyl group oxygens. Details of the structure are reported.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01053861
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  • 26
    Electronic Resource
    Electronic Resource
    Absolute configuration and conformation of the pure opioid antagonist (+)-2,9α-dimethyl-5-(m-hydroxyphenyl)morphan (1992)
    New York, NY [u.a.] : Wiley-Blackwell
    Chirality 4 (1992), S. 377-383 
    Details
    ISSN: 0899-0042
    Keywords: crystal structure ; molecular mechanics ; MM2-87 ; phenylmorphan ; phenyl-equatorial ; opioid ligand model ; μ-receptors ; K-receptors ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: (+)-2,9α-Dimethyl-5-(m-hydroxyphenyl)morphan is the only phenylmorphan analog whose affinity for opioid K-receptors is greater than its affinity for opioid κ-receptors. Pharmacologically, the compound is a pure opioid antagonist devoid of agonist activity in in vivo assays of antinociception. The absolute configuration of the compound has been determined to be (1R,5S,9R) from an X-ray crystallographic study of the chloride salt. Thus, the absolute configuration corresponds to that of the atypical opioid agonist (-)-phenylmorphan while the weak atypical agonist (-)-2,9α-dimethyl-5-(m-hydroxyphenyl)morphan corresponds to the potent morphine-like (+)-phenylmorphan. The preferred orientations of the phenyl ring for the two stereoisomers were determined using the molecular mechanics program MM2-87 and found to vary from that of the two parent compounds. The atypical properties of the two 9α-methyl analogs is consistent with an opioid ligand model which proposes that morphine-like properties require a particular range of phenyl orientations. There was good agreement between the structure obtained from X-ray crystallography and computed with the MM2-87 program. © 1992 Wiley-Liss, Inc.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/chir.530040608
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  • 27
    Electronic Resource
    Electronic Resource
    Lamellar and whisker single crystals of poly(2,6-oxynaphthoate) (1992)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 30 (1992), S. 1469-1482 
    Details
    ISSN: 0887-6266
    Keywords: poly(2,6-oxynaphthoate) ; crystal structure ; whiskers ; lamellae ; unit cell ; transitions ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Electron diffraction from single crystal lamellae and whiskers of poly(2,6-oxynaphthoate) reveals the presence of at least 3 unit cells. The equatorial reflections in the patterns from the whiskers correspond to the dominant (phase I) hk0 diffraction pattern from the lamellae; phase I is monoclinic with 2 chemical repeats per physical repeat. The intensity distributions in the hk0 patterns of phase I and II resemble those of the same phases in poly(p-oxybenzoate). The hk0 reflections of phase III suggest a common internapthalene unit spacing, but variable lateral (and possibly axial) shifts; apparently related orthorhombic and monoclinic patterns, with variable γ*, are observed. At elevated temperature, above the crystalliquid crystal transition (ca. 330°C), quadrant reflections are retained; the change in the hk0 pattern from any given crystal is gradual, extending over some 40°C. Above the liquid crystal-liquid crystal transition (ca. 460°C) the pattern can be interpreted in terms of nematic or possibly smectic A packing. © 1992 John Wiley & Sons, Inc.
    Additional Material: 19 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/polb.1992.090301306
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  • 28
    Electronic Resource
    Electronic Resource
    Ein neues Syntheseverfahren für die Wolframbronze Cs0,29WO3 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 95-98 
    Details
    ISSN: 0044-2313
    Keywords: Tungsten bronze, Cs0.29WO3 ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Novel Synthetic Access to the Tungsten Bronze Cs0.29WO3 and its Crystal StructureThe hexagonal tungsten bronze Cs0.29WO3 was obtained in form of black, prismatic crystal by the reduction of WO3 with molten cesium iodide at 700°C. Its crystal structure was determined by X-ray diffraction (399 unique observed reflexions, R = 0.058). Crystal data: a = 741.2(3), c = 760.0(5) pm, space group P6322, Z = 6. It corresponds to the known structure of hexagonal tungsten bronzes, having tungsten atoms displaced from the octahedra centres by 11.9 pm and with three different W—O bond lengths (198, 191, 187 pm). The WO6 octahedra are slightly titled mutually.
    Notes: Bei der Reaktion von WO3 in einer Caesiumiodid-Schmelze bei 700°C entsteht die hexagonale Wolframbronze Cs0.29WO3 in Form schwarzer, hexagonal-prismatischer Kristalle. Ihre Struktur wurde durch Röntgenbeugung bestimmt (399 beobachtete unabhängige Reflexe, R = 5,8%). Kristalldaten: a = 741,2(3), c = 760,0(5) pm, Raumgruppe P6322, Z = 6. Es handelt sich um die bekannte Struktur der hexagonalen Wolframbronzen mit Wolframatomen, die aus den Oktaedermitten um 11,9 pm herausgerückt sind und mit drei verschiedenen W—O-Bindungslängen (198, 191, 187 pm). Die WO6-Oktaeder sind leicht gegeneinander verkippt.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926090318
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  • 29
    Electronic Resource
    Electronic Resource
    Röntgenstrukturanalyse des 1,3-Bis(diethylamino)-1,3-dibenzyl-2,4-diphenyl-1λ5, 3λ5-diphosphets (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 99-102 
    Details
    ISSN: 0044-2313
    Keywords: Diphosphete ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: X-Ray Crystal Structure Determination of 1,3-Bis(diethylamino)-1,3-dibenzyl-2,4-diphenyl-1λ5, 3λ5-diphospheteBenzylidene-diethylamino-benzylfuorophosphorane, 1, reacts with lithium bis(trimethylsilyl)amide to give the title compounds 2 and 1-diethylamino-2,3-diphenylphosphirane, 3. Only one of the stereoisomers of 2 is formed in which the two benzyl groups are located on the same side of the planar four-membered ring. 2 crystallizes in the monoclinic space group P21/n.
    Notes: Benzyliden-diethylamino-benzylfuorphosphoran, 1, reagiert mit Lithium-bis(trimethylsilyl)-amid zur Titelverbindung 2 und 1-Diethylamino-2,3-diphenylphosphiran, 3. Von 2 wird nur das Stereoisomer gebildet, bei dem die beiden Benzylgruppen auf der gleichen Seite des ebenen viergliedrigen Rings angeordnet sind. 2 kristallisiert in der monoklinen Raumgruppe P21/n.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926090319
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  • 30
    Electronic Resource
    Electronic Resource
    Structures of Xenon Oxygen Compounds (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 153-156 
    Details
    ISSN: 0044-2313
    Keywords: Xenon oxygen compounds ; Xe(OTeF5)4 ; O2Xe(OTeF5)2 ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Strukturen von Xenon-Sauerstoff-VerbindungenDie Struktur des lange bekannten Xe(OTeF5)4 wurde durch die Kristallstrukturanalyse aufgeklärt. Das Xenonatom ist von vier Sauerstoffatomen in einer regelmäßigen quadratisch planaren Anordnung umgeben. O2Xe(OTeF5)2 ensteht gemäß O — Xe(OTeF5)4 → O2Xe(OTeF5)2 + F5Te—O—TeF5. Die Struktur - wiederum mit Hilfe der Röntgenstrukturanalyse bestimmt - zeigt das Xenonatom in einer sehr verzerrten tetraedrischen oder pseudo-trigonal bipyramidalen Umgebung. Das Elektronenpaarabstoßungsmodell versagt hier bei der Erklärung der Feinheiten dieser Struktur.
    Notes: The structure of long known Xe(OTeF5)4 is established by x-ray crystallography. The xenon atom is surrounded by four equidistant oxygen atoms in a square planar manner. O2Xe(OTeF5)2 is formed according to OXe(OTeF5)4 → O2Xe(OTeF5)2 + F5TeOTeF5, Its structure, again established by x-ray crystallography, shows a very distorted tetrahedral or pseudo-trigonal bipyramidal xenon environment. The electron pair repulsion models fails here in explaining the details of this geometry.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926090327
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  • 31
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    Synthese und Kristallstruktur von Hydronium-tris-ethylendiamin-cobalt(rhodium)-μ-trichloro-nonachlorotrirhenat(II)-chlorid, H3O[MEn3][Re3Cl12]Cl (M=Co, Rh) (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 607 (1992), S. 91-95 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium complexes ; 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 Hydronium-tris-ethylenediamine-cobalt(rhodium)-μ-trichloro-nonachlorotrirhenate(III)-chloride, H3O[MEn3][Re3Cl12]Cl (M=Co, Rh)The chlorides H3O[MEn3][Re3Cl12]CI (M = Co, 1; Rh, 2) crystallize from hydrochloric acid solutions of ReCl3 and MEn3 · 3H2O as deep red hexagonal columns. They are isotypic and crystallize with the hexagonal system (P6, Z = 1; 1: a = 1010.87(3); c = 794.30(4) pm, R = 0.023, Rw = 0.016; 2: a = 1018.58(3); c = 794.74(4) pm, R = 0.026, Rw = 0.018). The anions [Re3Cl12]3- are connected via H3O+ cation (C.N. 3). The large channels that run in the [001] direction contain, alternatively, the cations [MEn3]3+ and the lonesome Cl--anions
    Notes: Die Chloride H3O[MEn3][Re3CI12]CI(M = Co, 1; Rh, 2) Kristallisieren in Form tiefroter hexagonaler Säulen aus salzsauren Lösungen von ReCI3 und MEn3CI3 · 3H2O aus. Sie sind isotyp und Kristallisieren im hexagonalen System (P6, Z = 1; 1: a = 1010,87(3); C = 794,30(4)pm, Rw = 0,016; : a = 1018,58(3); c = 794,74(4)pm, R = 0,026, Rw = 0,018). Die Anionen [ Re3Cl12]3- werden über H3O+ (C.N. 3) verknüpft; in die entstehenden Kanäle sind längs [001] abwechselnd die Kationen [MEn3]3+ und die einsamen Cl--Ionen eingelagert.
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    Neue Untersuchungen an quaternären Fluoriden (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 607 (1992), S. 121-123 
    Details
    ISSN: 0044-2313
    Keywords: Quaternary fluorides ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Investigations on Quaternary FluoridesFor the first time the quaternary fluorides M12MIILnF7 (M1 = Na, Ag; MII = Ca, Cd; Ln = Er—Lu) had been prepared and examined with with X-ray diffraction. All these compounds crystallize in a cubic face-centered lattice. Colourless single crystals of Na2CdYbF7 were obtained and the structure was determined. Na2CdYbF7 crystallizes in the space group Fm3M-O5h, No. 225. The single-crystal diffraction data refer to a Defect-Fluorite-Structure. The R-value for 332 observed (29 independend) reflections is 2.2%.
    Notes: Erstmals wurden die quarternären Fluoride M12M11LnF7 (M1 = Na, Ag; M11 = Ca, Cd; Ln = Er—Lu) dargestellt und röntgenographisch untersucht. Alle Verbindungen kristallisieren kubisch flächenzentriert. An farblosen Einkristallen von Na2CdYbF7 wurde eine Strukturbestimmung durchgeführt. Na2CdYbF7 kristallisiert in der Raumgruppe Fm3m-O5h, Nr. 225. Die Meßwerte verweisen auf eine Defekt-Fluorit-Struktur. Der R-Wert fär 332 beobachtete (29 unabhängige) Röntgenreflexe beträgt 2,2%.
    Additional Material: 3 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19926070120
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    Zur Addition von Übergangsmetallhalogeniden an Acetylacetonate zweiwertiger Metallionen (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 614 (1992), S. 65-72 
    Details
    ISSN: 0044-2313
    Keywords: Transition metal halides acetylacetonate complexes ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Addition of Transition Metal Dihalides to Acetylacetonates of Divalent Metal IonsTransition metal dihalides aMIIX2 (FeCl2, CoCl2 NiBr2 etc.) are added by the chelates MII(acac)2 under formation of binuclear complexes (THF)2MII(acac)2(aMIIX2). The octahedral and the tetrahedral centre of these compounds are connected by tridentate oxygen atoms of the two acetylacetonato ligands which are simultaneously included in four-membered rings (MIIO2aMII). The addition is combined with a deformation of the octahedral centre, as a prerequisite of a closest package of the atoms within the MIIO2aMII-ring.In the trinuclear complex (THF)2Ni(acac)2(HgCl2)2 III the interaction between the three coordination centres is weak. No structural change of the octahedral centre (THF)2Ni(acac)2 is found, but the HgCl2-groups diverge slightly from linearity (Cl—Hg—Cl 171.1°).No binuclear complexes with a central ion of the oxidation state III in the octahedral centre were obtained. One reason is the lowered donor strength of the bidentate Lewis base function of the octahedral centre [(THF)2Mn+(acac)2]n-2 with M+3 as a centralatom. Reacting systems with di- and trivalent ions prefer ionic complexes, as it is shown by the formation of [(THF)2V(acac)2][(THF)CoCl3] IV from VCl3 and Co(acac)2.The crystal structures of (THF)2Co(acac)2CoCl2II and [(THF)2V(acac)2][(THF)CoCl3] IV were determined by x-ray diffraction. II: orthorhombic-primitive; space group P212121, Z = 4; a = 967.4(2), b = 1453.4(3), c = 1715.9(4) pm; R = 0.049 for 3084 observed reflections. IV: triclinic; space group P1, Nr. 2; Z = 2; a = 871,5(2), b = 930,6(3), c = 1865,6(6) pm; α = 101,70(2), b̃ = 92,45(2), γ = 91,06(2)°; R = 0,060 für 4221 observed reflections.
    Notes: Bis(acetylacetonate) von Magnesium(II), Cobalt(II) oder Nickel(II) addieren Dihalogenide wie FeCl2, CoCl2 oder NiBr2 (aMIIX2) unter Bildung binuklearer Komplexe (THF)2MII(acac)2(aMIIX2), in denen ein oktaedrisches und ein tetraedrisches Zentrum über zwei dreibindige Sauerstoffatome der Acetylacetonatliganden miteinander verknüpft sind (Bildung eines viergliedrigen MIIO2aMII-Ringes). Die Addition ist mit einer Deformation des oktaedrischen Zentrums verbunden, die eine dichte Packung der vier Atome des MIIO2aMII-Ringes ermöglicht.Im trinuklearen Komplex (THF)2Ni(acac)2(HgCl2)2 III bleibt die Wechselwirkung zwischen den drei Koordinationszentren gering. Das oktaedrische Zentrum (THF)2Ni(acac)2 wird strukturell nicht verändert, allerdings weichen die beiden HgCl2-Bausteine (Valenzwinkel 171,1°) von der Linearität ab.Es gelang nicht, binukleare Komplexe mit einem Zentralatom der Oxidationsstufe III im oktaedrischen Zentrum darzustellen. Ein Grund dafür ist die verringerte Donorstärke der zweizähligen Lewisbasen-Funktion im oktaedrischen Zentrum [(THF)Mn+(acac)2]n-2 für M+3 als Zentralion. Reaktive Systeme mit zwei- und dreiwertigen Kationen weichen auf die Seite von ionischen Komplexen aus, wie die Bildung von [(THF)2V(acac)2][(THF)CoCl3] IV aus VCl3 und Co(acac)2 zeigt.Die Kristallstrukturen von (THF)2Co(acac)2CoCl2 II und [(THF)2V(acac)2][(THF)CoCl3] IV wurden durch Röntgenbeugung bestimmt.II: orthorhombisch primitiv, Raumgruppe P212121, Z = 4; a = 967,4(2), b = 1453,4(3), c = 1715,9(4) pm; R = 0,049 für 3084 beobachtete Reflexe.IV: triklin, Raumgruppe P1, Nr.2; Z = 2; a = 871,5(2), b = 930,6(3), c = 1865,6(6) pm; α = 101,70(2), b̃ = 92,45(2), γ = 91,06(2)°; R = 0,060 für 4221 beobachtete Reflexe.
    Additional Material: 4 Ill.
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    Die Kristallstrukturen von Me3SiI · β-Picolin und Me3SiI · γ-Picolin Vergleich der Lewis-Basen Pyridin, β-Picolin und γ-Picolin (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 145-150 
    Details
    ISSN: 0044-2313
    Keywords: Iodinetrimethylsilane · β-picoline ; -.γ-picoline ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Me3SiI · β-Picoline and Me3SiI · γ-Picoline A Comparison between the Lewis-Bases Pyridine, β-Picoline, and γ-PicolineThe reaction of Iodinetrimethylsilane with β- und γ-Picoline (Pic) leads to solid 1 : 1 compounds Me3SiI · β-Picoline 1, Me3SiI · γ-Picoline 2. The reaction was performed at room temperature. Yellow single crystals were obtained by sublimation. Single crystal X-ray investigations confirm that both compounds are ionic [Me3SiPic]+I-. The comparison of β-Picoline with γ-Picoline and Pyridine (Py) demonstrates that the presence of a methyl group and also its position has no significant influence on the Si—N bond length in compound 1, 2 and on the adduct Me3SiI · Py.
    Notes: Iodtrimethylsilan reagiert mit β- und γ-Picolin (Pic) bei Raumtemperatur zu festen 1 : 1 Addukten (M3SiI · β-Picolin 1, Me3SiI · γ-Picolin 2), die durch Sublimation leicht gelblich gefärbte Einkristalle bilden. Die Röntgenstrukturanalyse beider Verbindungen beweist eine ionische Struktur des Typs [Me3SiPic]+ I-. Der Vergleich von β-Picolin mit γ-Picolin und Pyridin (Py) zeigt, daß die Anwesenheit einer Methylgruppe und auch deren Position keinen signifikanten Einfluß auf die Si—N-Bindungslänge in Verbindung 1, 2 und dem Addukt Me3SiI · Py hat.
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    URL: http://dx.doi.org/10.1002/zaac.19926100124
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    Hydrate schwacher und starker Basen. VII. Zum System Caesiumhydroxid-Wasser: Die Kristallstrukturen von CsOH · 2H2O und CsOH · 3H2OHerrn Professor Joseph Grobe zum 60. Geburtstage am 2. November 1991 gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 608 (1992), S. 123-130 
    Details
    ISSN: 0044-2313
    Keywords: Cesium hydroxide hydrates ; 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. VII. Concerning the System Cesium Hydroxide - Water: The Crystal Structures of CsOH · 2H2O and CsOH · 3H2OIn the context of structural studies of hydrates of the alkali metal hydroxide the crystal structure of CsOH · 2H2O and CsOH · 3H2O have been determined for the first time. The diffractometer data, obtained at -150 · C,made it possible to locate and refine also all the H-atoms. The dihydrate was found to probably form only one phase, melting incongruently at 2,5 · C. It is orthorhombic with space group Pca21 and Z = 8 formula units per unit cell. The lattice constants are a = 13.238, b = 6.747 and c = 9.121 A. With 1870 independent observed reflection a final R value of 0.013 was obtained. The trihydrate, melting congruently et -5.5 ·C, is monoclinic with space group P21/n,Z = 4 and lattice constants a = 8.637, b = 5.984, c = 10.061 Å and ß = 96.57 ·. With 2098 independent observed reflection the final R is 0.026. In both hydrate structures there are no simple characteristic coordination polyhedra for the cations; in each case it is rather the hydrogen-bonded and fully ordered anionic water structure which shows up as the determining building principle. Both these water structures are altogether three-dimensional, but primarily contain layers. The anionic layers are formed by condensation of small and medium rings, namely four-, five- and seven-membered rings in CsOH · 2H2O and four-, five- and six membered ones in CsOH · 3H2O. They are linked together by one set each of extra H2O molecules between the layers as well as by the Cs+ ions.
    Notes: In Zusammenhang mit Untersuchungen zur Struktur von Hydraten der Alkalimetallhydroxide wurden die Kristallstrukturen von CsOH · 2H2O und CsoH · 3H2O erstmalig bestimmt. Die bei - 150°C erhaltenen Diffraktometerdaten erlaubten dabei auch die Lokalisierung und Verfeinerung Sämtlicher H-Atome. Das nach eigenen Untersuchungen wahrscheinlich nur einphasig vorliegende Dihydrat schmilzt inkongruent bei 2,5°C und kristallisiert orthorhombisch mit der Raumgruppe Pca21 und Z = 8 Formeleinheiten pro Elementarzelle sowie den Gitterkonstanten a = 13,238, b = 6,747 und c = 9,121 ß. Mit 1870 unabhängigen beobachteten Reflexen wurde ein abschließender R-Wert von 0,013 erreicht. Das bei - 5,5°C kongruent schmelzende Trihydrat ist monoklin mit der Raumgruppe P21/n und Z = 4. Die Gitterkonstanten betragen a = 8,637, b = 5,984, c = 10,061 A und ß = 96,57°. Mit 2098 unabhängigen beobachteten Reflexen liegt der abschließende R-Wert bei 0,026. In beiden Hydratstrukturen gibt es keine einfachen charakteristischen Koordinationspolyeder für die Kationen; vielmehr wird jeweils die durch H-Brücken gebildete und vollständig geordnete anionische Wasserstruktur zum bestimmenden Bauprinzip. Beide Wasserstrukturen sind insgesamt dreidimensional, enthalten primär aber Schichten. Die aus Kondensierten Kleinen und mittleren Ringen, nämlich Vier-, Fünf - und Siebenringen (CsOH · 2H2O) bzw. Vier-, Fünf- und Sechsringen (CsOH · 3H2O), bestehenden anionischen Schichten werden jeweils über einen Satz weiterer H2O-Moleküle zwischen den Schichten sowie über die Cs+-Ionen miteinander verknüpft.
