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  • 1
    Electronic Resource
    Electronic Resource
    The structure of Mo4Cl8(PEt3)4: How unrecognized disorder previously reduced the quality of the refinement (1991)
    Springer
    Journal of cluster science 2 (1991), S. 121-129 
    Details
    ISSN: 1572-8862
    Keywords: Molybdenum tetranuclear cluster ; rectangular ; triethylphosphine ligand ; preparation ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract The preparation and structure of the title compound were reported several years ago by McCarly and co-workers ((1978).J. Am. Chem. Soc. 100, 7900). Curiously, it was reported that refinement of the structure converged at exceptionally high figures of merit (R=0.126;R w =0.158), but no reason was given. In view of a recent observation in this laboratory (Chen and Cotton (1991).J. Am. Chem. Soc. 113, 5857) that a similar type of compound, [Re4Cl8(μ-O)2(μ-OMe)2]2− exhibited a subtle but elegant disorder, we reexamined the crystal structure of the title compound. It is found to have 92% of the Mo4 rectangles in one orientation (the only one previously included in the refinement) and 8% in an orientation perpendicular to the main one. In both orientations the ligand positions are approximately the same. The figures of merit are nowR=0.041;R w =0.064. The three structure parameters previously reported are now only slightly different: Mo-Mo=2.210(1) vs. 2.211(3) Å; Mo-Mo'=2.897(1) vs. 2.901(2) Å; angle Mo-Clb-Mo=74.2[8]° vs. 74.4(2)°. We report here the complete structure.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00702953
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  • 2
    Electronic Resource
    Electronic Resource
    The characterization of high-tech materials: Perspectives, challenges, trends (1991)
    Springer
    Microchimica acta 104 (1991), S. 177-214 
    Details
    ISSN: 1436-5073
    Keywords: atomic structure ; crystal structure ; microstructure ; constructions ; topochemistry ; graphite ; glassy carbon ; pyrolytic carbon ; microelectronics ; carriers of information ; refractory metal alloys ; life time ; recrystallization ; fatigue ; photon probe techniques ; electron probe techniques ; ion probe techniques ; electrical field probes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract From the Stone Age on, developmental periods of mankind carry the names of materials. Materials determine the applicability of key technologies and these are in turn of major significance for the economic success and the social development in modern society. Today's high-tech materials are the consequence of an improved understanding of the structure and composition of matter and of the interplay of microstructure and minor and trace constituents. We can distinguish four basic dimensional structural categories of materials: (a) the atomic structure level; (b) the crystal, glassy or amorphous structural level; (c) the microstructural level; (d) the level of constructions. As an example, these structural levels are described in some detail for graphite, a material used extensively throughout Analytical Chemistry. Decisive differences at the microstructural level result in graphitic materials with very varying properties: polycrystalline electrographite, glassy carbon, and pyrolytic graphite. Examples for the use of these materials in ETAAS are discussed. Structural features together with topochemical and trace chemical characteristics are studied today by a wide variety of analytical instrumentation and methods of modern materials analysis which can be grouped into four categories of techniques: (a) photon probe techniques; (b) electron probe techniques; (c) ion probe techniques; (d) electrical field probes. The most important of those techniques are discussed shortly with respect to their main characteristics as lateral and depth resolution, detection sensitivity, additional bonding or structural information, depth profiling possibilities etc. The constructions are the ultimate level of a materials structure. Structures of microelectronic components reach dimensionally into the domain of microstructure whereas constructions in heavy industry are of meter-ton dimensions. Progress in the use of materials as carriers of information is visualized by a morphological comparison of the sound tracks of conventional records with the information imprinted in optical