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    Bis(triphenylphosphaniminato)niobtrichlorid, [NbCl3(NPPh3)2], ein Komplex mit fünffach koordiniertem NiobProfessor Osvald Knop zum 70. Geburtstage am 11. Juli 1992 gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 7-10 
    Details
    ISSN: 0044-2313
    Keywords: Phosphorane iminato complex of niobium ; synthesis ; IR spectrum ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Bis(triphenylphosphorane-iminato)niobium Trichloride, [NbCl3(NPPh3)2], a Complex with Coordination Number Five at the Niobium AtomThe title compound has been prepared from niobium pentachloride with Me3SiNPPh3 in acetonitrile solution, forming colourless, moisture sensitive crystals. They were characterized by IR spectroscopy and by an X-ray structure determination. [NbCl3(NPPh3)2] crystallizes monoclinically in the space group Cc with four formula units per unit cell, 3682 observed, unique reflections, R = 0.042%. Lattice dimensions at 20°C: a = 1025.1(2); b = 1870.6(6); c = 1832.5(5) pm, β = 91.83(2)°. The niobium atom of the complex is coordinated in a distorted trigonal bipyramidal fashion, while the nitrogen atoms of the two phosphorane iminato ligands are in equatorial position along with one chlorine atom. NbN and PN distances accord with double bonds; with a mean value of 242.0 pm the Nb—Cl distances are remarkably long.
    Notes: Die Titelverbindung entsteht in Form farbloser, feuchtigkeitsempfindlicher Kristalle bei der Reaktion von Niobpentachlorid mit Me3SiNPPh3 in Acetonitrillösung. Sie wird durch das IR-Spektrum und eine röntgenographische Strukturanalyse charakterisiert. [NbCl3(NPPh3)2] kristallisiert monoklin in der Raumgruppe Cc mit vier Formeleinheiten pro Elementarzelle, 3682 beobachtete unabhängige Reflexe, R = 4,2%. Gitterabmessungen bei 20°C: a = 1025,1(2); b = 1870,6(6); c = 1832,5(5) pm, β = 91,83(2)°. In dem Komplex ist das Niobatom verzerrt trigonal-bipyramidal koordiniert, wobei die N-Atome der beiden Phosphaniminatoliganden zusammen mit einem Chloratom äquatorial angeordnet sind. NbN- und PN-Abstände entsprechen Doppelbindungen; die Nb—Cl-Abstände sind mit dem Mittelwert von 242,0 pm auffällig lang.
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    Die Kristallstruktur von Na2NiAlF7 - ein Beitrag zum Problem der wahren Raumgruppe orthorhombischer WeberiteProfessor Osvald Knop zum 70. Geburtstage am 11. Juli 1992 gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 11-15 
    Details
    ISSN: 0044-2313
    Keywords: Weberite ; crystal structure ; nickel aluminium fluoride ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Na2NiAlF7  -  a Contribution to the Problem of the True Space Group of Orthorhombic WeberitesThe X-ray single crystal structure determination of the orthorhombic weberite Na2NiAlF7 (a = 707.4(2), b = 1003.8(2), c = 731.5(1) pm; Z = 4) was performed in space group Imma, after all reflections hk0 with h(k) = 2n + 1 could be eliminated, as they proved simulated by Renninger effect and/or λ/2 reflections. The alternative space groups Imm2 resp. I212121 of former weberite structure determinations thus became obsolete. The refinement using 880 independent reflections ended at wR = 0.0232. The resulting average distances within the framework of octahedra are Ni—F = 197.3, Al—F = 180.4 pm.
    Notes: Die Röntgen-Einkristallstrukturbestimmung des orthorhombischen Weberits Na2NiAlF7 (a = 707,4(2), b = 1003,8(2), c = 731,5(1) pm; Z = 4) wurde in der Raumgruppe Imma vorgenommen, nachdem alle Reflexe hk0 mit h(k) = 2n + 1 eliminiert werden konnten, weil sie sich durch Renninger-Effekt und/oder λ/2-Reflexe als vorgetäuscht erwiesen. Damit wurden die alternativen Raumgruppen Imm2 bzw. I212121 früherer Weberit-Strukturbestimmungen obsolet. Die Verfeinerung mit 880 unabhängigen Reflexen schloß ab mit wR = 0,0232. Die resultierenden Mittelwerte für die Abstände im Oktaedernetz betragen Ni—F = 197,3 pm, Al—F = 180,4 pm.
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    Molekül- und Kristallstruktur von Ytterbium(III)-triaqua-trinitrat, Yb(H2O)3(NO3)3 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 16-18 
    Details
    ISSN: 0044-2313
    Keywords: Ytterbium nitrates ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Molecular and Crystal Structure of Ytterbium(III)-triaqua-trinitrate, Yb(H2O)3(NO3)3Yb(H2O)3(NO3)3 crystallizes from a concentrated solution of Yb2O3 in nitric acid in a vacuum desiccator at ambient temperature as colourless single crystals. The crystal structure was determined from single crystal four-circle diffractometer data (R3, Z = 6, a = 1175.5(1), c = 1117.7(2) pm, Vm = 134.25 cm3/mol, R = 3.0%, Rw = 2.9%). The structure may be viewed at as a heavily compressed packing of [Yb(H2O)3(NO3)3] molecules. Yb3+ is coordinated by three bidentate nitrate ligands and three water molecules so that a tricapped trigonal prism (C.N. 9) of oxygen atoms results as the coordination polyhedron.
    Notes: Yb(H2O)3(NO3)3 kristallisiert aus einer konzentrierten Lösung von Yb2O3 in Salpetersäure im Vakuumexsikkator bei Raumtemperatur in Form farbloser Einkristalle aus. Die Kristallstruktur wurde aus Einkristall-Vierkreis-Diffraktometer-Daten bestimmt (R3, Z = 6, a = 1175,5(1), c = 1117,7(2) pm, Vm = 134,25 cm3/mol, R = 3,0%, Rw = 2,9%). Sie kann als stark gestauchte Kugelpackung von [Yb(H2O)3(NO3)3]- Molekülen aufgefaßt werden. In diesen ist Yb3+ von drei zweizähnigen Nitratliganden und drei Wassermolekülen in Form eines dreifach bekappten trigonalen Prismas (C. N. 9) von Sauerstoffatomen umgeben.
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    Chelate von Chinolin-8-ol-Derivaten. XIIXI. Mitt. s. [1].. Die Kristall- und Molekülstruktur von Bis(7-isopropylchinolin-8-olato)nickel(II) (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 39-42 
    Details
    ISSN: 0044-2313
    Keywords: Bis(7-isopropyl-8-quinolinato)nickel(II) ; crystal structure ; association of nickel 8-quinolates ; steric hindrance ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chelates of 8-Quinolinol Derivatives. XII. Crystal and Molecular Structure of Bis(7-isopropyl-8-quinolinato)nickel(II)The crystal and molecular structure of bis(7-isopropyl-8-quinolinato)nickel(II) was determined by X-ray diffraction. The structure is monoclinic with the space group P21/n (Z = 2, 1403 observed independent reflections, R = 0.049. Lattice dimensions at 20°C: a = 1328.3(5) pm, b = 632.8(2) pm, c = 1330.0(5) pm, β = 112.99(3)°). The coordination of the nickel atom is planar with the quinoline rings in trans position.
    Notes: Die Kristallstruktur von Bis(7-isopropylchinolin-8-olato)nickel(II) wurde durch eine Röntgenkristallstrukturuntersuchung bestimmt. Es liegt ein monoklines Kristallsystem mit der Raumgruppe P21/n vor (Z = 2, beobachtete unabhängige Reflexe 1403, R = 4,9%, Gitterabmessungen bei 20°C: a = 1328,3(5) pm, b = 632,8(2) pm, c = 1330,0(5) pm, β = 112,99(3)°). Das Nickelatom ist planar koordiniert mit den beiden Chinolinringen in trans-Stellung.
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    Zur Kristallstruktur von Ba2ZnO3 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 17-20 
    Details
    ISSN: 0044-2313
    Keywords: Barium ; zinc ; oxygen ; 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 Ba2ZnO3Single crystals of Ba2ZnO3 were prepared by solid state reaction. It crystallizes monoclinic: space group C62h — C12/c1; a = 5.833; b = 11.376; c = 12.585 Å; β = 93.63°; Z = 8. The crystal structure is characterised by 1∞[ZnO3] chains along [100]. They are connected by Ba2+ in seven fold oxygen coordination.
    Notes: Ba2ZnO3 wurde durch Festkörperreaktion in einkristalliner Form dargestellt. Es kristallisiert in der Raumgruppe C62h — C12/c1; a = 5,833; b = 11,376; c = 12,585 Å, β = 93,63°; Z = 8. Die Kristallstruktur ist durch 1∞[ZnO3]-Ketten längs [100] gekennzeichnet. Diese werden durch Ba2+ (siebenfach durch O2- koordiniert) verknüpft.
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    Ein neues Oxometallat mit Mangan(II): Ba5Mn4Nd8O21 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 21-24 
    Details
    ISSN: 0044-2313
    Keywords: Barium ; manganese ; neodymium ; oxygen ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On a New Oxometallate of Manganese (II): Ba5Mn4Nd8O21Single crystals of Ba5Mn4Nd8O21 were prepared for the first time by CO2-Laser technique using H2-atmosphere. It was investigated by a single crystal X-ray diffractometer study. Ba5Mn4Nd8O21 crystallizes with tetragonal symmetry space group: C54h—I4/m; a = 14.2104 Å; c = 5.8581 Å; Z = 2. Mn2+ is found in square pyramids of oxygen.
    Notes: Ba5Mn4Nd8O21 wurde erstmals mit CO2-Lasertechnik in H2-Atmosphäre dargestellt und an Einkristallen röntgenographisch untersucht. Es kristallisiert tetragonal in der Raumgruppe C54h—I4/m; a = 14,2104 Å; c = 5,8581 Å; Z = 2. Mn2+ liegt in tetragonal pyramidaler Sauerstoffkoordination vor.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926120105
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    Synthese und Strukturuntersuchungen von Iodocupraten(I). XV Iodocuprate(I) mit solvatisierten Kationen: [Li(CH3CN)4]1∞[Cu2I3] und [Mg{(CH3)2CO}6][Cu2I4] (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 45-50 
    Details
    ISSN: 0044-2313
    Keywords: Iodocuprates(I) ; solvated cations ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure Investigations of Iodocuprates(I). XV Iodocuprate(I) with Solvated Cations: [Li(CH3CN)4]1∞[Cu2I3] and [Mg{(CH3)2CO}6][Cu2I4][Li(CH3CN)4]1∞[Cu2I3] 1 and [Mg((CH3)2CO)6][Cu2I4] 2 were prepared by reactions of CuI with LiI in acetonitrile and of CuI with MgI2 in acetone. 1 crystallizes orthorhombic, Pnma, a = 552.7(2), b = 1258.8(8), c = 2516(1) pm, z = 4. [Li(CH3CN)4]+ cations are located between rod packings of CuI4 tetrahedra double chains 1∞ [(CuI2/2I2/4)2]- parallel to the axis. Short intermolecular anion/cation contacts were observed. The crystal structure of 2 (monoclinic, P21/n, a = 1840(2), b = 1059.2(2), c = 1879(2)pm, β = 112.94(4)°, z = 4) is built up by [Mg((CH3)2CO)6]2+ cations forming a simple hexagonal sphere packing. The binuclear anions [Cu2I4]2- occupy holes in the trigonal prismatic channels formed by the cations.
    Notes: [Li(CH3CN)4]1∞[Cu2I3] 1 und [Mg((CH3)2CO)6][Cu2I4] 2 wurden durch Umsetzung von CuI mit LiI in Acetonitril bzw. von CuI mit MgI2 in Aceton dargestellt. 1 kristallisiert orthorhombisch, Pnma, a = 552,7(2), b = 1258,8(8), c = 2516(1) pm, z = 4. Zwischen Stabpackungen von CuI4-Tetraederdoppelketten 1∞[(CuI2/2I2/4)2]- parallel zur a-Achse sind [Li(CH3CN)4]+ -Kationen unter Ausbildung kurzer, intermolekularer Anionen-Kationen-Kontakte eingelagert. In der Kristallstruktur von 2 (monoklin, P21/n, a = 1840(2), b = 1059,2(2), c = 1879(2) pm, β = 112,94(4)°, z = 4) sind [Mg((CH3)2CO)6]2+ -Kationen in der Art einer hexagonal einfachen Kugelpackung angeordnet. In die dabei gebildeten, trigonal prismatischen Kanäle sind die zweikernigen Anionen [Cu2I4]2- eingebaut.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926120109
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  • 43
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    Vorstufen für polymere Silazane mit Fluoralkyl-Seitenketten und ihr Kondensationsverhalten (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 101-106 
    Details
    ISSN: 0044-2313
    Keywords: (Trifluoroethyl)aminosilane ; silane tetramin; alkylsilazalane ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preliminary Stages of Polymeric Silazanes with Fluoroalkyl Side Chains and their Condensation BehaviourTetrakis(2,2,2-trifluoroethyl)aminosilane has been synthesized by aminolysis of silicon tetrachloride with 2,2,2-trifluorethylamine. The characterisation of the silane tetramine was carried out spectroscopically and by X-ray-methods. The thermal condensation has been investigated between 60°C and 300°C. At 300°C the formation of oligospirocycloorganoazanes was observed which have been identified spectroscopically. The new silane tetramine reacts with trimethylalumina in toluene. The product has been characterized by crystal structure analysis to be a dimeric (C18H26N8F24Si2Al2). (P1; a = 920.39(9), b = 943.32(2), c = 1235.4(1) pm, α = 68.8(7)°, β = 86.9(4)°, γ = 62.6(4)°, Z = 1, 3923 independent reflections; R = 0.059, Rw = 0.054)
    Notes: Tetrakis[(2,2,2-trifluorethyl)amino]-silan wurde durch Aminolyse von Siliciumtetrachlorid mit 2,2,2-Trifluorethylamin dargestellt, spektroskopisch und röntgenographisch charakterisiert, sowie das thermische Kondensationsverhalten im Bereich von 60 - 300°C untersucht. Bei 300°C konnte die Bildung von Oligospirocyclo-silaorganoazanen massenspektrometrisch nachgewiesen werden. Das neu erhaltene Silantetramin wurde bei 80°C mit Trimethylaluminium im Verhältnis 1 : 1 in Toluol umgesetzt. Nach der Kristallstrukturanalyse liegt das erhaltene Alkylsilazalan im Kristall als Dimeres C18H26N8F24Si2Al2 vor. (P1; a = 920,39(9), b = 943,32(2), c = 1235,4(1) pm, α = 68,8(7)°, β = 86,9(4)°, γ = 62,6(4)°; Z = 1, 3923 unabhängige Reflexe, R = 0,059, Rw = 0,054)
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926120117
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  • 44
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    Korrektur zur Kristallstruktur von „Cs4PbO3“ und die Strukturverwandtschaft zwischen den Modifikationen von Cs4PbO4 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 143-148 
    Details
    ISSN: 0044-2313
    Keywords: Caesium tetraoxoplumbate ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Correction of the Crystal Structure of “Cs4PbO3” and the Structural Relationship between the Modifications of Cs4PbO4The compound that has been described as Cs4PbO3 really is Cs4PbO4. It does not crystallize in the space group P21, as assumed, but in P21/c. The observed fictitiuous violation of the extinction law for the c glide plane is due to twinning. The structure was refined using the original data as well as new data from an untwinned crystal. The denomination β-Cs4PbO4 is used to distinguish this structure from another known modification (α-Cs4PbO4). Both structures, α-Cs4PbO4 and β-Cs4PbO4, can be derived from the sphere packing of γ-plutonium when certain voids in its packing are occupied with oxygen atoms.
    Notes: Bei der früher als Cs4PbO3 beschriebenen Substanz handelt es sich tatsächlich um Cs4PbO4. Dieses kristallisiert nicht, wie angenommen, in der Raumgruppe P21, sondern in P21/c. Die beobachtete scheinbare Verletzung des Auslöschungsgesetzes für die c-Gleitspiegelebene ist auf Verzwillingung zurückzuführen. Die Struktur wurde sowohl mit den ursprünglichen Daten wie auch mit neuen Daten eines unverzwillingten Kristalls verfeinert. Die Bezeichnung β-Cs4PbO4 dient zur Unterscheidung von einer bereits bekannten Modifikation (α-Cs4PbO4). Beide Strukturen, α-Cs4PbO4 und β-Cs4PbO4, lassen sich von der des γ-Plutoniums ableiten, wenn bei dieser bestimmte Lücken mit Sauerstoffatomen besetzt werden.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926120124
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  • 45
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    Darstellung und Kristallstruktur von LnAl3Br12 (Ln = La, Ce, Pr, Nd, Sm, Gd) und thermischer Abbau zu LnBr3 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 613 (1992), S. 45-48 
    Details
    ISSN: 0044-2313
    Keywords: Lanthanoide bromoaluminates ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of LnAl3Br12 (Ln = La, Ce, Pr, Nd, Sm, Gd) and Thermal Decomposition to LnBr3LnAl3Br12 (Ln = La, Ce, Pr, Nd, Sm, Gd) was prepared in crystalline form for the first time. The crystal structures of LaAl3Br12, PrAl3Br12, and NdAl3Br12 were determined on single crystals by X-ray methods. The isotypic compounds crystallize with trigonal symmetry, space group P 3112, Z = 3. A structural comparison to lanthanoide chloroaluminates of equal composition is given and thermal decomposition of LnAl3Br12 (Ln = Nd) to the corresponding lanthanoide tribromide is described.
    Notes: Die Bromide LnAl3Br12 (Ln = La, Ce, Pr, Nd, Sm, Gd) wurden erstmals in kristalliner Form dargestellt und die Kristallstrukturen von LaAl3Br12, PrAl3Br12 anhand von röntgenographischen Einkristalluntersuchungen bestimmt. Alle kristallisieren in der trigonalen Raumgruppe P 3112, Z = 3. Ein struktureller Vergleich mit Lanthanoidchloroaluminaten der gleichen Zusammensetzung und der thermische Abbau von LnAl3Br12 (Ln = Nd) zum entsprechenden Lanthanoidtribromid werden beschrieben.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926130107
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  • 46
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    Zur Kristallstruktur von Cu3NbTaO8 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 613 (1992), S. 60-62 
    Details
    ISSN: 0044-2313
    Keywords: Copper ; tantalum ; niobium ; oxygen ; 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 Cu3NbTaO8Single crystals of Cu3NbTaO8 were prepared by solid state reaction. X-ray investigations led to triclinic symmetry, space group C1i—P1 with a = 5.179; b = 5.474; c = 6.003 Å; α = 72.85°; β = 83.39°; γ = 65.77°; Z = 1. Nb5+ and Ta5+ occupy one point position statistically. Both ions show an octahedral oxygen surrounding. Cu(1) is inside an elongated CuO6 octahedra and Cu(2) is coordinated by 5 O2- forming a distorted square pyramid. The polyhedra connection is shown and discussed.