discs. It is important to conceive materials as dynamic systems with limited lifetime. Fatigue and recrystallization are prominent relevant phenomena which must be studied by microstructural and topochemical methods. Dispersion strengthened microalloys like TZM, HT-molybdenum and NS-tungsten are discussed as examples how materials can be improved with respect to their extended use under extreme conditions. Again, a thorough structural and topochemical characterization was the basis of a successful respective materials development although a multitude of relevant topochemical questions still remain to be solved. Lifetime investigations are an essential tool of materials development as well as quality control. Relevant investigations for various tube materials for ETAAS are discussed.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01245508
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  • 3
    Electronic Resource
    Electronic Resource
    Conformational analysis of fluorinated copolymers of tetrafluoroethylene (1991)
    Springer
    Colloid & polymer science 269 (1991), S. 477-482 
    Details
    ISSN: 1435-1536
    Keywords: Polytetrafluoroethylene ; copolymers ; conformation ; conformational disorder ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract Conformational analysis of fluorinated copolymers of tetrafluoroethylene (TFE) is performed by taking into account only intramolecular effects (isolated-chain model). In particular, variations of the chain conformation, which are induced by incorporating different side groups, such as −Cl, −CF3, −OCF3, −OCF2CF3, and −OCF(CF3)2, are investigated and discussed with respect to qualitative correlations between conformation, crystal structure, and supramolecular morphology.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00655885
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  • 4
    Electronic Resource
    Electronic Resource
    Atomistic calculations of crystal structures of polyisobutylene (1991)
    Springer
    Colloid & polymer science 269 (1991), S. 449-454 
    Details
    ISSN: 1435-1536
    Keywords: Polyisobutylene ; atomistic calculations ; conformational analysis ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract Semiempirical atomistic calculations are performed to investigate the crystalline structure of stretched poly(1,1-dimethylethylene), or polyisobutylene. The packing analysis was done without any lattice symmetry assumptions. The results are in good agreement with the x-ray analysis and favor Tanaka's model II. The calculations show several other crystalline structures with the chains in an all-gauche conformation. They have a somewhat higher density and may play a role in a hypothetical high-pressure phase of polyisobutylene.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00655881
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  • 5
    Electronic Resource
    Electronic Resource
    Structural studies of 2,2-Diphenyl-1-picrylhydrazine: A clathrate forming compound (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 10 (1991), S. 203-217 
    Details
    ISSN: 1573-1111
    Keywords: Diarylpicrylhydrazine ; clathrate ; single crystal ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract 2,2-Diphenyl-1-picrylhydrazine was crystallized from both tetrahydrofuran and chloroform. The crystal structures of samples from both preparations were determined by X-ray diffraction at low temperatures. Both crystals are clathrates with solvent molecules included as guest species in a host framework formed by the diphenylpicrylhydrazine molecules. The structures are rhombohedral, space groupR3. For the crystal from tetrahydrofuran, at 228 K,a = 25.820(4),c = 15.096(2) Å,Z = 18,R = 0.084 andwR = 0.133. For the crystal from chloroform, at 115 K,a = 25.453(12),c = 15.083(3) Å,Z = 18,R = 0.117 andwR = 0.153. Each unit cell contains three cavities which have approximate cylindrical shape with diameter 7.8 Å and height 6.0 Å, and 3 point symmetry. The integrity of the host framework is maintained only through van der Waals forces rather than through intermolecular hydrogen bonding as is found in many other known organic cathrates. The conformation of the trinitroanilino group of the hydrazine molecule is similar to that in the related trinitroanilinocarbazole molecule. The N-N bond approximates a single bond, and both hydrazine N atoms aresp 2 hybridized.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01066204