    Notes: Einkristalle von Cu3NbTaO8 wurden durch Feststoffreaktion dargestellt. Die röntgenographische Untersuchung führte zu trikliner Symmetrie, Raumgruppe C1i  -  P1 mit a = 5,179; b = 5,474; c = 6,003 Å; α = 72,85°; β = 83,39°; γ = 65,77°; Z = 1. Nb5+ und Ta5+ besetzen eine Punktlage statistisch. Beide Ionen sind oktaedrisch von O2- koordiniert. Cu(1) zeigt ein stark gestrecktes CuO6-Oktaeder, während Cu(2) tetragonal pyramidal koordiniert ist. Die Polyederverknüpfung wird gezeigt und diskutiert.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926130110
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  • 47
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    Chelatkomplexe von Rheniumtetrachlorid. Die Kristallstrukturen von ReCl4(DME) und ReCl4(DPPE) · Tolan (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 613 (1992), S. 49-54 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium tetrachloride chelate complexes ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chelate Complexes of Rhenium Tetrachloride. The Crystal Structures of ReCl4(DME) and ReCl4(DPPE) · TolanBright green crystals of ReCl4(DME) have been prepared by the reaction of rhenium pentachloride with dimethoxyethane (DME) in dichloromethane. ReCl4(DPPE) · tolan was obtained in form of red crystals by the reaction of the alkyne complex [ReCl4(Ph—C≡C—Ph)(POCl3)] with bis(diphenylphosphino)ethane (DPPE) in dichloromethane. The complexes were characterized by X-ray structure determinations.ReCl4(DME): Space group I42d, Z = 8, 829 observed unique reflexions, R = 0.022. Lattice dimensions at 19.5°C: a = b = 960.60(6), c = 2337.2(6) pm. The complex forms monomeric molecules with DME as chelating ligand; the Re—O bond lengths are 213.1 pm. The chlorine atoms, arranged in trans position to the chelating ligand, have slightly shorter Re—Cl bonds than the chlorine atoms in cis position (232,1 pm).ReCl4(DPPE) · tolan: Space group P21/n, Z = 4,4313 observed unique reflexions, R = 0.040. Lattice dimensions at -80°C: a = 1095.7(1), b = 1764.2(2), c = 1898.0(2) pm, β = 99.229(8)°. The compound consists in form of monomeric molecules [ReCl4(DPPE)] and diphenylacetylene molecules, which are incorporated in the lattice. The two phenyl rings of the tolan molecules are twisted towards each other along the C—C axis with a dihedral angle of 21°. The DPPE molecules are bonded to the rhenium atom in a chelating fashion with medium Re—P lengths of 250.4 pm. The chlorine atoms, arranged in trans position to this ligand, with Re—Cl bond lengths of 234.5 pm are slightly longer than the Re—Cl bonds in cis position with 232.3 pm.
    Notes: ReCl4(DME) wird in Form leuchtend grüner Kristalle durch Reaktion von Rheniumpentachlorid mit Dimethoxyethan (DME) in Dichlormethan hergestellt. ReCl4(DPPE) · Tolan erhielten wir als rote Kristalle bei der Reaktion des Alkinkomplexes [ReCl4(Ph—C≡C—Ph)(POCl3)] mit Bis(diphenylphosphino)ethan (DPPE) in Dichlormethan. Die Komplexe wurden durch röntgenographische Strukturanalysen charakterisiert.ReCl4(DME): Raumgruppe I42d, Z = 8, 829 beobachtete unabhängige Reflexe, R = 2,2%. Gitterkonstanten bei 19,5°C: a = b = 960,60(6); c = 2337,2(6) pm. Der Komplex bildet monomere Moleküle mit dem DME-Liganden als Chelat und Re—O-Abständen von 213,1 pm. Die hierzu trans-ständig angeordneten Chloratome haben mit 228,1 pm etwas kürzere Re—Cl-Bindungen als die cis-ständigen Cl-Atome (232,1 pm).ReCl4(DPPE) · Tolan: Raumgruppe P21/n, Z = 4, 4313 beobachtete, unabhängige Reflexe, R = 4,0%. Gitterkonstanten bei -80°C: a = 1095,7(1); b = 1764,2(2); c = 1898,0(2) pm, β = 99,229(8)°. Der Komplex bildet monomere Moleküle [ReCl4(DPPE)] und in das Gitter eingelagerte Diphenylacetylenmoleküle, deren Phenylringe einen Diederwinkel von 21° zueinander bilden. Die DPPE-Moleküle sind chelatartig am Rheniumatom gebunden mit Abständen Re—P von im Mittel 250,4 pm. Die hierzu trans-ständig angeordneten Chloratome sind mit Re—Cl—Abständen von 234,5 pm etwas länger als die cis-ständigen Re—Cl-Bindungen mit 232,3 pm.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926130108
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    Kristallstrukturverfeinerungen an Natriumtrifluorometallaten NaMF3 (M = Mg, Co, Ni, Zn): Oktaederkippung und Toleranzfaktor orthorhombischer FluorperowskiteProfessor Rudolf Hoppe zum 70. Geburtstage gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 616 (1992), S. 133-140 
    Details
    ISSN: 0044-2313
    Keywords: Sodium trifluorometallates ; fluoroperovskites ; crystal structure ; tolerance factor ; antiferromagnetism ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure Refinements of Sodium Trifluorometallates NaMF3 (M = Mg, Co, Ni, Zn): Tilting of Octahedra and Tolerance Factor of Orthorhombic FluoroperovskitesBased on newly measured X-ray single crystal data the crystal structures of the orthorhombic fluoroperovskites NaMF3 (M = Mg, Co, Ni, Zn) were refined in space group Pbnm (GdFeO3 type, Z = 4). The octahedra are but slightly distorted; the average distances (and bridge angles M—F—M) are: Mg—F = 197.8 pm (150.9°), Co—F = 203.8 pm (146.1°), Ni—F = 200.3 pm (148.0°) and Zn—F = 202.3 pm (147.4°). With respect to the axes of the pseudocell (Z = 1) the octahedra are rotated by tilt angles which vary, including NaMnF3 and NaFeF3, between 14.6 and 18.8°. The tilting becomes the more pronounced, the smaller the tolerance factor of the compound, so as to yield uniformly average values of Na—F = 232 pm for the four shortest distances within the [NaF8] coordination (distorted tetrahedron and bicapped trigonal prism, respectively). Measurements of magnetic powder susceptibilities show that tilting of octahedra is no sufficient cause to produce spin canting resulting in ferromagnetism: This property is confirmed only for NaNiF3 (TN = 150 K), whereas NaCoF3 exhibits a sharp minimum in its χ-l-T curve (TN = 75 K) and remains uncanted antiferromagnetic then down to 4.2 K.
    Notes: Auf der Basis neu gemessener röntgenographischer Einkristalldaten wurden die Kristallstrukturen der orthorhombischen Fluorperowskite NaMF3 (M = Mg, Co, Ni, Zn) in der Raumgruppe Pbnm verfeinert (GdFeO3-Typ, Z = 4). Die Oktaeder sind kaum verzerrt; die mittleren Abstände (und Brückenwinkel M—F—M) betragen: Mg—F = 197,8 pm (150,9°), Co—F = 203,8 pm (146,1°), Ni—F = 200,3 pm (148,0°) und Zn—F = 202,3 pm (147,4°). Unter Einbeziehung von NaMnF3 und NaFeF3 ergeben sich von 14,6 bis 18,8° variierende Kippungswinkel der Oktaeder gegen die Achsen der Pseudozelle (Z = 1). Die Oktaeder sind um so stärker gekippt, je kleiner der Toleranzfaktor der Verbindungen ist, so daß einheitlich ein Mittelwert von Na—F = 232 pm für die vier kürzesten Abstände innerhalb der [NaF8]-Koordination resultiert (verzerrtes Tetraeder bzw. zweifach überkapptes trigonales Prisma). Messungen der magnetischen Pulversuszeptibilität zeigen, daß die Oktaederkippung kein ausreichender Grund für Spinverkantung und daraus resultierenden Ferromagnetismus ist: Dieser kann nur für NaNiF3 (TN = 150 K) bestätigt werden, während NaCoF3 ein scharfes Minimum in der χ-1-T-Kurve zeigt (TN = 75 K) und dann bis herab zu 4,2 K unverkantet antiferromagnetisch bleibt.
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    URL: http://dx.doi.org/10.1002/zaac.19926161020
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    Organoruthenaborane Chemistry. X. The SM2-catalysed formation of [ l-(η6-C6Me6)-isocloso-RuB9H9], and some B-phenylamino derivatives. NMR and X-ray diffraction studiesDedicated to Professor Rudolf Hoppe on his 70th Birthday (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 616 (1992), S. 79-85 
    Details
    ISSN: 0044-2313
    Keywords: Organoruthenaboranes ; ruthenium ; boranes ; n.m.r. spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Organoruthenaboran-Chemie. X. Die SMe2-katalysierte Bildung von [1-(η6-C6Me6)-isocloso-RuB9H9] und einige B-Phenylamino-Derivate. NMR- und Röntgen-UntersuchungenDie Einwirkung von SMe2, auf das zehneckige nido-Ruthenaboran [1-(η6-C6Me6)RuB9H13] (1) führt in hoher Ausbeute zum unsubstituierten isocloso-Ruthenaboran [1-(η6-C6Me6)RuB9H9] (2). Die analoge Verbindung mit Benzol [1-(η6-C6Me6)RuB9H9] wird entsprechend erhalten. Im Gegensatz dazu führt die Reaktion von (1) mit PhNH2 zu einer Reihe von B-Phenylamino-isocloso-Derivaten wie [1-(η6-C6Me6)-2-(PhNH)-isocloso-1-RuB9H8] (3) (orange Kristalle), [1-(η6-C6Me6)-2,3-(PhNH)2-isocloso-1-RuB9H7] (4) (rotorange) und [1-(η6-C6Me6)-5,6,7-(PhNH)3-isocloso-l-RuB9H6] (5) (dunkelrot). Detaillierte 1H- und 11B-NMR-Spektren werden angegeben. Die Struktur von (3) wird durch eine Einkristall-Röntgen-Strukturanalyse des Solvats [1-(η6-C6Me6)-2-(PhNH)-isocloso-1-RuB9H8] · 1/2 CH2C12 ermittelt; die Kristalle sind monoklin, Raumgruppe C2/c, mit a = 1895,1(3), b = 1556,6(3), c = 1716,4(3)pm, β = 104,37(1)° und Z = 8.
    Notes: The action of SMe2 on the ten-vertex nido-ruthenaborane [6-(η6-C6Me6)RuB9Hl3] (1) provides a high-yield route to the unsubstituted isocloso-ruthenaborane [1-(η6-C6Me6)RuB9H9] (2). The benzene analogue [1-(η6-C6Me6)RuB9H9] is prepared similarly. By contrast, reaction of (1) with PhNH2 gives a variety of B-phenylamino isocloso derivatives, including orange crystals of [1-(η6-C6Me6)-2-(PhNH)-isocloso-1-RuB9H8] (3), red-orange [1-(η6-C6Me6)-2,3-(PhNH)2-isocloso-1-RuB9H7] (4) and dark-red [1-(η6-C6Me6)-5,6,7-(PhNH)3-isocloso-1-RuB9H6] (5). Detailed 1H and 11B nmr properties of these various compounds are described. The structure of (3) has been established by a single-crystal X-ray diffraction study of the solvate [1-(η6-C6Me6)-2-(PhNH)-isocloso-1-RuB9H8] · 1/2 CH2Cl2; the crystals were monoclinic, space group C2/c, with a = 1895.1(3), b = 1556.6(3), c = 1716.4(3) pm, β = 104.37(1)° and z = 8.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926161013
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  • 50
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    Temperaturabhängige Phasenumwandlungen natriumreicher AmalgameProfessor Rudolf Hoppe zum 70. Geburtstage gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 616 (1992), S. 35-38 
    Details
    ISSN: 0044-2313
    Keywords: Amalgams ; sodium-rich amalgams ; phase transitions ; crystal structure ; DTA measurements ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Temperature Dependent Phase Transitions of Sodium-rich AmalgamsStarting from thermoanalytical measurements the temperature dependent phase transitions of the microcrystalline, sodium rich amalgams Na8Hg3 (= Na2.67Hg) and Na3Hg are investigated using a fast, position sensitive X-Ray detector in combination with a modified counter Guinier system. Near the melting point (64°C) Na8Hg3 shows two phase transitions.At 54°C α-Na8Hg3 forms a slightly distorted monoclinic defect variant of the cubic Li3Bi-structure (β-Na8Hg3). At 62°C this modification transforms into the corresponding undistorted cubic phase (γ-Na8Hg3). The increase of symmetry results mainly from the fact, that small deviations of the mercury atoms from the positions of an ideal close packing vanish due to strong thermal vibrations.The “literature-melting point” of Na3Hg (33°C) corresponds to a phase transition from α-Na3Hg (hexagonal, modified Na3As type) into β-Na3Hg (monoclinic distorted Li3Bi type, corresponding to β-Na8Hg3). The actual melting point of Na3Hg is 59°C.
    Notes: Ausgehend von thermoanalytischen Messungen werden die temperaturabhängigen Phasenumwandlungen der mikrokristallinen natriumreichen Amalgame Na8Hg3 (Na2.67Hg) und Na3Hg mit einem schnellen, ortsempfindlichen Röntgendetektor in Kombination mit einer modifizierten Zählrohr-Guinierkamera untersucht. Na8H3 zeigt dicht unter dem Schmelzpunkt (64°C) zwei Phasenumwandlungen: Bei 54°C wandelt sich α-Na8Hg3 zunächst in eine monoklin verzerrte Defektvariante (β-Na8Hg3) der kubischen Li3Bi-Struktur um. Daraus entsteht bei 62°C die entsprechende unverzerrte kubische Phase (γ-Na8Hg3). Die Symmetrieerhöhung resultiert aus der Aufhebung geringfügiger Abweichungen der Hg-Atompositionen von einer dichtesten Kugelpackung infolge starker thermischer Schwingung.Der „Literaturschmelzpunkt“ von Na3Hg (33°C) entspricht einer Phasenumwandlung von α-Na3Hg (hexagonal, modifizierte Na3As-Struktur) in β-Na3Hg (monoklin verzerrter Li3Bi-Typ, entsprechend β-Na8Hg3). Der Schmelzpunkt der Verbindung Na3Hg liegt dagegen tatsächlich bei 59°C.
    Additional Material: 1 Ill.
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    Zur Kenntnis von Ba6Ru2PtO12Cl2 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 59-62 
    Details
    ISSN: 0044-2313
    Keywords: Ruthenium ; oxygen ; chlorine ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: About Ba6Ru2PtO12Cl2Single crystals of Ba6Ru2PtO12Cl12 were prepared by a BaCl2 flux and investigated by X-ray methods (D3d3—P3M1; a = 5,805; c = 15.006 Å; Z = 1). The characteristic face shared M3O12-octahedratriples show an ordered (Ru/Pt/Ru) occupation. Calculation of the Coulomb term of lattice energy support the charge distribution (5+/4+/5+) ions engage three point sites with different coordinations. The connection to other compounds are discussed.
    Notes: Durch Schmelzmittelreaktion mit BaCl2 wurde Ba6Ru2PtO12Cl2 an Einkristallen dargestellt und röntgenographisch untersucht (D3d3-P3m1; a = 5,805; c = 15,006 Å; Z = 1). Die charakteristischen flächenverknüpften M3O12-Oktaedertripel weisen eine geordnete Besetzung mit Ru/Pt/Ru auf. Berechnungen des Coulombanteils zur Gitterenergie unterstützen eine Ladungsverteilung in den M3O12-Baugruppen von (5+/4+/5+). Ba2+ -Ionen besetzen drei Punktalgen mit jeweils unterschiedlicher Koordination. Der Zusammenhang mit anderen Strukturen wird diskutiert.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926090311
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  • 52
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    Crystal and magnetic structures of the layer Compound TlMnF4 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 71-76 
    Details
    ISSN: 0044-2313
    Keywords: Thallium tetrafluoromanganate(III), TlMnF4 ; crystal structure ; magnetic structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kristall- und magnetische Struktur von TlMnF4, einer Verbindung mit SchichtstrukturDie Kristallstruktur und die magnetischen Eigenschaften des Fluoromanganates(III) TlMnF4 wurden untersucht. Die Struktur wurde in der monoklinen Raumgruppe I2/a, Elementarzelle mit a = 539,7(2); b = 544,1(2); c = 1248,4(5) pm, β = 90,19(3)° (Z = 4) auf R/wR 0,057/0,043 verfeinert. TlMnF4 zeigt eine Schichtstruktur, die durch Eckenverknüpfung von MnF6-Oktaedern über ihre vier äquatorialen Ecken gebildet wird. Die Mn—F-Abstände innerhalb des Oktaeders liegen im Bereich von 178 bis 215 pm. Die magnetische Austauschenergie (J/K) innerhalb der Schicht wurde durch Anpassung der experimentellen Suszeptibilitätsdaten im Temperaturbereich von 10-300 K auf der Basis des Heisenbergmodells für quadratische Schichten zu -0,45 K bestimmt. Dreidimensionale antiferromagnetische Ordnung tritt bei 4,2(5) K ein. Die magnetische Zelle entspricht der kristallographischen, jedoch mit primitivem Translationsgitter. Die magnetische Struktur wurde auf R = 0,058 in der magnetischen Raumgruppen P2′/a′ verfeinert. Die magnetischen Momente an MnIII sind colinear zur b-Achse und zeigen antiparallele Ordnung innerhalb der Schichten.
    Notes: The crystal structure and the magnetic properties of the fluoromanganate(III) TlMnF4 have been investigated. The structure has been refined down to R/wR of 0.057/0.043 in the monoclinic I2/a space group with the unit cell constants a = 539.7(2) pm; b = 544.1(2) pm; c = 1248.4(5) pm; β = 90.19(3)° (Z = 4). TlMnF4 is characterized by a layer structure formed of MnF6 octahedra sharing their four equatorial corners. Within each octahedron the Mn—F distances range from 178 pm to 215 pm. The intralayer magnetic interaction (J/K) has been evaluated to be approximately -0.45 K by fitting the experimental susceptibility in the 10-300 K range using the quadratic layer Heisenberg model. A 3 D-antiferromagnetic ordering occurs at Tn = 4.2(5) K. The magnetic cell corresponding to the nuclear one but with a primitive symmetry. The magnetic structure has been refined down to R = 0.0528 in the P2′/a′ magnetic group. The MnIII moments are colinear to the b-axis and show antiparallel ordering within the layers.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926090314
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    Über Perrhenate. 3über Perrhenate. 2  -  siehe [4]. Zum Aufbau des Mesoperrhenates Na3[ReO5]Herrn Dr. Werner Hanke zum 60. Geburtstage am 14. April 1992 gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 7-14 
    Details
    ISSN: 0044-2313
    Keywords: Na3ReO5 ; crystal structure ; ReO5 groups ; Na3Re frame analogous to Li3Bi type ; MAPLE of perrhenates ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: About Perrhenates. 3 On the Structure of the Mesoperrhenate Na3[ReO5]By tempering powder samples (prepared from mixtures of binary oxides: Na2O2/ReO2 and Na2O/ReO3 respectively, Na : Re = 3 : 1, Ar and O2 atmosphere respectively, 400-450°C, corundum boat) in a closed Ag cylinder (500-550°C, 10 d) yellow single crystals of Na3ReO5, sensitive to moisture, were grown. The compound crystallizes trigonal, space group P31, P32 respectively, with a = 5.544(1), c = 13.580(7) Å, Z = 3, drö. = 4.62 g/cm3. The crystal structure [4-circle diffractometer data, 1091 I0(hkl), AgKα, R = 6.14, Rw = 6.08%] is characterized by “isolated” bipyramids ReO5. Na+ ions are occupying all the tetrahedral (Na2, Na3) and octahedral (Na1) holes of the pseudocubic face centred (c/a = 2.441) Re part of the lattice; resulting in a Na3Re kation framework corresponding to the Li3Bi type of structure. Effective Coordination Numbers (ECoN), the Madelung Part of Lattice energy (MAPLE) and the charge distribution (CHARDI) are computed and discussed.
    Notes: Durch Tempern von Pulverproben (erhalten aus Gemengen binärer Oxide: Na2O2/ReO2 bzw. Na2/ReO3, Na : Re = 3 : 1, Ar- bzw. O2-Atmosphäre, 400-450°C, Korundschiffchen) in verschlossenen Ag-Bomben (500-550°C, 10 d) wurden feuchtigkeitsempfindliche, gelbe Einkristalle von Na3ReO5 gezüchtet, die trigonal, Raumgruppe P31 bzw. P32, mit a = 5,544(1), c = 13,580(7) Å, Z = 3, drö. = 4,62 g/cm3 kristallisieren. Die Kristallstruktur [4-Kreisdiffraktometerdaten, 1091 I0(hkl), AgKα, R = 6,14, Rw= 6,08%] zeigt “isolierte” Bipyramiden ReO5.Na+ besetzt Tetraeder-(Na2, Na3) und Oktaeder-(Na1) Lücken des pseudokubisch-flächenzentrierten (c/a = 2,449) Re-Teilgitters; das Na3Re-Kationengerüst entspricht somit dem Li3Bi-Typ. Effektive Koordinationszahlen (ECoN), der Madelunganteil der Gitterenergie (MAPLE) sowie die Ladungsverteilung (CHARDI) werden berechnet und diskutiert.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926100102
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    Synthese, Kristallstruktur und thermischer Abbau von Cs1,5[Re3I3Cl7,5(H2O)1,5] (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 15-19 
    Details
    ISSN: 0044-2313
    Keywords: Mixed ternary ReIII-halides ; synthesis ; crystal structure ; infrared spectroscopy ; thermal behaviour ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Crystal Structure and Thermal Behaviour of Cs1,5[Re3I3Cl7,5(H2O)1,5]Dark brown tetrahedra of Cs1,5[Re3I3Cl7,5(H2O)1,5] crystallize on slow cooling of a hot saturated solution of ReI3 and CsCl in conc. hydrochlorid acid. The crystal structure (cubic, P43m (No. 215), a = 1241.06(3)pm, Vm = 287.8(1) cm3mol-1, Z = 4, R = 0.067, Rw = 0.037) is built up from isolated building units [Re3I3Cl7,5(H2O)1,5]1,5- with statistical distribution of chloride ions and water molecules in the in plane, terminal positions. Consistent with the result based on the X-ray analysis, the IR-spectrum shows one band for the OH stretching frequencies of the water molecules coordinated to the Re3 triangle at 3240 cm-1. The anions are arranged in the fashion of a cubic closest packing with the cesium ions occupying all octahedral and one quarter of the tetrahedral interstices. Temperature-dependent Guinier-Simon photographs in connection with DTA/TG investigations reveal that Cs1,5[Re3I3Cl7,5(H2O)1,5] releases water at 190°C accompanied with a structural transition and the dehydration product decomposes at 370°C to Cs2ReCl6-xIx, Re3I3+yCl6-y and rhenium metal.
    Notes: Tiefdunkelbraune Tetraeder von Cs1,5[Re3I3Cl7,5(H2O)1,5] Kristallisieren beim langsamen Eindunsten einer heißen, gesättigten Lösung von ReI3 und CsCl in konz. Salzsäure. In der Kristallstruktur (kubisch, P43m (Nr. 215), a = 1241,06(3) pm, Vm = 287,8(1) cm3mol-1, Z = 4, R = 0,067, Rw = 0,037) sind isolierte Baugruppen [Re3I3Cl7,5(H2O)1,5]1,5- mit statistischer Verteilung von Chlorid-Ionen und Wassermolekülen in den in plane, terminal-Positionen strukturbestimmend. übereinstimmend mit diesem röntgenographischen Befund beobachtet man im IR-Spektrum eine Bande für die Valenzschwingungen des Koordinationswassers bei 3240 cm-1. Die Anionen sind nach dem Motiv einer kubisch-dichtesten Packung angeordnet, die Caesium-Ionen besetzen in ihr sämtliche Oktaeder- und ein Viertel der Tetraederlücken. Heiz-Guinier-Simon-Aufnahmen und DTA/TG-Untersuchungen zeigen, daß Cs1,5[Re3I3Cl7,5(H2O)1,5] bei 190°C zunächst Koordinationswasser unter Änderung der Struktur abgibt und sich bei 370°C zu Cs2ReCl6-xIx, Re3I3+yCl6-y und Rhenium zersetzt.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926100103
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  • 55
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    A4N2O5 (A = Na, K), neue Oxidnitrite der Alkalimetalle und eine Bemerkung zum quasi-binären System K3NO3/K3OBr (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 28-32 
    Details
    ISSN: 0044-2313
    Keywords: Alkali metal oxide nitrites ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A4N2O5 (A = Na, K) Novel Alkali Metal Oxide Nitrites, and a Comment on the System K3NO3/K3OBrK4N2O5 and Na4N2O5 have been prepared for the first time: the respective alkali metal nitrites and -oxides in molar ratios 2 : 1 have been reacted in the solid state. Their crystal structure (for crystallographic data see „Inhaltsübersicht“) derive from the anti-K2NiF4 type of structure. Na4N2O5 undergoes two phase transitions (at -15°C and -60°C) upon cooling.The behavior of solid solutions in the system K3NO3/K3OBr at cooling gives support for the phase transition being driven by the OK3-framework, where as in Na3NO3 order-disorder transitions of the NO2- group seem to induce the phase transitions.
    Notes: K4N2O5 und Na4N2O5 wurden erstmals erhalten durch Festkörperreaktionen der entsprechenden Alkalimetallnitrite und Alkalimetalloxide im Mol-Verhältnis 2 : 1. Die Kristallstrukturen (K4N2O5: I4/m; a = 520,4(2), c = 1592,6(8) pm; 150 Reflexe; R = 0,035. Na4N2O5: Pulverdaten; a = 457,2(1), 903,5(1), 1495,3(3) pm; orthorhombisch) leiten sich von dem anti- K2NiF4-Typ ab. Na4N2O5 durchläuft zwei Phasentransformationen bei -15°C und -60°C.Das Tieftemperaturverhalten der Mischkristalle im quasibinären System K3NO3/K3OBr (vollständige Mischbarkeit) stützt die Auffassung, daß die Phasenumwandlung durch das OK3-Gerüst getrieben wird, während dafür in Na3NO3 Ordnungs-Unordnungsübergänge der NO2--Anionen verantwortlich sind.
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    URL: http://dx.doi.org/10.1002/zaac.19926100106
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    Quecksilberverbindungen mit Cyancarbanionen. II. Synthese und Kristallstruktur von Diquecksilber(I)-bis(1,1,3,3-tetracyanpropenid) (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 46-50 
    Details
    ISSN: 0044-2313
    Keywords: Mercury compounds ; dimercury(I)-bis-(1,1,3,3-tetracyanpropenide) ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Mercury Compounds with Cyancarbanions. II Synthesis and Crystal Structure of Dimercury(I)-bis(1,1,3,3-tetracyanpropenide)The structure of dimercury(I)-bis(1,1,3,3-tetracyanpropenide), Hg2(tcp)2, has been determined by single-crystal X-ray diffraction methods. The crystals are monoclinic, space group P 21/n. The unit cell dimensions are: a = 9.9193(3) Å, b = 5.6912(6) Å, c = 13.3806(4), β = 92.544(4)° and Z = 2. The mercury atoms in the centrosymmetric cation are three-coordinate with Hg—Hg 2.503, Hg—N 2.207, 2.207, 2.560 Å. tcp behaves as a bidentate ligand forming infinite chains running parallel to the a-axis.
    Notes: Die Struktur von Diquecksilber(I)-bis(1,1,3, 3-tetracyanpropenid), Hg2(tcp)2, wurde durch Einkristall-Röntgenstrukturanalyse ermittelt. Die Kristalle sind monoklin, Raumgruppe P 21/n. Die Zelldimensionen sind a = 9,9193(3) Å, b = 5,6912(6) Å, c = 13,3806(4) Å, β = 92,544(4)° und Z = 2. Die Quecksilberatome im zentrosymmetrischen Kation werden dreifach koordiniert mit Hg—Hg 2,503; Hg—N 2,207; 2,560 Å. tcp fungiert als zweizähniger Ligand unter Ausbildung unendlicher Ketten parallel zur a-Achse.
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    URL: http://dx.doi.org/10.1002/zaac.19926100108
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    Verfeinerung der Kristallstruktur von K2O2 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 64-66 
    Details
    ISSN: 0044-2313
    Keywords: Dipotassium peroxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Refinement of the Crystal Structure of K2O2The crystal structure of K2O2 has been refined using 241 diffractometer data (Cmca; a = 6.733(1), b = 6.996(1), c = 6.474(1) Å; Z = 4; Rw = 0.050). The distance O—O (1.541(6) Å) is significantly larger than that one assumed for alkali metal peroxides, so far.
    Notes: Die Kristallstruktur von K2O2 wurde auf der Basis von Vierkreisdiffraktometerdaten (241 unabhängige Strukturfaktoren) verfeinert (Cmca; a = 6,733(1), b = 6,996(1), c = 6,474(1) Å; Z = 4; Rw = 0.050). Der gefundene O—O-Abstand weist mit 1,541(6) Å einen deutlich größeren Wert auf als bisher für die Alkalimetallperoxide angenommen.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926100111
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    Copper Weberites: Crystal Structure and Magnetic Investigation of Na2CuGaF7 and Na2CuInF7 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 67-74 
    Details
    ISSN: 0044-2313
    Keywords: Copper weberites, Na2CuGaF7, Na2CuInF7 ; crystal structure ; magnetic investigation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kupferweberite: Kristallstruktur und magnetische Untersuchung von Na2CuGaF7 und Na2CuInF7Die Kristallstruktur von zwei neuen Kupferweberiten Na2CuGaF7 und Na2CuInF7 wurde bestimmt. Na2CuGaF7: monokline Raumgruppe C2/c; a = 1232,5(5), b = 731,8(1), c = 1278,0(5) pm, β = 109,29(2)°, Z = 8. Na2CuInF7: orthorhombische Raumgruppe Pmnb; a = 731,8(1) pm, b = 1060,2(2) pm, c = 771,2(1) pm Z = 4. Die Strukturen wurden verfeinert mit 1175 Reflexen bis zu R = 0,043 (wR = 0,035) für Na2CuGaF7 und mit 1917 Reflexen bis zu R = 0,034 (wR = 0,025) für Na2CuInF7. Die Strukturen bestehen aus [CuF5]n3n--Ketten, die im Na2CuInF7 parallel zur a-Achse orientiert sind und in zwei alternierenden Richtungen im Na2CuGaF7. Die Natriumatome besitzen entweder siebenfache oder achtfache Koordination. Obwohl starke antiferromagnetische Wechselwirkungen innerhalb der Ketten beobachtet werden, gibt es keine Hinweise auf eine dreidimensionale Ordnung.
    Notes: The crystal structures of two new copper weberites Na2CuGaF7 and Na2CuInF7 have been determined. Na2CuGaF7 has the monoclinic space group C2/c: a = 1232.5(5) pm, b = 731.8(1) pm, c = 1278.0(5) pm, β = 109.29(2)° and Z = 8. Na2CuInF7 crystallizes in the orthorhombic space group Pmnb: a = 731.8(1) pm, b = 1060.2(2) pm, c = 771.2(1) pm and Z = 4. The structures have been refined from 1175 reflections to R = 0.043 (wR = 0.035) for Na2CuGaF7, and from 1917 reflections to R = 0.034 (wR = 0.025) for Na2CuInF7. The structures consist of [CuF5]n3n- chains which are parallel the a-axis in Na2CuInF7 and oriented in two alternating directions in Na2CuGaF7. Sodium atoms exhibit either seven-fold or eight-fold coordination. Although strong antiferromagnetic interactions are observed inside the chains, there is no evidence for three-dimensional ordering.
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    URL: http://dx.doi.org/10.1002/zaac.19926100112
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    Quecksilberverbindungen mit Cyancarbanionen. I. Synthese und Kristallstruktur von Diquecksilber(I)-bis(tricyanmethanid)Herrn Professor Wolfgang Beck zum 60. Geburtstage am 5. Mai 1992 gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 29-34 
    Details
    ISSN: 0044-2313
    Keywords: Mercury compounds ; dimercury(I)-bis(tricyanmethanide) ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Mercury Compounds with Cyancarbanions. I . Synthesis and Crystal Structure of Dimercury(I)-bis(tricyanmethanide)With the triclinic unit cell, space group P1, with the lattice constants a = 5.2794(1) Å, b = 9.9279(1) Å, c = 11.3376(2) Å, α = 71.004(4)°, β = 76.459(2)° and γ = 74.601(4)° are two formula units. The three-dimensional network, which characterizes the structure, results from dimercury(I) ions with sp3 hybridization, which form beside the homonuclear metal bonding three covalent bonds to cyanonitrogen atoms. The tricyanmethanide ion acts by losing symmetry as a tridentate ligand.
    Notes: Innerhalb der triklinen Elementarzelle, Raumgruppe P1, mit den Gitterkonstanten a = 5,2794(1) Å, b = 9,9279(1) Å, c = 11,3376(2) Å, α = 71,004(4)° und β = 74,601(4)° befinden sich zwei Formeleinheiten. Das den Strukturaufbau charakterisierende dreidimensionale Netzwerk resultiert aus sp3-hybridisierten Diquecksilber(I)-ionen, die neben der homonuklearen Metallbindung drei weitere kovalente Bindungen zu Cyanstickstoffatomen ausbilden. Das Tricyanmethanidion wirkt unter Symmetrieverlust als dreizähniger Ligand.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926090305
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    Darstellung und NMR-spektroskopische Untersuchungen der tert-Butylimino-cyclopentadienylvanadium (V)-Verbindungen tC4H9N=VCpX2 (X=SR, SeC6H5, Br, I)Herrn Professor Paul Binger zum 60. Geburtstage gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 45-50 
    Details
    ISSN: 0044-2313
    Keywords: Thiolato ; selenolato ; bromo ; iodo complexes of vanadium(V) ; 1H, 51V NMR ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and NMR Spectroscopic Studies of tert-Butylimino-cyclopentadienylvanadium(V) Compounds tC4H9N=VCpX2 (X=SR, SeC6H5, Br, I)Syntheses of the cyclopentadienylvanadium(V) compounds tC4H9N=VCpX2 (X=SR, SeC6H5, Br, I) tC4H9N=VCp (StC4H9) and tC4H9N=VCp[S—(CH2)3—S] (4) are described starting from tC4H9N=VCpCl2. tC4H9N=VCl3 reacts with BBr3 and BI3 by halogen exchange forming the trihalogenides tC4H9N=VX3 (X=Br, I). All compounds obtained are characterized by 1H and 51V NMR spectroscopy. 4 has been found by X-ray diffraction analysis to be a distorted tetrahedral vanadium complex with a chair conformation of the VS2C3-ring.
    Notes: Die Darstellung der Cyclopentadienyl-vanadium(V)-Verbindungen tC4H9N=VCpX2 (X=SR, SeC6H5, Br, I), tC4H9N=VCp(StC4H9) und tC4H9N=VCp[s—(CH2)3—S] (4) wird beschrieben; als Ausgangsverbindung wird tC4H9N=VCpCI2 eingesetzt. tC4H9N=VCl3 reagiert mit BBr3 und Bl3 unter Halogenaustausch und Bildung der Trihalogenide tC4H9N=VX3 (X=Br, I). Alle dargestellten Verbindungen werden 1H- und 51V-NMR-spektroskopisch charakterisiert. Die Röntgenstrukturanalyse von 4 zeigt das Vanadiumatom in einer verzerrt tetraedrischen Anordnung der Liganden; der VS2C3-Ring liegt in der Sesselkonformation vor.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926090308
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    Zur Reaktion von Makrozyklen mit Lanthanoiden. I. Die Struktur von [Li(thf)][(C22H22N4)2Ce] · THF (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 77-80 
    Details
    ISSN: 0044-2313
    Keywords: CeIII double decker 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 Macrocycles with Lanthanoids. I. The Crystal Structure of [Li(thf)][(C22H22N4)2Ce] · THFIn THF CeBr3 forms with [(TMTAA)Li2] the paramagnetic doubledecker complex [Li(thf)][(TMTAA)2Ce]. The complex crystallizes with 1 Mol THF per formula unit. The structure was characterized by X-ray single crystal structure analysis (space group C2 (No. 5), z = 6, a = 1741.8(2) pm, b = 1622.1(2) pm, c = 2540.4(3) pm, β = 104.72(1)°). The sandwich-like arrangement of the heterocyclic ligands leads to a quadratic-prismatic coordination of the Ce3+ ion. One macrocyclic ligand is additionally coordinated by a [Li(thf)]+ fragment. The coordination of the Li ion is square pyramidal.
    Notes: CeBr3 reagiert mit [(TMTAA)Li2] in THF zu dem paramagnetischen Doppeldeckerkomplex [Li(thf)][(TMTAA)2Ce], der mit 1 Mol THF pro Formeleinheit kristallisiert. Der Aufbau konnte durch eine Kristallstrukturanalyse aufgeklärt werden (Raumgruppe C2 (Nr. 5), Z = 6, a = 1741,8(2) pm, b = 1622,1(2) pm, c = 2540,4(3) pm, β = 104,72(1)°). Durch die sandwichartige Anordnung der TMTAA-Liganden erhält das Ce3+-Ion eine quadratisch-prismatische Koordination. An einen der makrozyklischen Liganden koordiniert zusätzlich ein [Li(thf)]+-Fragment. Das Li-Ion besitzt tetragonal-pyramidale Umgebung.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926150915
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    Zur Reaktion von Makrozyklen mit Lanthanoiden. II. Die Strukturen von [K(thf)3]2[(C22H28N4)2Sm2] · 4THF und [(C22H22N4)Co] · DME (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 81-85 
    Details
    ISSN: 0044-2313
    Keywords: SmIII polynuclear complex ; CoII 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 Macrocycles with Lanthanoids. II. The Crystal Structures of [K(thf)3]2[(C22H28N4)2Sm2] · 4 THF and [(C22H22N4)Co] · DMEIn a complicated redox reaction [(TMTAA)K2] and [SmI2(thf)2] form the polynuclear metal complex [K(thf)3]2[(TMTAT)2Sm2]. This complex crystallizes with four molecules THF per formula unit and its structure was determined by single crystal X-ray investigation (spacegroup P21/c (No. 14), z = 4, a = 998.0(2) pm, = b = 2618.3(6) pm, c = 1619.4(3) pm, β = 96.52(2)°). In the dimeric unit [(TMTAT)2Sm2]2- the Sm3+ ions are bonded to the four N atoms of the macrocyclic ligand and one C6H4 ring of the second ligand is attached η6 like to one metal ion. Additionally two [K(thf)3]+ fragments are bonded to this central unit, and therefor coordination number seven results for the K+ ion. [TMTAA]2- is not reduced by [Cp2Co] in a similar reaction. The monomeric paramagnetic complex [(TMTAA)Co] (μeff = 2,76 μB) is formed instead. The structure reveils a square planar coordination of the Co atom by the four N atoms of the TMTAA ligand (spacegroup C2/c (No. 15), z = 4, a = 1945.1(4) pm, b = 1165.6(2) pm, c = 1144.7(2) pm, β = 116.38(1)°).
    Notes: [(TMTAA)K2] und [SmI2(thf)2] reagieren in einer unübersichtlichen Redoxreaktion zu dem mehrkernigen Metallkomplex [K(thf)3]2[(TMTAT)2Sm2]. Der Aufbau dieser mit vier Molekülen THF pro Formeleinheit kristallisierenden Verbindung konnte durch eine Röntgenstrukturanalyse aufgeklärt werden (Raumgruppe P21/c (Nr. 14), Z = 4, a = 998,0(2) pm, b = 2618,3(6) pm, c = 1619,4(3) pm, β = 96,52(2)°). In der dimeren Einheit [(TMTAT)2Sm2]2- sind die Sm3+-Ionen außer an die vier N-Atome eines makrozyklischen Liganden auch η6-artig an einen C6H4-Ring des zweiten Liganden gebunden. Zusätzlich koordinieren an die zentrale Einheit zwei [K(thf)3]+-Fragmente. Dies führt zu einer Koordinationszahl von 7 für das K+-Ion. [TMTAA]2- wird in einer analogen Reaktion mit [Cp2Co] nicht reduziert. Statt dessen bildet sich der monomere paramagnetische Komplex [(TMTAA)Co] (μeff = 2,76 μB). Nach der Kristallstrukturanalyse ist das Co-Atom quadratisch planar von den vier N-Atomen des TMTAA-Liganden koordiniert (Raumgruppe C2/c (Nr. 15), Z = 4, a = 1945,1(4) pm, b = 1165,6(2) pm, c = 1144,7(2) pm, β = 116,38(1)°).