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  • 6
    Electronic Resource
    Electronic Resource
    Channel inclusion of potassium and tetrachloroplatinate ions in a complex formed between 1,3-diamino-2-propanone and K2PtCl4 in an acidic medium (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 10 (1991), S. 225-232 
    Details
    ISSN: 1573-1111
    Keywords: Diaminopropanone ; potassium tetrachloroplatinate ; channel inclusion ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystalline complex dipotassium 1,3-diammonio-2-propanone tetrachloroplatinate trihydrate, formulated as K2[(NH3CH2C)2O][PtCl4]2 · 3H2O, has been prepared while synthesizing complexes analogous tocis-dichlorodiamine Pt(II). Its structure is orthorhombic, space groupPnma,M r = 896.1,F(000) = 1640,a = 8.428(4),b = 20.360(10),c = 12.141(7)A,V = 2083.3Å3,Z = 4,D x = 2.860 g cm−3, μ(MoK x) = 196 cm−1, finalR = 0.083 for 1379 unique reflections. The structure consists of a very extended hydrogen bonded network which involves half of the PtCl4 2− ions, the organic molecules and the water molecules of hydration, leaving large oval channels which accommodate potassium cations and tetrachloroplatinate anions. Within the channel the potassium and tetrachloroplatinate ions pack in columns extending along the a axis. The dense packing is rather reminiscent of that found in the neat salt where each potassium ion is surrounded by six chlorine atoms which describe a polyhedron of a distorted trigonal prism with K+ —C1 distances ranging between 3.163–3.187 Å. There is some indirect evidence for the formation of 1,3-diammonio-2-propanone dications which counterbalance the charges of half of the PtCl4 2− ions by protonation of each of the amino nitrogens. The carbonyl oxygens, however, are involved only in a very weak O-C-O interactions along thea axis.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01066206
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  • 7
    Electronic Resource
    Electronic Resource
    Molecular encapsulation of transition metal complexes in cyclodextrins. Part 2. Synthesis and crystal structures of 2:1 adducts between α-cyclodextrin and metallocenium hexafluorophosphates [η5-C5H5)2M]PF6(M = Fe, Co, Rh) (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 10 (1991), S. 255-265 
    Details
    ISSN: 1573-1111
    Keywords: Cyclodextrin inclusion compound ; metallocene ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The title metallocenium salts form crystalline 2:1 host:guest inclusion compounds withα-cyclodextrin, [(η5-C5H5)2M]PF6 · 2α-CD · 8H2O (1, M = Fe;2, M = Co;3, M = Rh). The X-ray crystal structures of1 and3, and the lattice constants, crystal system and space group of2 have been determined. Crystal data: triclinic, space groupP1 (No. 1),Z = 1;1,a = 13.865 (2) Å,b = 13.839 (2) Å,c = 15.520 (2) Å,α = 91.43 (2)°,β = 85.81 (2)°,γ = 120.22 (2)°, andR F = 0.089 for 4257 observed MoK α reflections [I 〉 3δ(I)];2,a = 13.810 (2) Å,b = 13.872 (2) Å,c = 15.560 (2) Å,α = 93.99 (2)°,β = 87.06 (2)°,γ = 120.04 (2)°;3,a = 13.756 (1) Å,b = 13.863 (1) Å,c = 15.561 (2) Å,α =94.39 (1)°,β = 86.92 (1)°,γ = 119.89 (1)°, andR F = 0.061 for 11142 observed MoK α reflections [I 〉 3δ(I)]. In the crystals of1 and3, two α-cyclodextrin molecules are arranged head-to-head to form a dimer by means of intermolecular hydrogen bonding across the secondary hydroxyl faces of adjacent α-CD monomers. The dimers are stacked along the crystallographicc axis to form a channel-type structure. The metallocenium cation is encapsulated within the cavity of the dimer, while the PF 6 − anion is located outside the cavity, being centered between the primary hydroxyl faces of adjacent dimers. Eight water molecules of hydration per asymmetric unit reside in the spaces between the α-CD columns. In view of the almost identical crystal data for2 a similar structure can be assumed for the cobaltocenium adduct.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01066209
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  • 8
    Electronic Resource
    Electronic Resource
    The crystal structures of α, ω-diaminoalkanecadmium(II) tetracyanonickelate(II)-Aromatic molecule inclusion compounds. V. Toluidine clathrates of the hosts built of the diamines, 1,4-diaminobutane, 1.5-diaminonentane, and 1,8-diaminooctane (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 11 (1991), S. 137-152 
    Details
    ISSN: 1573-1111
    Keywords: cadium ; crystal structure ; Hofmann-diam-type ; 1,4-diaminobutane ; 1,5-diaminopentane ; 1,6-diaminohexane ; 1,8-diaminooctane ; tetracyanonickelate ; toluidine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structures have been analyzed for the threeo-toluidine clathrates,catena-[catena-μ-(1,4-diaminobutane)cadmium(II) tetra-μ-cyanonickelate(II)]-o-toluidine(2/3),4-o,catena-[catena-μ-(1,5-diaminopentane)cadmium(II) tetra-μ-cyanonickelate(II)]-o-toluidine(3/4),5-o, andcatena-[catena-μ-(1,8-diaminooctane)cadium(II) tetra-μ-cyanonickelate(II)]-o-toluidine(1/1),8-o, for am-toluidine onecatena-[catena-μ-(1,5-diaminopentane)cadmium(II) tetra-μ-cyano-nickelate(II)]-m-toluidine(1/1),5-m, and for ap-toluidine onecatena-[catena-μ-(1,8-diaminooctane)cadium(II) tetra-μ-cyanonickelate(II)]-p-toluidine(1/1),8-p. 4-o crystallizes in the triclinic space groupPī,a/Å = 9.806(3),b/Å = 14.388(3),c/Å = 7.725(2), α/° = 89.71(2), β/° = 89.96(2), γ/° = 98.12(2),V/Å3 = 1078.8(5),Z = 2, 3750 reflections,R = 0.056;5-o: tetragonalP4lmmm, (a = b)/Å = 7.485(7),c/Å = 10.06(3),V/Å3 = 563(2),Z = 1, 573 reflections,R = 0.19;8-o: monoclinicP2/m,a/Å = 11.513(4),b/Å = 7.626(1),c/Å = 7.101(1), β/° = 109.63(3),V/Å3 = 587.2(2),Z = 1, 1682 reflections,R = 0.058;5-m: orthorhombicPbam,a/Å = 12.254(6),b/Å = 20.62(1),c/Å = 7.804(1),V/Å3 = 1972(1),Z = 4, 2240 reflections,R = 0.059; and8-p: triclinic,Pī,a/Å = 11.52(1),b/Å = 7.632(3),c/Å = 7.039(4), α/° = 88.93(4), β/° = 109.71(5), γ/° = 82.81(9),V/Å3 = 576.9(6),Z = 1, 2598 reflections,R = 0.042. Their structures are substantially similar to the already-known structure ofcatena-[catena-μ-(1,6-diaminohexane)cadmium(II) tetra-μ-cyanonickelate(II)]-o-toluidine(1/1): the guest toluidine molecules are accommodated in the cavities formed betweencatena-[cadmium(II) tetra-μ-cyanonickelate(II)] layers bridged by the ambidentate α,ω-diaminoalkane ligands at the cadmium(II) atoms. The carbon chain length of the α,ω-diaminoalkane influences the number of cavities per formula unit and the deformation of the metal complex layers.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01153297
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  • 9
    Electronic Resource
    Electronic Resource
    Crystal and molecular structures ofp-(1,1,3,3-tetramethylbutyl)calix[5]arene and its 1 : 1 complex with toluene (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 11 (1991), S. 171-183 
    Details
    ISSN: 1573-1111
    Keywords: Calixarene ; inclusion compounds ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A cyclic pentamer was obtained fromp-(1,1,3,3-tetramethylbutyl) phenol. It crystallizes from a mixture of acetone and toluene at room temperature giving a 1 : 1 complex with toluene (compound A), whereas at 50°C the empty form (compound B) is obtained. Crystals of A are orthorhombic, space groupPna21,a = 20.083(2),b = 12.936(6),c = 28,423(1) Å,Z = 4, finalR value = 0.067. The empty form, B, is monoclinicP21/c,a = 18.695(2),b = 11.673(5),c = 35.100(4) Å, β = 114.33(1),Z = 4, finalR value = 0.135. The macrocycle is in the cone conformation for both compounds; the toluene molecule lies in the cone as often found for calix[4]arenes.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01153300
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  • 10
    Electronic Resource
    Electronic Resource
    Novel cage-like cavity accommodating a pair of guest molecules in the structure ofcatena-[dl-1,2-diaminopropanecadmium(II) tetra-μ-cyanocadmate(II)]-(1,2-dichloroethane)(1/1) (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 11 (1991), S. 397-403 
    Details
    ISSN: 1573-1111
    Keywords: Cadmium cyanide ; cadmium tetracyanocadmate ; crystal structure ; dichloroethane ; metal complex host ; propylenediamine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The title clathrate Cd(dl-pn)Cd(CN)4·CH2CICH2CI (pn=dl-1,2-diaminopropane=dl-propy-lenediamine) crystallizes in the monoclinic space groupP2 ,a = 8.278(2),b = 14.904(2),c = 14.477(1) Å,β = 91.24(1)°,V = 1785.7(1) Å3,Z = 4,R = 0.068 for 4993 independent reflections. A novel three-dimensional host is built of the alternate array of the pn-chelated octahedral Cd and the tetrahedral Cd(CN)4 linked at every N atom to the former Cd to provide a cage-like cavity for a pair of 1,2-dichloroethane guest molecules.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01041417