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926150916
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    Cadmium iodide complexes with dimethylsulphoxide, and their crystal structures (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 143-148 
    Details
    ISSN: 0044-2313
    Keywords: Cadmium iodide dimethylsulfoxide complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cadmiumiodid-Komplexe mit Dimethylsulfoxid und ihre KristallstrukturenEinkristalldaten der Verbindungen [{CdI2(dmso)}n] (1,) und [Cd2I4(dmso)4] (2,) zeigen, daß mit steigendem Anteil von dmso Übergang zu ionischen Species wie [Cd(dmso)6]2+ [Cd(dmso)I3]2- · EtOH (3,) und [Cd(dmso)6]2+ [CdI4]2- (4,) erfolgt. Bei (1,) liegen polymere Ketten mit Cd2+ der CN 4 bzw. 6 vor, wobei I- überbrückt. Die Ketten von (2,) weisen ein bi-nukleares Segment auf und sind als Vorläufer der typisch ionischen Stoffe (3,) bzw. (4,) aufzufassen. Wegen der lockeren Packung der konstituierenden Ionen in (3,) ist Ethanol eingebaut.
    Notes: The crystalline compounds [{CdI2(dmso)}n] (1,) and [Cd2I4(dmso)4] (2,) provide a structural sequence illustrating the conversion of CdI2 into the ionic derivatives [Cd(dmso)6]2+ [Cd(dmso)I3]2- · EtOH (3,) and [Cd(dmso)6]2+ CdI42- (4,), with increasing proportions of dmso. (1,) comprises polymeric chains with Cd centres linked by bridging iodide atoms, and alternately in four- and six-coordination. (2,) is a binuclear segment of the chains and can be seen as the structural forerunner of the ionic compounds (3,) and (4,). The ion packing in (3,) is loose, with lattice ethanol.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926150929
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  • 64
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    Untersuchungen über Zinn(IV)-alkoxide. II. Isolierung und Charakterisierung der Verbindung Sn3O(OiBu)10 · 2i-BuOH. Das erste Beispiel für ein partielles Hydrolyseprodukt eines Zinn(IV)-alkoxids (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 137-142 
    Details
    ISSN: 0044-2313
    Keywords: Tin(IV) alkoxides ; partially hydrolized tin(IV) alkoxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Investigations into Tin(IV) Alkoxides. II. Isolation and Characterization of the Compound Sn3O(OiBu)1010 · 2i-BuOH. The First Example of a Partially Hydrolized Tin(IV) AlkoxideThe partial hydrolysis product Sn3O(OiBu)10 · 2i-BuOH was obtained by slow hydrolysis of the reaction product of tin tetrachloride with sodium isobutoxide. The compound forms colourless, moisture sensitive crystals, which easily release the coordinated solvent molecules in dry air. Its crystal and molecular structure has been determinated by single crystal X-ray diffraction. The compound crystallizes in the triclinic space group P1 with a = 1363.5(7), b = 1462.7(10), c = 1637.7(7) pm, α = 95.40(5)°, β = 96.79(4)°, γ = 102.12(5)° and Z = 2. The crystal structure consists of discrete, trimeric molecules with octahedrally coordinated tin atoms which are connected to each other corresponding to the formulation Sn3(μ3-O)(μ2-OiBu)3(O1Bu)7 · (i-BuOH)2 by three isobutoxide groups bridging two metal atoms and a single threefold bridging oxygen atom
    Notes: Das partielle Hydrolyseprodukt Sn3O(OiBu)10 · 2i-BuOH des Zinn(IV)-isobutanolats wurde bei der schonenden Hydrolyse des Reaktionsproduktes von Zinntetrachlorid mit Natriumisobutanolat erhalten. Die Verbindung bildet farblose, feuchtigkeitsempfindliche Kristalle, die in trockener Luft unter Abspaltung der Lösungsmittelmoleküle rasch verwittern. Die Kristall- und Molekülstruktur wurde durch Röntgenstrahlbeugung an einem Einkristall bestimmt. Die Verbindung kristallisiert in der triklinen Raumgruppe P1 mit den Gitterkonstanten a = 1363,5(7), b = 1462,7(10), c = 1637,7(7) pm, α = 95,40(5)°, β = 96,79(4)°, γ = 102,12(5)° und Z = 2. Die Kristallstruktur besteht aus diskreten, trimeren Molekülen, in denen die oktaedrisch koordinierten Zinnatome entsprechend der Formulierung Sn3(μ3-O)(μ2-OiBu)3(OiBu)7(i-BuOH)2 über drei, je zwei Metallatome verbrückende Isobutanolat-Gruppen und ein einzelnes dreifach verbrückendes Sauerstoffatom miteinander verbunden sind.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926150928
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    Darstellung, Struktur und magnetische Eigenschaften der Natriumeisenchalkogenide Na6FeS4 und Na6FeSe4Professor Rudolf Hoppe zum 70. Geburtstage gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 616 (1992), S. 14-18 
    Details
    ISSN: 0044-2313
    Keywords: Sodium iron chalcogenides, Na6FeS4, Na6FeSe4 ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Structure, and Magnetic Properties of the Sodium Iron Chalcogenides Na6FeS4 and Na6FeSe4The compounds Na6FeS4 and Na6FeSe4 have been synthesized by fusion reactions of sodium carbonate with iron and chalcogen in a stream of hydrogen.Structural investigations on single crystals show that both compounds crystallize in an atomic arrangement isotypic with Na6ZnO4 (space group P63mc). The structure is characterized by isolated [FeX4]-tetrahedra.The magnetic susceptibilities show Curie-Weiss behaviour. The deviations at low temperatures are obviously caused by antiferromagnetic interactions.
    Notes: Durch Schmelzreaktionen von Natriumcarbonat mit Eisen und Chalkogen im Wasserstoffstrom gelang die Darstellung von Na6FeS4 und Na6FeSe4.Röntgenstrukturuntersuchungen an Einkristallen ergaben daß die beiden Verbindungen isotyp kristallisieren. Die Atomanordnung entspricht der des Na6ZnO4 (Raumgruppe P63mc). Als charakteristische Baueinheit treten isolierte [FeX4]6--Tetraeder auf.Die Temperaturabhängigkeiten der magnetischen Suszeptibilitäten lassen sich mit einem Curie-Weiss-Verhalten beschreiben. Bei tiefen Temperaturen treten Abweichungen von diesem Verhalten auf, die offensichtlich auf antiferromagnetische Wechselwirkungen zurückzuführen sind.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926161003
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  • 66
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    Darstellung und Kristallstrukturen der Verbindungen CaPdAs, CaPdSb und CaPdBi (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 618 (1992), S. 30-34 
    Details
    ISSN: 0044-2313
    Keywords: Calcium palladium pnictides ; Preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structures of the Compounds CaPdAs, CaPdSb, and CaPdBiThe new compounds CaPdAs, CaPdSb, and CaPdBi were prepared by heating appropriate mixtures of the elements. X-ray structure determinations carried out with single crystals (space group and lattice constants see “Inhaltsübersicht”) showed, that the arsenide crystallizes in a distorted stacking variant of the AlB2, type structure, where the Pd atoms have a planar environment of As atoms. CaPdSb and CaPdBi are isotypic and form the TiNiSi type structure, where the Pd-Atoms are surrounded tetrahedrally (strongly distorted) by Sb or Bi atoms.
    Notes: CaPdAs (Pnma; a = 7,137(1) Å, b = 8,646(2) Å, c = 16,590(3) Å; Z = 16) kristallisiert in einer verzerrten Stapelvariante des AlB2-Typs, bei der die Pd-Atome planar von drei As-Atomen umgeben sind. CaPdSb (a = 7,354(2) Å, b = 4,617(1) Å, c = 7,903(2) Å) und CaPdBi (a = 7,422(2) Å, b = 4,753(1) Å, c = 8,085(2) Å) sind isotyp und bilden die TiNiSi-Struktur (Pnma; Z = 4) mit einer stark verzerrten Tetraederkoordination um die Pd-Atome. Die Verbindungen wurden durch Erhitzen der entsprechenden Elementgemenge dargestellt, die Strukturen röntgenographisch mit Einkristallmethoden bestimmt.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926180106
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    Synthese, Struktur und Thermolyse von NH4[Re3Br10] (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 618 (1992), S. 26-29 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium complexes ; synthesis ; crystal structure ; thermal behaviour ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Structure and Thermolysis of NH4[Re3Br10]NH4[Re3Br10] crystallizes as dark brown single crystals upon slow cooling of a hot, saturated hydrobromic-acid solution of [Re3Br9(H2O)2] after the addition of NH4Br. The crystal structure (monoclinic, C2/m (Nr. 12); Z = 4; a = 1461.6(7), b = 1 085.6(4), c = 1030.3(7) pm, β = 92.63(4)°, Vm = 245.9(4)cm3/mol; R = 0.097, Rw = 0.043) contains [Re3Br12]- units that share two common edges. These chains run along [010] and are held together by NH4+ ions. Each NH4+ is surrounded by eight Br- from four different chains. The first step of the thermal decomposition at 290°C is the disproportionation to ReBr3 (ReCl3 type), rhenium metal and (NH4)2[ReBr6]. Secondly, the internal reduction of (NH4)2[ReBr6] at 390°C to rhenium metal takes place.
    Notes: Aus heißer, gesättigter, bromwasserstoffsaurer Lösung von [Re3Br9(H2O)2] erhält man nach Zugabe von NH4Br beim langsamen Abkühlen dunkelbraune Einkristalle von NH4[Re3Br10]. In der Kristallstruktur (monoklin, C2/m (Nr. 12); Z = 4; a = 1 461,6(7); b = 1 085,6(4); c = 1030,3(7) pm, β = 92,63(4)°, Vm = 245,9(4) cm3/mol; R = 0,097, Rw = 0,043) erstrecken sich entlang [010] doppelt kantenverknüpfte [Re3Br12]--Baueinheiten. Diese Stränge werden durch NH4+-Ionen zusammengehalten, wobei jedes NH4+ von acht Br- aus vier unterschiedlichen Strängen umgeben ist. Der thermische Abbau erfolgt im wesentlichen in zwei Schritten: Bei 290°C entsteht durch Disproportionierung ReBr3 im ReCl3-Typ bzw. Rhenium-Metall neben (NH4)2[ReBr6], das bei 390°C durch “innere Reduktion” zu Rhenium-Metall abgebaut wird.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926180105
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    Mg3Ni20P6 und Mn3Ni20P6  -  Zwei neue Phosphide mit Cr23C6-Struktur (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 618 (1992), S. 35-38 
    Details
    ISSN: 0044-2313
    Keywords: Ternary nickelphosphides ; magnesium ; manganese ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Mg3Ni20P6 and Mn3Ni20P6 - Two new Phosphides with Cr23C6-type StructureThe crystal structures of Mg3Ni20P6 (a = 11.113(3)A) and Mg3Ni20P6 (a = 11.085(1)Å) were determined by single crystal X-ray investigations. Both compounds, prepared by heating appropriate mixtures of the elements, crystallize in a ternary variant of the Cr23C6-type structure (Fm3m), which is well-known due to a large number of ternary borides.
    Notes: Die Kristallstrukturen von Mg3Ni20P6 (a = 11,113(3) Å) und Mn3Ni20P6 (a = 11,085(1) Å) wurden röntgenographisch mit Einkristallmethoden bestimmt. Beide Verbindungen, dargestellt durch Erhitzen entsprechender Elementgemenge, bilden eine Besetzungsvariante der Cr23C6-Struktur (Fm3m), in der viele ternäre Boride kristallisieren.
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    URL: http://dx.doi.org/10.1002/zaac.19926180107
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    I—N = S = N—I - Darstellung und Struktur (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 618 (1992), S. 89-92 
    Details
    ISSN: 0044-2313
    Keywords: N,N′-Diiodosulfur diimide ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: I—N = S = N—I, Preparation and ReactivityI—N = S = N—I is prepared form IN[Si(CH3)3]2 by reaction with SF4. It is a shock sensitive yellow powder, that appears in brown crystals after recrystallisation from CH2Cl2. The crystal structure reveals a syn-anti conformation for the molecule. Due to I … N contacts a layer lattice is formed.
    Notes: I—N=S=N—I entsteht aus IN[Si(CH3)3]2 durch Reaktion mit SF4. Es ist ein schlagempfindliches, gelbes Pulver, welches aus CH2Cl2 umkristallisiert in braunen Kristallen anfällt. Die Kristallstruktur zeigt für das Molekül die syn-anti Konformation. Durch I … N Kontakte entsteht ein Schichtengitter.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926180116
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    Die Reaktion von Tellurhexafluorid mit Trimethylamin, Strukturen der TeF5-- und SeF5--Anionen (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 618 (1992), S. 83-88 
    Details
    ISSN: 0044-2313
    Keywords: Pentafluoro tellurate(IV) ; pentafluoroselenateIV ; (dimethylamino)-methyl-trimethylammonium cation ; crystal structure ; weak fluorine interactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of Telluriumhexafluoride and Trimethylamine, Structures of the TeF5- and SeF5- AnionsThe reaction of TeF6 and (CH3)3N is of the redox kind, resulting in reduction of tellurium: X-ray single crystal analysis reveals the compounds (CH3)2N—CH2—N(CH3)2+TeF5- and [(CH3)3NH+]5(TeF5-)3(HF2-)2. By comparison with published data it can be shown that this mixture is identical to previously published [(CH3)3N]2TeF6. The latter was supposed to be one of the few examples of tellurium in a coordination state of eight. (CH3)4N+TeF5- and (CH3)4N4SeF5- are obtained and their structure is investigated by single crystal x-ray methods also. The anions SF5-, SeF5- and TeF5- are discussed in terms of weak interactions.
    Notes: Die Reaktion von TeF6 mit (CH3)3N ist eine Redoxreaktion, Tellur(VI) wird von Trimethylamin zu Tellur(IV) reduziert: Mittels der Kristallstrukturanalyse werden die Produkte (CH3)2N—CH2-N(CH3)3+TeF5- und [(CH3)3NH+]5(TeF5-)3(HF2-)2 nachgewiesen. Durch Vergleich mit publizierten Daten kann die Existenz von [(CH3)3N]2TeF6 mit achtfach koordiniertem Tellur widerlegt werden. Am (CH3)4N+SeF5- wird erstmals das SeF5--Anion strukturanalytisch und im Vergleich mit SF5- und TeF5- im Hinblick auf schwächere Wechselwirkungen untersucht.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926180115
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    Die Kristallstruktur des Tetrakis(di-tert.-butylphosphino)diphosphans. [(tBu)2P]2P—P[P(tBu)2]2 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 607 (1992), S. 26-28 
    Details
    ISSN: 0044-2313
    Keywords: Tetrakis(di-tert.-butylphosphino)diphosphane ; [(tBu)2P]2P—P[P(tBu)2]2 ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Tetrakis(di-tert.-butylphosphino)diphosphane [(tBu)2P]2P—P[P(tBu)2]2[(tBu)2P]2P—P[P(tBu)2]2 1 obtained at -20°C from a solution of (tBu)2P—P=P(Br)tBu2 forms yellow crystals (regular hexagons). 1 crystallizes monoclinic in the space group C2/c with a = 2145.6pm, b = 1137pm, c = 1696.1pm, β = 110.075° and Z = 4 formula units in the elementary cell. Due to high steric load the bond angles at the tertiary P atoms with δ = 115.7° are significantly larger than those at the primary P atoms with δ = 108.6°.
    Notes: [(tBu)2P]2P—P[P(tBu)2]2 1 sich aus (tBu)2P—P(Br)tBu2 (toluolische Lösung, -20°C) und fällt als gelbe Kristalle (regelmäßige Sechsecke) aus. 1 kristallisiert monoklin in der Raumgruppe C2/c mit den Gitterkonstanten a = 2145,6pm, b = 1137pm, c = 1696pm, β = 110,75°. Die Elementarzelle enthält 4 Formeleinheiten. Die Bindungswinkel an den tertiären P-Atomen mit δ = 115,7° sind infolge der hohen sterischen Belastung der tert. P-Atome gegenüber denen an den primären P-Atomen mit δ = 108,6° deutlich aufgeweitet.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926070106
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    Floridcarbonate der Alkalimetalle (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 607 (1992), S. 13-18 
    Details
    ISSN: 0044-2313
    Keywords: Alkali metal fluoride carbonates ; preparation ; crystal structure ; IR, Raman spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Alkali Metal Fluoride CarbonatesAlkali metal fluoride carbonates A3(CO3)F and A2A′(CO3)F with A,A′ = K, Rb, Cs have been obtained by solid state reaction between the respective alkali metal fluorides and carbonates. They crystallize isotype to K3(CO3)F. The cell dimensions of K2Rb(CO3)F, KRb2(CO3)F, and CsRb2(CO3)F have been determined and refined by X-ray powder diffraction methods. Solid solutions are formed between K3(CO3)F and Rb3(CO3)F. The crystal structures of K2Rb(CO3)F and KRb2(CO3)F were refined based on single crystal diffraction data. A factor group analysis allowed for interpretation of IR and Raman spectra of K3(CO3)F.
    Notes: Fluoridcarbonate der Alkalimetalle A3(CO3)F bzw. A2A ′(CO3)F mit A,A′ = K, Rb, Cs wurden durch Festköperreaktionen aus entsprechenden Alkalimetallfluoriden und -carbonaten dargestellt. Sei kristallisieren isotyp mit K3(CO3)F. Die Gitterkonstanten von K2Rb(Co3)F, KRb2(CO3)F und CsRb2(CO3)F wurden mittels Röntgenpulvertechniken bestimmt und verfeinert.Lückenlose Mischkristallbildung wurde für das System K3(CO3)F/Rb3(CO3)F nachgewiesen. Die Kristallstrukturen von K2Rb(CO3)F und KRb2(CO3) wurden mit Einkristalldaten verfeinert. für K3(CO3)F und Rb3(CO3)F wurden die Raman- und IR-Spektren auf der Basis der Faktorgruppennäherung interpretiert.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926070104
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    Zur Koordinationschemie des 1,3-Dithiol-2-selon-4,5-diselenolats (dsise) und des 1,3-Dithiol-2-selon-4,5-dithiolats (dmise). Kristall- und Molekülstruktur des Tetrabutylammonium-bis-(1,3-dithiol-2-selon-4,5-diselenolato)nickelat(II) und -(III), [(n-C4H9)4N]2[Ni(dsise)2] und (n-C4H9)4N[Ni(dsise)2] (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 103-116 
    Details
    ISSN: 0044-2313
    Keywords: Metal(II), -(III) bis-chelates (Bu4N)n[M-(dsise)2] ; (dsise) — 1,3-dithiole-2-selone-4,5-diselenolate ; i. r., 13C n.m.r., e.p.r., cyclovoltammetric data ; ab-initio SCF calculations ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Coordination Chemistry of 1,3-Dithiole-2-selone-4,5-diselenolate (dsise) and 1,3-Dithiole-2-selone-4,5-dithiolate (dmise). Crystal and Molecular Structure of Tetrabutylammonium bis(1,3-dithiole-2-selone-4,5-diselenolato)nickelate(II) and -(III), [(n-C4H9)4N]2[Ni(dsise)2 and (n-C4H9)4[Ni(dsise)2]Syntheses and properties of metal(II) and metal(III) bis-chelates of 1,3-dithiole-2-selone-4,5-diselenolate (dsise), of the general type (Bu4N)n)M(dsise)2] (n =2 : M = Zn, Cd, Hg, Cu, Ni, Pd; n = 1: M = Ni, Au) are reported and compared with chelates of the isologue 1,3-dichalcogenole-2-chalcogenoe-4,5-dichalcogenolate (i. r., 13C-n. m. r., e. p. r., cyclovoltammetric data). The unexpected rearrangement during the syntheses of dsise and 1,3-dithiole-2-selone-4,5-diselenolate (dmise) is characterized by ab-initio SCF calculations. The x-ray structures of (Bu4N)2[Ni(dsise)2] (space group P21/c, a = 8.5556(13) Å, b = 15.0009(12) Å, c = 19.696(3) Å, β = 96.018(7)°, V = 2513.9(5) Å3, Z = 2) and Bu4N[Ni(dsise)2] (space group C2/c, a = 25.133(6) Å, b = 9.828(4) Å, c = 18.104(7) Å, β = 132.81(1)°, V = 3281(2) Å3, Z = 4) are given.