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  • 11
    Electronic Resource
    Electronic Resource
    Analysis of the steric strain in the polypeptide backbone of protein molecules (1991)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 11 (1991), S. 223-229 
    Details
    ISSN: 0887-3585
    Keywords: protein structure ; crystal structure ; dihedral angles ; cis peptides ; protein active sites ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The extent to which local strain is present in the polypeptide backbone of folded protein molecules has been examined. The occurrence of steric strain associated with nonproline cis peptide bonds and energetically unfavorable main chain dihedral angles can be identified reliably from the well ordered parts of high resolution, refined crystal structures. The analysis reveals that there are relatively few sterically strained features. Those that do occur are located overwhelmingly in regions concerned with function. We attribute this to the greater precision necessary for ligand binding and catalysis, compared with the requirements of satisfactory folding.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prot.340110307
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  • 12
    Electronic Resource
    Electronic Resource
    X-Ray Structure and Crystal Lattice Interactions of the Taxol Side-Chain Methyl Ester (1991)
    Springer
    Pharmaceutical research 8 (1991), S. 908-912 
    Details
    ISSN: 1573-904X
    Keywords: taxol side chain ; crystal structure ; crystal lattice interactions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A colorless, parallelepiped crystal of methyl (2R,3S)-N-benzoyl-3-phenylisoserinate belonging to the space group P2l with a = 5.414(4), b = 7.813(1), c = 17.802(7) Å, β = 90.87(4)°, Z = 2, V = 752.9 Å3, D calc = 1.32 g cm−3, and µcalc = 1.02 cm−1 was selected and the structure solved using direct methods. Refinement led to a final R = 0.079 for 819 [F o ≥ 5σ(Fo)] reflections. Intermolecular hydrogen-bonding interactions are prevalent in the crystal lattice of this compound.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1015863814901
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  • 13
    Electronic Resource
    Electronic Resource
    Crystal and molecular structure ofN,N′,N″-tritosyl-5,8,14,17,23,26-hexamethyl-2,11,20-triaza[3.3.3]-paracyclophane 1 : 1 dichloromethane clathrate (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 11 (1991), S. 41-48 
    Details
    ISSN: 1573-1111
    Keywords: N-tosyl azamacrocycles ; crystal structure ; clathrate formation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal and molecular structure of the title compound, C51H57N3O6S3·CH2Cl2 has been determined by single crystal X-ray analysis and refined to anR-value of 0.069 for 1032 reflections. The crystal is trigonal, space groupR3, witha = 21.255(7),c = 11.317(4), andZ = 3. One molecule of dichloromethane used as solvent is enclathrated in the crystal lattice.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01073682
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  • 14
    Electronic Resource
    Electronic Resource
    Air stable liquid clathrates: Solid state structure and hydrocarbon solubility of organic cation triiodide salts (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 11 (1991), S. 103-114 
    Details
    ISSN: 1573-1111
    Keywords: Liquid clathrate ; triiodide ; NMR ; crystal structure ; molten salts
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A series of air and water stable organic cation triiodide salts have been prepared and characterized. Almost all of the salts isolated sustain liquid clathrate phases in the presence of benzene or toluene, the compositions of which were determined via1H NMR spectroscopy. Two of the salts were also characterized via X-ray crystallography in order to determine the nature of any solid state interionic interactions (1-ethylpyridinium triiodide, monoclinic,P21/c,a = 9.6031(7),b = 15.129(3),c = 8.8160(16) Å, β = 104.192(11)°,Z = 4,R = 0.041 for 2463 independent observed reflections; 1,2,4-trimethylpyridinium triiodide, orthorhombic,Pbcm,a = 9.434(4), 20.176(4), 7.411(4) Å,Z = 4,R = 0.045 for 966 observed reflections).