    Notes: Synthese und Eigenschaften von Metall(II) und Metall(III) Bis-Chelaten des 1,3-Dithiol-2-selon-4,5-diselenolats (dsise) vom Typ (Bu4N)n[M(dsise)2](n = 2: M = Zn, Cd, Hg, Cu, Ni, Pd; n = 1:M = Ni, Au) werden beschrieben und im Vergleich mit isologen 1,3-Dichalkogenol-2-chalkogenon-4,5-dichalkogenolat-Chelaten diskutiert (IR, 13C-NMR, EPR, Cyclovoltammetrie). Anhand von ab-initio-SCF-Rechnungen wird die bei der Synthese des dsise und des 1,3-Dithiol-2-selon-4,5-dithiolats (dmise) auftretende „Umlagerung“ charakterisiert. Die röntgenkristallographischen Daten von (Bu4N)2[Ni(dsise)2] (Raumgruppe P21/c, a = 8,5556(13) Å, b = 15,0009(12) Å, c = 19,696(3) Å, β = 96,018(7)°, V = 2513,9(5) Å3, (Z = 2) und von Bu4N[Ni(dsise)2] (Raumgruppe C2/c, a = 25,133(6) Å, b = 9,828(4) Å, c = 18,104(7) Å, β = 132,81(1)°, V = 3281(2) Å3, Z = 4) werden vorgestellt.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926090320
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    Ein Beitrag zur Kristallstruktur von CuYW2O8, CuHoW2O8 und CuYbW2O8 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 607 (1992), S. 52-56 
    Details
    ISSN: 0044-2313
    Keywords: Copper-lanthanoide-tungsten-oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Contribution on the Crystal Structure of CuYW2O8, CuHoW2O8, and CuYW2O8Single crystals of (I) CuY2O8, (II), CuHoW2O8, and (III) CuYbW2O8 were prepared and investigated by X-ray technique. (I) crystallizes with triclinic symmetry, space group C11—P1 (a = 5.939 Å, b = 6.042 Å, c = 5.025 Å; α = 112.30°, β = 111.77°; Z = 1). (II) and (III) belong to monoclinic symmetry, space group C2h4—P2/n (II) (a = 10.045 Å, b = 5.808 Å, c = 5.021 Å; β = 94.38°; z = 2 (III) a = 9.948 Å, b = 5.824 Å, c = 5.008 Å; β = 93.36°; Z = 2). The crystal structures will be discussed with respect to other to copper rare earth tungstates.
    Notes: (I) CuHoW2O8, (II) CuHoW2O8 und (III) CuYbW2O8 wurden einkristallin dargestellt und röntgenographisch untersucht. (I) kristallisiert triklin, Raumgruppe C11—P1 (a=5,939 AÅ, b= 6,042 AÅ, c= 5,025 AÅ; α=112,30°, β=92,84°, γ= 111, 77°; Z- 1). (II) und (III) Kristallisieren monoklin, Raumgruppe C2h4—P2/n (II) (a = 10,045 AÅ, b = 5,808 AÅ, c = 5,021 AÅ; β = 94,38°; Z = 2). Der Aufbau und die Einordnung in die bislang bekannten Kupferlanthanoid-Oxowolframate werden Diskutiert.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926070111
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  • 75
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    Darstellung und Kristallstruktur von Tetrakis(pentafluorphenylamino)silan (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 99-102 
    Details
    ISSN: 0044-2313
    Keywords: Aminosilane ; tetrakis(pentafluorophenylamino)silane ; 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 Tetrakis(pentafluorophenylamino)silaneColourless single-crystals of Tetrakis(pentafluorophenylamino) silane were obtained from the reaction of SiCl4 with monolithiated pentafluoroaniline at low temperatures. The aminosilane has been characterized by various spectroscopic methods and its crystal structure has been determined by x-ray diffraction (for details see “Inhaltsübersicht”). Thermal condensation has not been achieved. However, reaction of silicon(IV)-chloride with pentafluoroaniline in the presence of triethylamine yielded the respective tricyclosilazane.
    Notes: Tetrakis(pentafluorphenylamino)silan wurde erstmals (Umsetzung von Siliciumtetrachlorid mit monolithiiertem Pentafluoranilin) synthetisiert und durch verschiedene spektroskopische Techniken sowie Röntgenstrukturanalyse charakterisiert (I41/a; a = 19,6383(9), c = 6,5551(7) Å; 1842 Diffraktometerdaten; R = 0,054). Versuche zur thermischen Kondensation blieben ohne Erfolg, jedoch führte die Reaktion von Silicium (IV)-chlorid mit Pentafluoranilin in Gegenwart von Triethylamin als Hilfsbase zu dem entsprechenden Tricyclosilazan.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926100116
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    Neue Alkalioxoarsenate (V) Zur Kenntnis von Rb2Li[AsO4] und Cs2Li[AsO4] (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 103-111 
    Details
    ISSN: 0044-2313
    Keywords: Alkali metal orthoarsenate ; crystal structure ; MAPLE calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Alkalioxoarsenates (V). On Rb2Li[AsO4] and Cs2Li[AsO4]By heating of well-grounded mixtures of the binary oxides (A2O, Li2O2, and As2O3; A : Li : As = 2 : 1 : 1; Ni-tube, 550°C, 21 d; A = Rb, Cs) colourless single crystals of Rb2Li[AsO4] and Cs2Li[AsO4] were obtained for the first time. These new orthoarsenates(V) crystalize orthorhombic (space group C mc21—C2v12, No. 36) with Z = 4. As expected they are isotypic with the according orthovanadates(V) [2] A2Li[VO4], A = Rb, Cs. The lattice constants of Rb2Li[AsO4]: a = 582.1(4) pm, b = 1171.1(7) pm, c = 792.4(5) pm and Cs2Li[AsO4]: a = 596.4(2) pm, b = 1223.4(2) pm, c = 819.7(3) pm were taken from Guinier-Simon powder data. The structure was determined by four-circle-diffractometer data [Siemens AED II, MoKα, 6290 I0 (hkl), R = 3.5%, Rw = 3.2% to Rb2Li[AsO4]; 3518 I0 (hkl), R = 2.8%, Rw = 2.6% to Cs2Li[AsO4]; parameters see text]. The Madelung Part of Lattice Energy, MAPLE, and Effective Coordination Numbers, ECoN, these calculated via Mean Fictive Ionic Radii, MEFIR, as well as charge distribution CHARDI are calculated and discussed.
    Notes: Durch Tempern inniger Gemenge der binären Oxide (A2O, Li2O2 und As2O3; A : Li : As = 2 : 1 : 1; Ni-Bombe, 550°C, 21 d; A = Rb, Cs) wurden Rb2Li[AsO4] und Cs2Li[AsO4] erstmals in Form von farblosen Einkristallen erhalten. Die neuen Orthoarsenate(V) kristallisieren orthorhombisch (Raumgruppe C mc21—C2v12, Nr.36) mit Z = 4 und sind erwartungsgemäß isotyp zu den entsprechenden Orthovanadaten(V) [2] A2Li[VO4] mit A = Rb, Cs. Die Gitterkonstanten für Rb2Li[AsO4]: a = 582,1(4) pm, b = 1171,1(7) pm, c = 792,4(5) pm und Cs2Li[AsO4]: a = 596,4(2) pm, b = 1223,4(2) pm, c = 819,7(3) pm wurden aus Guinier-Simon-Pulverdaten ermittelt. Die Struktur wurde mittels Vierkreisdiffraktometerdaten [Siemens AED II, MoKα, 6290 I0 (hkl), R = 3,5%, Rw = 3,2% für Rb2Li[AsO4]; 3518 I0 (hkl), R = 2,8%, Rw = 2,6% für Cs2Li[AsO4]; Parameter siehe Text] bestimmt. Der Madelunganteil der Gitterenergie, MAPLE, und Effektive Koordinationszahlen, ECoN, diese über Mittlere Fiktive Ionenradien, MEFIR, sowie die Ladungsverteilung CHARDI werden berechnet und diskutiert.
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    URL: http://dx.doi.org/10.1002/zaac.19926100117
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    Die Kristallstruktur von [MoO2F2(2,2′-Bipyridyl)] (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 117-120 
    Details
    ISSN: 0044-2313
    Keywords: 2,2′-Bipyridyl molybdenum difluoridedioxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of [MoO2F2(2,2′-bipyridyl)]The title compound crystallizes in the space group P21/n with a = 869.6(1), b = 1390.1(3), c = 959.0(1) pm, β = 110.967(5)°, Z = 4; structure determination with 1718 observed independent reflections, R = 0.031. The compound consists of molecules having two cis oxo ligands and a bipyridyl chelate in the MoO2 plane.
    Notes: Die Titelverbindung kristallisiert in der Raumgruppe P21/n mit a = 869,6(1); b = 1390,1(3); c = 959,0(1) pm; β = 110,967(5)°, Z = 4; Strukturbestimmung mit 1718 beobachteten unabhängigen Reflexen, R = 3,1%. Die Verbindung besitzt eine Molekülstruktur mit cis-ständigen Oxoliganden und dem Bipyridylchelat in der MoO2-Ebene.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926100119
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    Darstellung, Kristallstruktur und IR-spektroskopische Untersuchung von Phosphor(V)-nitrid-imid, HPN2 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 121-126 
    Details
    ISSN: 0044-2313
    Keywords: Phosphorus nitride imide ; preparation ; crystal structure ; i. r. data ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation, Crystal Structure, and IR-spectroscopic Investigation of Phosphorus Nitride Imide, HPN2Pure and fine crystalline phosphorus nitride imide (HPN2) is obtained by heterogeneous ammonolysis of P3N5 with gaseous NH3 (T = 580°C, p = 30 bar, 6 d). X-ray powder diffraction data has been used to refine the crystal structure of HPN2 by the Rietveld full-profile technique (I42d; a = 461.82(2) pm, c = 702.04(3) pm; Z = 4; 41 reflections observed, 17° 〈 2Θ 〈 125°, CuKα1, germanium monochromator; R(wp) = 0.072, R(I,hkl) = 0.048). In the solid HPN2 contains a three-dimensional framework of corner-sharing PN4-tetrahedra (P—N: 159.9(4) pm; P—N—P: 130.1(4)°. The hydrogen atoms are covalently bonded to half of the nitrogen atoms. The IR spectrum exhibits six vibrational modes v(N—H): 3224; vas(PNP): 1330, 1223; vas(PNHP): 971, 901: δ(PNP): 531 cm-1).
    Notes: Reines und feinkristallines Phosphor(V)-nitrid-imid (HPN2) wurde durch heterogene Ammonolyse von P3N5 mit gasförmigem NH3 (T = 580°C, p = 30 bar, 6d) dargestellt. Die Kristallstruktur von HPN2 wurde auf der Basis von Röntgen-Pulverdiffraktometerdaten mit Hilfe der Rietveld-Methode verfeinert (I42d, a = 461,82(2) pm, c = 702,04(3) pm; Z = 4; 41 beobachtete Reflexe, 17° 〈 2Θ 〈 125°; Cu—Kα1, Germanium-Monochromator; R(wp) = 0,072; R(I,hkl) = 0,048). Im Festkörper ist HPN2 aus einem dreidimensionalen Netz allseitig eckenverknüpfter PN4-Tetraeder (P—N: 159,9(4) pm; P—N—P: 130,1(4)°) aufgebaut. Die H-Atome sind kovalent an die Hälfte der N-Atome gebunden. Im IR-Spektrum werden sechs Schwingungsbanden (v(N—H): 3224; vas(PNP): 1330, 1223; vas(PNHP): 971, 901; δ(PNP): 531 cm-1) beobachtet.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926100120
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    [Na(15-Krone-5)][ReFCl3(NO)(CH3CN)] Synthese, IR-Spektrum und Kristallstruktur (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 112-116 
    Details
    ISSN: 0044-2313
    Keywords: Nitrosyl-fluoride complex of rhenium ; synthesis ; IR spectrum ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Na(15-crown-5)][ReFCl3(NO)(CH3CN)] Synthesis, IR Spectrum, and Crystal StructureThe title compound has been prepared by the reaction of [ReCl3(NO)2(CH3CN)] with the equivalent amount of sodium fluoride in the presence of 15-crown-5 in boiling acetonitrile, forming blue crystals. They were characterized by IR spectroscopy and by an X-ray structure determination. Space group P21/n, Z = 4,2117 observed independent reflections, R = 0.037, wR = 0.029. Lattice dimensions at 20°C: a = 834.0(2), b = 1600.0(3), c = 1670.0(3) pm; β = 104.19(3)°. The compound forms an ion pair via one Na—F contact of 234.4 pm and one Na—Cl contact of 293.4 pm; the nitrosyl ligand ist in trans-position to the F atom of the anion [ReFCl3(NO)(CH3CN)]-.
    Notes: Die Titelverbindung wird aus [ReCl3(NO)2(CH3CN)] mit der äquivalenten Menge Natriumfluorid bei Gegenwart von 15-Krone-5 in siedendem Acetonitril in Form blauer Kristalle hergestellt und durch das IR-Spektrum und eine Kristallstrukturanalyse charakterisiert. Raumgruppe P21/n, Z = 4, 2117 beobachtete unabhängige Reflexe, R = 3,7%, wR = 2,9%. Gitterabmessungen bei 20°C: a = 834,0(2); b = 1600,0(3); c = 1670,0(3) pm; β = 104,19(3)°. Die Verbindung bildet ein Ionenpaar mit einem Na—F-Kontakt von 234,4 pm und einem Na—Cl-Kontakt mit 293,4 pm; der Nitrosylligand befindet sich in trans-Stellung zum Fluorliganden des [ReFCl3(NO)(CH3CN)]--Ions.
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    URL: http://dx.doi.org/10.1002/zaac.19926100118
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    Synthese und Kristallstruktur von [Ba(18-Krone-6)(DMF)4][Cd(Se4)2] (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 608 (1992), S. 17-22 
    Details
    ISSN: 0044-2313
    Keywords: Barium-crownether complex ; octaselenido cadmate ; 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 [Ba(18-Crown-6)(DMF)4][Cd(Se4)2]The title compound has been prepared by the reaction of a DMF-solution of lithium polyselenide with BaSe2 and cadmium acetate in the presence of 18-crown-6, forming black crystals. The compound was characterized by IR spectroscopy and by an X-ray structure determination. Space group P2/a, Z = 4, 5392 observed unique reflections, R = 0.048. Lattice dimensions at -90°C: a = 2021.9(12); b = 1019.8(6); c= 2270.8(14)pm, ß = 106.98(4)°. The structure consists of [Ba(18-crown-6)(DMF)4]2+ ions, in which the barium ions are coordinated by the six oxygen atoms of the crown ether molecule and by four oxygen atoms of the DMF molecules, and of [Cd(Se4)2]2- ions. The cadmium atoms are coordinated by two tetraselenide ions in a chelating fashion.
    Notes: Die Titelverbindung entsteht in Form schwarzer Kristalle bei der Einwirkung einer Lithiumpolyselenidlösung auf Bariumdiselenid und Cadmiumacetat in Dimethylformamid in Gegenwart von 18-Krone-6. Die Verbindung wurde durch das IR-Spektrum und eine röntgenographische Strukturanalyse charakterisiert. Raumgruppe P2/a, Z = 4, 5392 beobachtete unabhängige Reflexe, R = 4,8%. Gitterabmessungen bei -90°C: a = 2021,9(12); b = 1019,8(6); c = 2270,8(14) pm, ß = 106,98(4)°. Die Struktur ist aufgebaut aus [Ba(18-Krone-6)(DMF)4]2+-Ionen, in denen die Bariumionen von den sechs Sauerstoffatomen des Kronenethers und von vier O-Atomen der DMF-Moleküle koordiniert sind, und [Cd(Se4)2]2- -Anionen. In diesen sind die Cadmiumatome von zwei Tetraselenidionen chelatartig umgeben.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926080203
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    (PPh4)[(ReO2S2)CuI] und (NEt4)2[(ReOS3)Cu3Cl4]: Fixierung der bisher nicht isolierten Ionen [ReO2S2]- und [ReOS3]- durch Ausnutzung der Stabilität der CuS2(Re)- und Cu3S3(Re)-Fragmente (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 614 (1992), S. 115-120 
    Details
    ISSN: 0044-2313
    Keywords: Oxothioperrhenate ions, ReO2S2-, ReOS3- ; preparation ; crystal structure ; IR, UV/Vis spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: (PPh4)[(ReO2S2)CuI] and (NEt4)2[ReOS3)Cu3Cl4]: Fixation of the up to now not Isolated Ions [ReO2S2]- and [ReOS3]- Utilizing the Stability of the CuS2(Re) and Cu3S3(Re) Fragments(PPh4)[(ReO2S2)CuI] (1) and (NEt4)2[ReOS3)Cu3Cl4] (2) containing the up to now not isolated oxothioperrhenate ions [ReO2S2]- and [ReOS3]- as ligands, have been prepared by the reaction of (NEt4)[ReS4] with PPh3 and CuI in acetone in the presence of (PPh4)I ((1)) or with CuCl in CH2Cl2 in the presence of (NEt4)Cl ((2)), respectively. 1 and 2 have been characterized by X-ray structure analysis, elemental analysis and spectroscopic studies (IR, UV/Vis). The electronic spectra show bands which can approximately be assigned to interesting low-energy charge-transfer-transitions of the type d(Cu) → d(Re).For crystal data see Inhaltsübersicht.
    Notes: (PPh4)[(ReO2S2)CuI] (1) und (NEt4)2[(ReOS3)Cu3Cl4] (2), die die bisher nicht isolierten Oxothioperrhenat-Ionen [ReO2S2]- und [ReOS3]- als Liganden enthalten, wurden durch Reaktion von (NEt4)[ReS4] mit PPh3 und CuI in Aceton in Gegenwart von (PPh4)I ((1) bzw. entsprechend mit CuCl in CH2Cl2 in Gegenwart von (NEt4)Cl ((2) erhalten. 1 und 2 wurden durch Einkristall-Röntgenstrukturanalyse, Elementaranalyse, sowie spektroskopische Untersuchungen (IR, UV/Vis) charakterisiert. In den Elektronenspektren findet man Banden, die interessanten niederenergetischen Charge-Transfer-Übergängen des Typs d(Cu) → d(Re) näherungsweise zugeordnet werden können.Kristalldaten: 1P21/n, a = 1162,2(4), b = 1395,7(6), c = 1612,3(9)pm, β = 96,53(4)° V = 2598(2) · 106pm3, R = 0,049 für 4623 unabhängige Reflexe (F0≥4,0σ(F0)).2C2/c, a = 2059,0(5), b = 1352,9(3), c = 2217,1(5)pm, β = 90,26(22)° V = 6176(2) · 106pm3, R = 0,080 für 3162 unabhängige Reflexe (F0≥4,0σ(F0)).
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926140820
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  • 82
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    Ein neuartiges Iod(III, V) Gemischtvalentes Iodoxopolykation in (IO2)3 HSO4 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 608 (1992), S. 159-165 
    Details
    ISSN: 0044-2313
    Keywords: Iodine ; mixed valent iodine(III, V) polyoxocation ; preparation ; crystal structure ; Raman, i.r. spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Novel Iodine(III, V) Mixed Valent Iodinepolyoxocation in (IO2)3HSO4Previously unknown (IO2)3HSO4 is formed by action of firstly conc. H3PO4 upon HIO3 or H5IO6 at 310-330° C, and subsequently of conc. H2SO4 at room temperature. Its crystal structure (Pna21; a = 8.907(3), b = 20.464(6), c = 9.784(4) Å; Z = 8; 4354 diffractometer data; R = 0.087, Rw = 0.056) contain the novel polymeric cation (IO203nn+. Iodine(III) is coordinated square-planar by oxygen, iodine(V trigonal- pyramidal. The HSO4- anions are interconnected via hydrogen bonds. Raman and IR spectra are reported.
    Notes: Vorher unbekanntes (IO2)3 HSO4 bildet sich bei Einwirkung von Konz. H3POx4 bei 310-330°C auf Iodsäure(V) oder Hexaoxoiodsäure(VII) und danach von Konz. H2SO4 bei Raumtemperatur. Die Kristallstruktur (Pna21) a = 8,907(3), b = 20,464(6), c = 9,784(4)A; Z = 8; 4354 Diffraktometerdaten; R = 0,087, Rw = 0,056) enthält ein neuartiges Iodpolyoxokation (IO2)3nn+) mit quadratisch-planar von Sauerstoff koordiniertem Iod(III)) neben trigonal-pyramidal koordiniertem Iod(V. Die Hydrogensulfatgruppen sind über Wasserstoffbrückenbindungen untereinander verknüpft. Raman- und IR-Spektren werden mitgeteilt und interpretiert.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926080224
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  • 83
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    3s-Gd2C2Br2: Eine neue Stapelvariante (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 7-11 
    Details
    ISSN: 0044-2313
    Keywords: Gadolinium carbide chloride ; terbium carbide chloride ; condensed clusters ; crystal structure ; electrical resistivity ; magnetic susceptibility ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 3s-Gd2C2Br2: An Isomorph with a New Stacking SequenceGd2C2Br2 has been described in [1]. Here we describe the new stacking variant 3s-Gd2C2Br2 prepared by reaction of stoichiometric amounts of GdBr3, Gd, and C at 1 320 K. 3s-Gd2C2Br2 with a stacking sequence different to that described in [1] crystallizes in space group C2/m with lattice constants a = 706.6(2) pm, b = 382.7(1) pm, c = 996.7(4) pm and β = 99.95(3)°. In the structure C2 units are octahedrally surrounded by Gd atoms. Such Gd6(C2) octahedra are condensed via edges to form sheets, which are separated by two layers of Br-ions. In contrast to the modification described previously three slabs BrGd(C2)GdBr are stacked in [103] direction until identity is reached. The isotypic 3s-Tb2C2Br2 has also been prepared at 1 370 K. It is characterized by the lattice constants a = 701.5(3) pm, b = 380.1(1) pm, c = 994.8(3) pm and β = 100.05°.
    Notes: Die Verbindung Gd2C2Br2 wurde erstmals in [1] beschrieben. Die hier vorgestellte Stapelvariante 3s-Gd2C2Br2 erhält man durch Reaktion von stöchiometrischen Mengen GdBr3, Gd und C bei 1 320 K in verschweißten Ta-Ampullen. Sie kristallisiert in der Raumgruppe C2/m mit a = 706,6(2), b = 382,7(1), c = 996,7(4) pm und β = 99,95(3)°. In der Struktur sind C2-Gruppen von Gd-Atomen oktaedrisch umgeben. Diese Gd6(C2)-Oktaeder sind zweidimensional zu Schichten kondensiert, die durch Br-Doppelschichten voneinander sind getrennt. Im Gegensatz zu der in [1] dargestellten Strukturvariante sind hier 3 solcher Schichtpakete BrGd(C2)GdBr bis zur Identität in der Stapelrichtung [103] gestapelt. Die isotype Verbindung 3s-Tb2C2Br2 wird bei Temperaturen von 1 370 K dargestellt. Die Gitterkonstanten sind a = 701,5(3), b= 380,1(1), c = 994,8(1) pm und β = 100,05(3)°.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926090302
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  • 84
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    Synthese und Molekülstruktur von meso-(1,2,3-Tricyclohexyltriphosphan-1,3-diyl)zirkonocen(IV), Cp2 (Cp = η5-C5H5, Cy = C6H11) (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 35-38 
    Details
    ISSN: 0044-2313
    Keywords: Zirconocene-phosphido complexes ; (tricyclohexyltriphosphane-1,3-diyl)zirconocene(IV) ; 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 meso-(1,2,3-Tricyclohexyltriphosphane-1,3-diyl)zirconocene(IV), Cp2(Cp = η5-C5H5, Cy = C6H11)Cp2ZrCl2 reacts with Li(THF)2PHCy (Cy = C6H11) to yield the metallacyclic compound Cp2 1., The 31P{1H} NMR spectrum of 1, shows a coupling pattern for an A2X system, indicating the presence of only the meso-forms in solution, which are also present in the solid state. 1, crystallizes in the monoclinic space group P21/n (No. 14) with a = 12.984(8), b = 9.241(7), c = 23.05(1) Å, β = 93.48(4)°, V = 2760.1 Å3 and four formula units in the unit cell (2718 independent observed reflections, R = 7.3%). The central ZrP3 ring in 1, is almost planar. The Zr—P bond lengths of 2.618(4) and 2.628(4) Å are nearly identical.
    Notes: Cp2ZrCl2 setzt sich mit Li(THF)2PHCy (Cy = C6H11) zu der metallacyclischen Verbindung Cp2 1, um. Im 31P{1H}-NMR-Spektrum von 1, tritt das für ein A2X-System zu erwartende Aufspaltungsmuster auf, was auf das Vorliegen der meso-Formen in Lösung hinweist. Auch im Festkörper liegen nur die meso-Formen vor. 1, kristallisiert monoklin in der Raumgruppe P21/n (Nr. 14) mit a = 12,984(8), b = 9,241(7), c = 23,05(1) Å, β = 93,48(4)°, V = 2760,1 Å3 und vier Formeleinheiten pro Elementarzelle (2718 unabhängige beobachtete Reflexe, R = 7,3%). Der zentrale ZrP3-Ring in 1, ist angenähert planar. Die Zr—P-Bindungslängen sind mit 2,618(4) und 2,628(4) Å fast gleich.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926150907
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  • 85
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    Komplexierung von Gold mit N,N-Dialkyl-N′-benzoylthioharnstoffen: Die Kristallstruktur von N,N-Diethyl-N′-benzoylthioureatogold(I)-chlorid (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 611 (1992), S. 99-102 
    Details
    ISSN: 0044-2313
    Keywords: N,N-Diethyl-N′-benzoylthioureatogold(I) chloride ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Complex Formation of Gold with N,N-Dialkyl-N′-benzoylthioureas: The Crystal Structure of N,N-0Diethyl-N′-benzoylthioureatogold(I) ChlorideN,N-Diethyl-N′-benzoylthioureatogold(I) chloride AuCiS12H16N2O crystallizes in the monoclinic space group P21/c. The cell parameters are a = 18.407(4), b = 5.456(1) and c = 196.322(3) Å, β = 113.6/8(1)°. The structure was solved with direct techniques and refined to final R-value of 5.92%. Gold(I) forms a monodentately sulfur-coordinated complex with the ligand N,N-Diethyl-N′-benzoylthiourea. The coordination sphere around Au(I) shows a nearly linear arrangement of sulfur and chloride.
    Notes: N,N-Diethyl-N′-benzoylthioureatogold(I)-chlorid AuCISC12H16N2O kristallisiert in der monoklinen Raumgruppe P21/c mit den Gitterkonstanten a = 18,407(4), b = 5,456(1) und c = 16,322(3) Å, β = 113,68(1)0. Die Struktur wurde mit direkten Methoden gelöst und bis zu einem R-Wert von 5,92% verfeinert. Gold(I) bildet mit dem Liganden N,N-Diethyl-N′-benzoylthioharnstoff einen monodental über Schwefel koordinierten Komplex. Die Ligandatome Schwefel und Chlor sind nahezu linear an das Zentralatom gebunden.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926110517
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  • 86
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    Synthese, Kristallstrukturen und 121Sb-Mößbauer-Spektren von [SbBr3(15-Krone-5)], [SbBr2Me(15-Krone-5)] und [SbBr2Ph(15-Krone-5)] (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 611 (1992), S. 149-157 
    Details
    ISSN: 0044-2313
    Keywords: Antimony crown ether complexes ; preparation ; crystal structure ; IR, 121Sb-Mössbauer spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Crystal Structure, and 121Sb-Mössbauer Spectra of [SbBr3(15-Crown-5)], [SbBr2Me(15-Crown-5)], and [SbBr2Ph(15-Crown-5)]The compounds [SbBr3(15-crown-5)] (1), [SbBr2Me(15-crown-5)] (2), [SbBr2Ph(15-crown-5)] (3), and [SbCl2Me(15-crown-5)] (4) are formed by the reaction of 15-crown-5 with SbBr3, SbBr2Me, SbBr2Ph, and SbCl2Me, respectively, in toluene solution at -40°C. The complexes were characterized by IR spectroscopy, 121Sb-Mössbauer spectroscopy, 1-3 as well as by X-ray structure determinations. 1: Space group P212121, Z = 4, 1735 observed, independent reflections, R = 0.050, Lattice dimensions at -65°C: a = 787.03(7); b = 1313.0(2); c = 1619.3(2) pm.2: Space group Pca21, Z = 8, 2730 observed, independent reflections, R = 0.050, Lattice dimensions at -65°C: a = 1308.2(2); b = 1611.8(2); c = 1640.5(3) pm.3: Space group P21/n, Z = 4,2458 observed, independent reflections, R = 0.040, Lattice dimensions at -60°C: a = 900.3(3); b = 1390.6(6); c = 1618.5(7) pm, β = 96.32(3)°.The complexes 1-3 have molecular structures, in which the antimony atoms are surrounded by the five oxygen atoms of the crown ether molecule and by three ligands Br3, Br2CH3, Br2Ph, respectively.
    Notes: Die Molekülkomplexe [SbBr3(15-Krone-5)] (1), [SbBr2Me(15-Krone-5)] (2), [SbBr2Ph(15-Krone-5)] (3) und [SbCl2Me(15-Krone-5)] (4) entstehen in Toluol bei -40°C aus den Komponenten 15-Krone-5 und SbBr3, SbBr2Me, SbBr2Ph, bzw. SbCl2Me. Die Komplexe werden durch IR-Spektren, durch 121Sb-Mößbauer-Spektren und 1-3 durch Kristallstrukturanalysen charakterisiert. 1: Raumgruppe P21212121, Z = 4, 1 735 beobachtete unabhängige Reflexe, R = 5,0%, Gitterabmessungen bei -65°C: a = 787,03(7); b = 1313,0(2); c = 1619,3(2)pm.2: Raumgruppe Pca21, Z = 8,2730 beobachtete, unabhängige Reflexe, R = 5,0%, Gitterabmessungen bei -65°C: a= 1308,2(2); b = 1611,8(2); c = 1640,5(3) pm.3: Raumgruppe P21/n, Z = 4, 2 458 beobachtete, unabhängige Reflexe, R = 4,0%, Gitterabmessungen bei -60°C: A = 900,3(3); b= 1 390,6(6); c =1 618,5(7) pm, β = 96,32(3)°.Die Komplexe 1, 2 und 3 haben Molekülstrukturen, in denen die Antimonatome von den fünf O-Atomen des Kronenethers 15-Krone-5 und jeweils drei Ligandatomen Br3, Br2CH3 bzw. Br2Ph koordiniert sind. Das freie Elektronenpaar an den Antimon(III)-Atomen weist vermutlich in Richtung auf den durch die Kronenethermoleküle gebildeten Hohlraum.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926110525
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  • 87
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    Element - Element-Bindungen. VII. Intermolekulare Wechselwirkungen bei Dihalogen(phenyl)stibanen (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 617 (1992), S. 59-71 
    Details
    ISSN: 0044-2313
    Keywords: Dichloro(phenyl)stibane ; dibromo(phenyl)stibane ; diiodo(phenyl)stibane ; crystal structure ; intermolecular interactions ; structural relations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Element - Element Bonds. VII. Intermolecular Interactions in Dihalogen(phenyl)stibanesIn keeping with the literature dichloro(phenyl)stibane (1) may be obtained in a quantitative yield via a metathesis reaction between antimony(III) chloride and triphenylstibane; the dibromo (2) and diiodo (3) derivatives are synthesized by halogen exchange with phosphorus(III) bromide or sodium iodide, respectively. X-ray structure determinations at -120±3°C (R = 0,044/0,041/0,024) show the series of compounds to crystallize isotypically in the triclinic space group P1. The molecules are associated two-dimensionally by a moderately excentric η3-Sb··arene interaction and two Sb··halogen contacts each. Provided that the phenyl ligand is being substituted by its centre, the coordination geometry of the antimony atom may be described as a distorted octahedron. The crystal structure represents a variant (hettotype) of the bismuth(III) iodide type.
    Notes: Dichlor(phenyl)stiban (1) kann in Übereinstimmung mit Literaturangaben aus der Metathesereaktion zwischen Antimon(III)-chlorid und Triphenylstiban in quantitativer Ausbeute erhalten werden; durch Halogen-Austausch mit Phosphor(III)-bromid bzw. Natriumiodid wird es in das Dibrom- (2) oder Diiod-Derivat 3 überführt. Nach den Ergebnissen von Röntgenstrukturanalysen bei - 120 ± 3°C (R = 0,444/0,041/0,024) kristallisieren die drei Verbindungen isotyp in der triklinen Raumgruppe P1; die Moleküle sind zweidimensionalüber je eine mäßig exzentrische η3-Sb··Aren-Wechselwirkung und je zwei Sb··Halogen-Kontakte vernetzt. Denkt man sich den Phenyl-Liganden durch seinen Schwerpunkt ersetzt, so ist das Antimonatom verzerrt oktaedrisch koordiniert. Die Kristallstruktur läßt sich als Variante (Hettotyp) des Bismut(III)-iodid-Typs beschreiben.
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    URL: http://dx.doi.org/10.1002/zaac.19926170110
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  • 88
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    Synthese und Kristallstruktur von Ba4,5Ca1,5La2Fe4O15, Ba5CaEu2Fe4O15 und Ba5CaNd2Co4O15 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 617 (1992), S. 84-88 
    Details
    ISSN: 0044-2313
    Keywords: Alkaline earth lanthanoide iron (cobalt) 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 Ba4.5Ca1.5La2Fe4O15, Ba5CaEu2Fe4O15 and Ba5CaNd2Co4O15The compounds (I) Ba4.5Ca1.5La2Fe4O15, (II) Ba5CaEu2Fe4O15 and (III) Ba5CaNd2Co4O15 were prepared and investigated by single crystal X-Ray technique. They belong to the Ba6Nd2Al4O15 typ, space group C6v4—P63mc, (I): a = 11.677, c = 6.959 Å; (II): a = 11.570, c = 6.892 Å; (III): a = 11.604, c = 6.839 Å, Z = 2. The crystal chemistry of these substances will be discussed.
    Notes: Die Verbindungen (I) Ba4,5Ca1,5La2Fe4O15, (II) Ba5CaEu2Fe4O15 und (III) Ba5CaNd2Co4O15 wurden einkristallin dargestellt und röntgenographisch untersucht. Sie kristallisieren im Ba6Nd2Al4O15-Typ, Raumgruppe C6v4—P63mc mit (I): a = 11,677, c = 6,959 Å; (II): a = 11,570, c = 6,892 Å; (III): a = 11,604, c = 6,839 Å, Z = 2. Die Kristallchemie dieser Stoffe wird diskutiert.
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    URL: http://dx.doi.org/10.1002/zaac.19926170113
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  • 89
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    3-Diethylamino-5-phenyl-1,2,4-diselenazolium-tetrachloroniccolat(II)  -  Synthese und Struktur (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 617 (1992), S. 89-92 
    Details
    ISSN: 0044-2313
    Keywords: 3-Diethylamino-5-phenyl-1,2,4-diselenazolium-tetrachloroniccolate(II) ; 1,2,4-diselenazolium salt ; selenaheterocyclic cation ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 3-Diethylamino-5-phenyl-1,2,4-diselenazolium-tetrachloroniccolate(II)  -  Synthesis and StructureBis-(N′, N′-diethyl-N-benzoylselenoureato)nickel(II) reacts with diphosgene in benzene to 3-diethylamino-5-phenyl-1,2,4-diselenazolium-tetrachloroniccolate(II). Its structure is confirmed by RKSA and ESCA. The compound consists of cations, which are planar fivemembered rings and of tetrahedral tetrachloroniccolate(II) anions. The complex is isomorphic with 3-diethylamino-5-phenyl-1,2,4-dithiazolium-tetrachloroniccolate(II).
    Notes: Bis-(N′, N′-diethyl-N-benzoylselenoureato)nickel(II) reagiert mit Diphosgen in Benzen zu 3-Diethylamino-5-phenyl-1,2,4-diselenazolium-tetrachloroniccolat(II), dessen Röntgenkristallstrukturanalyse und Röntgenphotoelektronenspektrum vorgestellt und interpretiert werden. Die Verbindung besteht aus 1,2,4-Diselenazolium-Kationen, die als planare Fünfringe vorliegen und aus tetraedrischen Tetrachloroniccolat(II)-Anionen. Sie ist zu 3-Diethylamino-5-phenyl-1,2,4-dithiazolium-tetrachloroniccolat(II) isomorph.
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    URL: http://dx.doi.org/10.1002/zaac.19926170114
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  • 90
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    Kristallstrukturbestimmung von N-Trimethylsily-N′-methylimidazoliumbromid (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 617 (1992), S. 93-95 
    Details
    ISSN: 0044-2313
    Keywords: Silicon ; addition compounds ; N-trimethylsilyl-N′-methylimidazolium ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure Determination of N-Trimethylsilyl-N′-Methylimidazolium BromideThe reaction of Trimethylbromosilane and N-Methylimidazole (NMI) led to a 1:1 compound stable at room temperature. The reaction was carried out at room temperature and colorless single crystals were obtained by sublimation. The addition compound crystallizes in the orthorhombic space group Pbnb (No. 56) with lattice constants a = 1218.3(2)pm, b = 1333.6(1)pm, c = 1360.2(2)pm, Z = 8, Dcalc = 1.414 g/cm3. For 1506 independent reflections, measured at 21°C the structure could be refined to R = 0.067 and Rw = 0.062.
    Notes: Die Reaktion von Trimethylbromsilan und N-Methylimidazol (NMI) führt zu einer bei Raumtemperatur stabilen 1:1 Verbindung. Die Umsetzung wurde bei Raumtemperatur durchgeführt und durch Sublimation ließen sich farblose Einkristalle der Verbindung erhalten. Die Additionsverbindung kristallisiert in der orthorhombischen Raumgruppe Pbnb (Nr. 56) mit den Gitterkonstanten a = 1218,3(2) pm, b = 1333,6(1) pm, c = 1360,2(2) pm, Z = 8 und Dcalc = 1,414 g/cm3. Unter Verwendung von 1506 symmetrieunabhängigen Reflexen konnte die Struktur, gemessen bei 21°C, bis auf R = 0,067 und Rw = 0,062 verfeinert werden.
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    URL: http://dx.doi.org/10.1002/zaac.19926170115
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    Crystal structure and magnetic properties of tetra(monomethylammonium)hexachloroytterbatochloride(CH3NH3)4YbCl7 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 617 (1992), S. 105-109 
    Details
    ISSN: 0044-2313
    Keywords: Tetra(monomethylammonium)hexachloroytterbatochloride ; preparation ; crystal structure ; Raman spectra ; magnetic susceptibility data ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kristallstruktur und magnetische Eigenschaften von Tetra(monomethylammonium)-hexachloro-ytterbiumchlorid(CH3NH3)4YbCl7Die verbindung (CH3NH3)4 YbCl7 wurde aus einer Lösung von CH3NH3Cl und YbCl3 in einem Ethanol/Acetonitril-Gemisch synthetisiert. Die Struktur wurde mit Hilfe der Patterson-Methode anhand von 1465 Einkristalldaten gelöst und auf einen R-Wert von Rw = 0,035 verfeinert, Raumgruppe P2, a = 9,972(6) Å, b = 7,605(5) Å, c = 12,866(6) Å, β = 90,53(4)°. Die Struktur besteht aus [YbCl6]3- -Oktaedern und tetraedrisch angeordneten [(CH3NH3)4Cl]3+-Einheiten. In Übereinstimmung mit den Ergebnissen aus der Strukturanalyse zeigen die Ramanspektren eine Aufspaltung der von einer Bewegung der CH3NH3+ -Gruppen herrührenden Frequenzen. Die magnetische Suszeptibilität zeigt unterhalb von 170 K eine bemerkenswerte Abweichung vom Curie-Weiss-Gesetz, die mit Kristallfeld-Effekten des Yb3+ erklärt werden kann.
    Notes: (CH3NH3)4YbCl7 has been synthesized from a solution of CH3NH3Cl and YbCl3 in a mixture of ethnole/acetonitrile. The structure was solved from 1464 single crystal data by Patterson methods and refined to a final Rw = 0.035 space group P2, a = 9.972(6) Å, b = 7.605(5) Å, c = 12.866(6) Å, β = 90.53(4)°. The structure consists of alternating [YbCl6]3- octahedra and of tetrahedrally arranged [(CH3NH3)4Cl]3+ units. Raman spectra display a splitting of frequencies related to the CH3NH3+ group in agreement with the structure determination. The magnetic susceptibility shows a remarkable deviation from a Curie-Weiss law below 170 K which may be explained by crystal field effects of Yb3+.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926170118
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  • 92
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    Über die Verbindung Sr7Mn4O15 und Beziehungen zur Struktur von Sr2MnO4 und α-SrMnO3 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 617 (1992), S. 99-104 
    Details
    ISSN: 0044-2313
    Keywords: Strontium manganate, Sr7Mn4O15 ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Compound Sr7Mn4O15 and Structure Relations to Sr2MnO4 and α-SrMnO3The “compound” hitherto described as a α modification of Sr2MnO4 is shown to consist of a mixture of SrO and the new monoclinic compound Sr7Mn4O15 crystallizing in the space group P 21/c, a = 681.78(6), b = 962.24(8), c = 1038.0(1) pm, β = 91.886(7)°, Z = 2. Up to 0.3 mm long black crystals were grown from prereacted Sr7Mn4O15, SrO, and SrCl2 at 1350°C in a sealed platinum tube under argon. Its structure is related to α-SrMnO3. It contains layers of cornershared double octahedra [O2/2OMnO3MnO2O1/2]7- parallel to (100). Above 100 K the magnetism of Sr7Mn4O15 follows the Curie Weiss law with Θ ∼ -426 K and a moment μeff = 3.62 μB corresponding Mn4+.
    Notes: Die bisher als α-Modifikation von Sr2MnO4 beschriebene Substanz stellt ein Gemenge aus SrO und Sr7Mn4O15 dar. Bis zu 0,3 mm lange schwarze Einkristalle wurden durch Erhitzen von vorreagiertem Sr7Mn4O15, SrO und SrCl2 in einer unter Argon zugeschmolzenen Platinampulle auf 1350°C erhalten. Die neue Verbindung kristallisiert monoklin in der Raumgruppe P 21/c mit den Gitterkonstanten a = 681,78(6), b = 962,24(8), c = 1038,0(1)pm, β = 91,886(7)° und Z = 2 in einem neuen Strukturtyp, der mit α-SrMnO3 verwandt ist. Charakteristisch für die Struktur von Sr7Mn4O15 sind Schichten eckenverknüpfter Doppeloktaeder[O2/2OMnO3MnO2O1/2]7- parallel zur (100). Oberhalb 100K folgt der Magnetismus von Sr7Mn4O15 dem Curie-Weiss-Gesetz mit Θ ∼ -426K und einem Moment μeff = 3,62μB pro Mn entsprechend Mn4+.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926170117
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  • 93
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    Bis(benzoylpyridin-p-toluensulfonylhydrazido)nickel Ni(BPSH)2 · H2O  -  Beziehungen zwischen Struktur und Redox- bzw. Extraktionsverhalten heterocyclischer Sulfonamidochelate (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 613 (1992), S. 55-59 
    Details
    ISSN: 0044-2313
    Keywords: Nickel complex, Ni(BPSH)2 · H2O ; bis(benzoylpyridin-p-toluensulfonylhydrazido)nickel ; heterocyclic sulfonamido chelates ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Bis(benzoylpyridin-toluensulfonylhydrazido)nickel Ni(BPSH)2 · H2O  -  Relations between Structure, Redox, and Extraction Properties of Heterocyclic Sulfonamido ChelatesThe crystal structure of Ni(BPSH)2 · H2O was determined by x-ray diffraction: monoclinic, space group P21/c (Nr. 14); a = 15.077(4) Å, b = 14.901(3) Å, c = 16.335(3) Å, β = 95.74(1)°. R = 0.047 for a total of 5564 observed reflexions. Ni(BPSH)2 · H2O has a distorted tetrahedral structure with two six-membered chelate rings, one of them with a boat from. The electron system of the building blocks CNN⊖ within the chelate rings approaches that of a diazallyl group. The result is a high electron density on the sp2-hybridized donor atom N⊖ and, as a consequence, a short Ni—N⊖-distance (1.908 or 1.924 Å). The electronic properties of N⊖ also explain the high NH-acidity of the acid H(BPSH) (pks = 9,51 in 75 per cent dioxane) and the ligand field strength of BPSH⊖ which is low compared to that of other bidentate sulfonamido ligands and which is reflected in the paramagnetism of Ni(BPSH)2 · H2O.The redox behavior of metal chelates of the type, which is represented by Ni(BPSH)2 · H2O, is caused by a building block of the ligand which is also present in bipyridyl or in the 1,4-diaza-1,3-dienes. The central atoms M11 have only the function of interference factors.
    Notes: Die Kristallstruktur von Ni(BPSH)2 · H2O wurde durch Röntgenbeugung bestimmt: monoklin, Raumgruppe P21/c (Nr. 14), a = 15,077(4) Å, b = 14,901(3) Å, c = 16,335(3) Å, β = 95,74(1) ° R = 0,047 für 5564 beobachtete Reflexe. Ni(BPSH)2 ° H2O besitzt eine verzerrt tetraedrische Struktur mit zwei Chelatsechsringen, von denen einer in der Wannenform vorliegt. Die Baugruppen CNN⊖ innerhalb der Ringe weisen ein Elektronensystem auf, das sich an das einer Diazallylfunktion annähert. Die Folge davon ist eine hohe Elektronendichte auf dem sp2-hybridisierten Stickstoffhaftatom N⊖ und ein kurzer Ni—N⊖-Abstand (1,908 bzw. 1,924 Å). Die elektronischen Eigenschaften von N⊖ erklären weiterhin die hohe NH-Acidität der Säure H(BPSH) pks = 9,51 in 75% (Dioxan) und die verglichen mit anderen Sulfonamidochelatliganden geringe Ligandenfeldstärke von BPSH⊖, die sich im Paramagnetismus von Ni(BPSH)2 · H2O äußert.Das Redoxverhalten der Metallchelate des durch Ni(BPSH)2 · H2O repräsentierten Typs wird durch ein Bauelement des Liganden bestimmt, das sich im α, α′-Dipyridyl und in den 1,4-Diaza-1,3-dienen wiederfindet. Metallionen M2+ wirken über das Diazalylsystem lediglich als Störfaktoren.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926130109
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  • 94
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    Ein neuer Zugang zu Alkalivanadaten(IV,V) Die Kristallstruktur von Rb2V3O8 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 613 (1992), S. 63-66 
    Details
    ISSN: 0044-2313
    Keywords: Rubidium vanadate (IV, V) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A New Access to Alkali Vanadates(IV,V) Crystal Structure of Rb2V3O8By heating vanadium(V) oxide with rubidium iodide to 500°C, the vanadium experiences partial reduction and Rb2V3O8 is obtained. It has the fresnoite structure. Crystal data: a = 892.29(7), c = 554.49(9) pm at 20°C, tetragonal, space group P4bm, Z = 2. X-ray crystal structure determination with 620 observed reflexions, R = 0.027. V2O7 units share vertices with VO5 square pyramids, forming layers; a layer can be regarded as association product of VO2+ and V2O74- ions. The Rb+ ions between the layers have pentagonal-antiprismatic coordination.
    Notes: Beim Erhitzen von Vanadium(V)-oxid mit Rubidiumiodid auf ca. 500°C wird Vanadium partiell reduziert, es entsteht Rb2V3O8. Dieses kristallisiert in der Fresnoit-Struktur. Kristalldaten: a = 892,29(7), c = 554,49(9) pm bei 20°C, tetragonal, Raumgruppe P4bm, Z = 2. Röntgenstrukturbestimmung mit 620 beobachteten Reflexen, R = 2,7%. V2O7-Einheiten und quadratische Pyramiden VO5 sind untereinander zu Schichten eckenverknüpft; die Schicht kann als Assoziat aus VO2+ - und V2O74--Ionen aufgefaßt werden. Die Rb+-Ionen zwischen den Schichten sind verzerrt pentagonal-antiprismatisch koordiniert.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926130111
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  • 95
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    AlCl3 · 2NH3 - eine Verbindung mit der Kristallstruktur eines Tetraammindichloroaluminium-tetrachloroaluminats - [AlCl2(NH3)4]+[AlCl4]- (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 614 (1992), S. 25-29 
    Details
    ISSN: 0044-2313
    Keywords: Aluminiumtrichloride diammoniate ; tetraammine dichloro aluminium - tetrachloroaluminate ; preparation ; crystal structure ; i. r., mass spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: ACl3 · 2NH3 - a Compound with the Crystal Structure of a Tetraammine Dichloroaluminiumtetrachloroaluminate - [AlCl2(NH3)4]+[AlCl4]-Ammoniates of aluminiumchloride AlCl3 · xNH3 are in discussion as starting materials for the synthesis of aluminiumnitride. Therefore the reactions of melts of monoamminealuminiumchloride with ammonia were investigated. They react at 150°C within 10 min with one mole of ammonia to the diammoniate, [AlCl2(NH3)4]+[AlCl4]-. The pure compound can be obtained by sublimation at 200°C in vacuumline apparatus.X-ray structure determination on [AlCl2(NH3)4]+[AlCl4]- was carried out: see “Inhaltsübersicht”.
    Notes: Ammoniakate von Aluminiumchlorid, AlCl3 · xNH3 werden als Edukte für die Aluminiumnitridherstellung diskutiert. Deshalb wurden Reaktionen von geschmolzenem Monoamminaluminiumchlorid, AlCl3(NH3), mit Ammoniak untersucht. Die Schmelze setzt sich bei 150°C innerhalb von 10 min mit einem Mol Ammoniak zu dem Diammoniakat [AlCl2(NH3)4]+[AlCl4]- um. Ein phasenreines Produkt wird durch Sublimation bei 200°C in einer Vakuumapparatur erhalten.An Kristallen von [AlCl2(NH3)4]+[AlCl4]- wurde eine röntgenographische Strukturanalyse durchgeführt:Pnma, Z = 4, ρ = 1,675 g/cm3 a = 11,300(2), Å, b = 18,318(6) Å, c = 6,415(2) Å R = 0,035, Rw = 0,039, Z(F02) ≥ 3 s̰(F02) = 629, Z(Var.) = 85 Das Diammoniakat enthält gestreckte [AlCl2(NH3)4]+- Oktaeder und [AlCl4]--Tetraeder, deren Schwerpunkte so zueinander angeordnet sind wie Ni und As im NiAs-Typ. Neben ionogenen Wechselwirkungen treten Wasserstoffbrückenbindungen mit 3,44 Å ≤ d(N—H … Cl) ≤ 3,67 Å auf.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926140806
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  • 96
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    Ag5GeO4, das erste subvalente ternäre SilberoxidProfessor Rudolf Hoppe zum 70. Geburtstage gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 616 (1992), S. 95-100 
    Details
    ISSN: 0044-2313
    Keywords: Subvalent ternary silver oxide ; [Ag6]4+ cluster ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ag5GeO4, the First Subvalent Ternary Silver OxideApplying high oxygen pressure the first subvalent ternary silver oxide Ag5GeO4 was obtained (for crystallographic data c.f. “Inhaltsübersicht”). Ag5GeO4 contains tetrahedral GeO44--ions besides [Ag6]4+ clusters, which have not been observed in ternary silver oxides, so far. The electrical and magnetical properties prove the localisation of two paired electrons in each silver octahedron. The thermal decomposition occurs in two steps at 432.7 °C and 524.5°C.
    Notes: Durch Anwendung von Sauerstoffüberdruck gelang die Darstellung des ersten bezüglich Silber zweifelsfrei subvalenten Silberoxids, Ag5GeO4 (P21/n,a = 637,66(2) pm, b = 991,78(4) pm, c = 923,44(3)pm,β = 91,379(3)°, Z = 4, 2495 symmetrieunabhängige Reflexe, R = 0,061, Rw = 0,054). Ag5GeO4 enthält tetraedrische Orthogermanat-Ionen GeO44- und für ternäre Silberoxide neuartige [Ag6]4+-Cluster, neben Ag+ . Die elektrischen und magnetischen Eigenschaften belegen die Lokalisierung von jeweils zwei Elektronen in den Ag6--Einheiten. Der thermische Abbau erfolgt in zwei Stufen bei 432,7 °C und 524,5 °C.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926161015
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  • 97
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    Nd4Ti9O24: Präparation und StrukturProfessor Rudolf Hoppe zum 70. Geburtstage gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 616 (1992), S. 86-94 
    Details
    ISSN: 0044-2313
    Keywords: Nd4Ti9O24 ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of Nd4Ti9O24The compound Nd4Ti9O24 was prepared by heating mixtures of Nd2O3/TiO2 (1 : 4.5) at temperatures of T = 1 330°C in air (2× 1d). Single crystals of Nd4Ti9O24 were obtained by chemical transport reaction (T2→T1; T1 = 1000°C, T1 = 900°C, 14 d) using chlorine (p(Cl2, 298 K) = 1 atm) as transport agent with Nd4Ti9O24 as starting material.Nd4Ti9O24 crystallizes in the orthorhombic space group Fddd (No. 70) with a = 13.9926(11) Å, b = 35.2844(21) Å, c = 14.4676(17) Å (Z = 16). The structure was refined to give R = 4.0% and R, = 3.7%. Main building units are TiO6 octahedra, NdO6 distorted square antiprisms and NdO6 octahedra.
    Notes: Pulverförmige Präparate der Verbindung Nd4Ti9O24 ließen sich durch Erhitzen (an Luft; Pt-Tiegel) eines Gemenges Nd2O3/TiO2 (1 : 4,5) phasenrein darstellen (1 330°C, 2× 1 d). Einkristalle wurden durch chemischen Transport (T2 → T1; T2 = 1000 °C, T1 = 900°C, 14d) mit Nd4Ti9O24 als Startbodenkörper bei T2 sowie mit Chlor (p(Cl2 298 K) = 1 atm) als Transportmittel erhalten.Nd4Ti9O24 kristallisiert orthorhombisch: RG Fddd (No. 70) mit den Gitterkonstanten a = 13,9926(11) Å,b = 35,2844(21) Å, c = 14,4676(17) Å mit Z = 16. Die Struktur wurde bis zu R = 4,0% bzw. Rw = 3,7% verfeinert. Der Aufbau kann durch ein kompliziertes dreidimensionales Gerüst aus TiO6- und Nd(2)O6-Oktaedern beschrieben werden, in dessen Lücken Nd(1) und Nd(3) mit CN = 8 lokalisiert sind. Die Koordination der Metallteilchen 1äßt sich durch TiO6- Oktaeder, NdO8 quadratische Antiprismen (verzerrt) und durch NdO6-Oktaeder beschreiben.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926161014
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    Tl3Al7S12  -  ein neues Al-reiches Thioaluminat: Darstellung, Kristallstruktur und EigenschaftenProfessor Rudolf Hoppe zum 70. Geburtstage gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 616 (1992), S. 145-153 
    Details
    ISSN: 0044-2313
    Keywords: Thallium thioaluminate ; preparation ; crystal structure ; vibrational spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tl3Al7S12  -  a Novel Al-rich Thioaluminate: Preparation, Crystal Structure, and PropertiesThe new ternary phase Tl3Al7S12 was prepared from the binary compounds Tl2S and Al2S3 at 700 °C under vacuum. The structure of a yellow plateshaped single crystal was determined at room temperature. The compound crystallizes in the monoclinic polar space group P21 (No. 4) with a = 9.040(2), b = 12.381(2), c = 9.569(2) Å and β = 95.91(2)°.The polymeric anionic part of the structure can be described as a puckered layer-like arrangement of cornersharing [AlS4]-tetrahedra parallel to (001). The aluminium-sulfur layers are connected via single sulfur atoms. The voluminous monovalent thallium atoms bridge the layers of the anionic framework. The mean Al—S bond lengths are 2.227 Å for μ2-S—Al and 2.298 Å for μ2-S—Al. In the strongly asymmetric coordination sphere of thallium the Tl—S bond lengths vary from 3.009(9) to 3.907(9) Å and contain four short and two or three longer distances. A rather short Tl…Tl distance of 3.619(3) Å is observed between two of the three crystallographically independent Tl atoms, so that a weak bonding interaction has to be discussed. Vibrational spectroscopic data for the new phase are reported and discussed.
    Notes: Die neue ternäre Phase Tl3Al7S12 konnte aus den binären Komponenten Tl2S und Al2S3 bei 700 °C im Vakuum dargestellt werden. Die hellgelbe Verbindung kristallisiert in der monoklinen, polaren Raumgruppe P21 (No. 4) mit a = 9,040(2), b = 12,381(2), c = 9,569(2) Å und β = 95,91(2)°. Der polymere, anionische Teil der Kristallstruktur wird aus ausschließlich eckenverknüpften [AlS4]-Tetraedern so aufgebaut, daß eine gewellte, schichtartige Anordnung etwa parallel zu (001) resultiert. Zwischen den Schichten, die über einzelne Schwefelatome miteinander verbunden werden, sind die sterisch anspruchsvollen Tl+ -Kationen eingelagert. Die mittleren Al—S-Bindungslängen betragen für μ2-S—Al 2,227 Å und für μ3-S—Al 2,298 Å. Die Tl—S—Bindungslängen variieren von 3,009(9) bis 3,907(9) A mit vier einseitig orientierten kurzen und zwei bis drei längeren Abständen. Zwischen zwei der drei kristallographisch unabhängigen Thalliumatome wird ein kurzer Abstand von 3,619(3) Å beobachtet, so daß schwach bindende Wechselwirkungen diskutiert werden müssen. Die schwingungsspektroskopischen Daten der neuen Phase werden diskutiert.
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    URL: http://dx.doi.org/10.1002/zaac.19926161022
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    Zur Darstellung von Yttriumhydridhalogeniden YXHn (X = Cl, Br)Professor Rudolf Hoppe zum 70. Geburtstage gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 616 (1992), S. 157-161 
    Details
    ISSN: 0044-2313
    Keywords: Yttrium hydride halides ; YClHn, YBrHn (0.7 ≤ n ≤ 1.0) ; YClH2 ; YBrH2 ; preparation ; H-concentration ; phase relation ; X-ray powder investigation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Preparation of Yttrium Hydride Halides YXHn (X = Cl, Br)The compounds YCl and YBr described in a previous paper as “monohalides” in reality are hydridehalides YClHn and YBrHn with the H-concentration in the range 0.7 ≤ n ≤ 1.0. Dehydrogenation experiments on YCIH0.7 in all cases resulted in heterogeneous products consisting of YCl3, Y and YClHn. With increasing hydrogen content the c-lattice parameter decreases. Observed minimal c-lattice parameter is 2727.0(7) pm (for n ≍ 1), maximum c-lattice parameter is 2752.3(4) pm (for n ≍ 0.68). YBrHn crystallizes in the ZrBr-structure type, YClHn for 0.7 ≤ n ≤ 0.8 in the ZrBr-type, for 0.8 ≤ n ≤ 1.0 in the ZrCl-type.YXHn (X = Cl, Br) has a graphite like colour and in H atmosphere can be hydrogenated to the colourless compound YXH2. YClH2 and YBrH2 are isotypic with TbBrD2. A miscibility gap was found between YClH1.0 and YClH2.0.
    Notes: Die als Monohalogenide beschriebenen Verbindungen YCl und YBr enthalten stets Wasserstoff. Der H-Gehalt schwankt für YClHn und YBrHn im Bereich 0,7 ≤ n ≤ 1,0. Unterschreiten des Minimalwertes nmin = 0,7 führt bei präparativen Ansätzen oder bei Dehydrierungsversuchen stets zu heterogenen Produkten YCl3, Y and YClHn. Mit steigendem H-Gehalt nimmt die Länge der c-Gitterkonstante ab. Als kleinster Wert wird c = 2727,0(7) pm (n ≍ 1,00), als größter c = 2752,3(4)pm (n ≍ 0,68) beobachtet. YBrHn kristallisiert im ZrCl-Typ, YClHn für kleine H-Konzentrationen 0,7 ≤ n ≤ 0,8 im ZrBr-Typ, für große H-Konzentrationen 0,8 ≤ n ≤ 1,0 im ZrCl-Typ. Die graphitfarbenen Verbindungen YXHn (X = C1, Br) lassen sich in H-Atmosphäre bei 500 °C zu farblosem YXH2 hydrieren. YClHn und YBrH2 sind mit TbBrD2 isotyp. Zwischen YClH1,0, und YClH2,0 besteht eine Mischungslücke.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926161024
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    Kristallstruktur von RbKSProfessor Rudolf Hoppe zum 70. Geburtstage gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 616 (1992), S. 183-185 
    Details
    ISSN: 0044-2313
    Keywords: Rubidium potassium sulphide ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of RbKSThe colourless compound RbKS has been prepared for the first time by annealing a mixture of K2S and Rb2S. Very hygroscopic RbKS crystallizes in the orthorhombic space group Pnma with the lattice parameters a = 822.2(3), b = 504.3(4), c = 945.2(2)pm, Z = 4 in the anti-PbC12 structure type.
    Notes: Erstmals wurden Einkristalle von farblosem RbKS durch Tempern eines äquimolaren Gemenges aus Kaliumsulfid und Rubidiumsulfid bei 820 K er- halten. Die sehr hygroskopische salzartige Verbindung kristallisiert orthorhombisch, Raumgruppe Pnma, a = 822,2(3), b = 504,3(4), c = 945,2(2)pm, Z = 4 im anti-PbC12,-Strukturtyp.
    Additional Material: 2 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19926161029
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