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01153294
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  • 15
    Electronic Resource
    Electronic Resource
    Thermoanalytical investigation of the guest-release process in aromatic-guest clathrates of three-dimensional metal complex hosts (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 10 (1991), S. 29-37 
    Details
    ISSN: 1573-1111
    Keywords: activation energy ; benzene ; cadmium complex ; crystal structure ; ethylenediamine ; guest-release process ; propylenediamine ; pyrrole ; tetracyanocadmate ; tetracyanomercurate ; tetracyanonickelate ; thermal analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The guest-release process was investigated in terms of the activation energy evaluated by thermogravimetry for the en-Td-type clathratescatena-μ-[catena-μ-(ethylenediamine)cadmium(II) tetra-μ-cyanocadmate(II) or -mercurate(II)]-benzene(1/2), -benzene-d 6(1/2), and -pyrrole(1/2), the Hofmannen-type clathratescatena-[catena-μ-(ethylenediamine)cadmium(II) tetra-μ-cyanonickelate(Il)]-benzene (1/2) and -pyrrole(1/2), the Hofmann-pn-type clathratecatena-[catena-μ-(dl- orl-propylenediamine (cadmium(II) tetra-μ-cyanonickelate(II)]-pyrrole(2/3), and the pn-Td-type clathratescatena-[catena-μ-(dl-propylenediamine) or -(l-propylenediamine)cadmium(II) tetra-μ-cyanocadmate(II)]-benzene(2/3). Values of the activation energy are correlated with the structural change in the metal complex host accompanied by the release of the guest molecules. The crystal structure ofcatena-[ethylenediaminecadmium tetra-μ-cyanonickelate(II)], the residual host of the Hofmann-en-type, has been analyzed to elucidate the correlation.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01041637
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  • 16
    Electronic Resource
    Electronic Resource
    Stabilization of H2O ⁗ BF3 by hydrogen bonding to 18-crown-6 (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 10 (1991), S. 153-158 
    Details
    ISSN: 1573-1111
    Keywords: Hydrogen bonding ; 18-crown-6 ; boron trifluoride ; water ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The decomposition of H2O ⁗ BF3 in both the solid and solution states is rapid at room temperature, but 18-crown-6 ⁗ H2O ⁗ BF3,1, is stable to its melting point, 72°C.1 crystallizes in the monoclinic space groupC2/c witha = 27.273(9),b = 8.432(5),c = 22.936(9) Å, β = 128.33(4)°, andD c = 1.27 g cm−3 forZ = 8. Least-squares refinement based on 1409 observed reflections led to a finalR = 0.083. The BF3 is covalently bonded to the oxygen atom of the water molecule which in turn is hydrogen bonded to the 18-crown-6.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01041648
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  • 17
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    Electronic Resource
    Molecular structures of complexes of rare-earth metals with benzo-12-crown-4 (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 10 (1991), S. 191-202 
    Details
    ISSN: 1573-1111
    Keywords: Crown ethers ; rare-earth metals ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract An X-ray diffraction study of the complexes [Nd(N03)3(Bl2C4)] (I), [La(NO3)3(Bl2C4)(H2O)]·MeCN (II), and [Er(NO3)3(H2O)3]·2(Bl2C4)·MeCN (III), (B12C4 = benzo-12-crown-4) has been carried out. Crystals ofI are monoclinic,a = 8.050(2),b = 29.92(1),c = 7.741(2) Å,β = 102.71(2)°, space groupP21/c,Z = 4,R = 0.047 for 4718 reflections. Crystals of II are triclinic,a = 8.211(2),b = 10.613(3),c = 12.837(4)Å,a = 94.46(3),β = 108.19(2), γ = 89.98(3)°, space groupPT,Z = 2,R = 0.037 for 5611 reflections. Crystals ofIII are monoclinic,a = 9.847(3),b = 17.201(4),c = 21.664(5)Å,β = 100.85(2)°, space groupP21/n,Z = 4,R = 0.040 for 8328 reflections. The chemical structures of the complexes have been elucidated. The correlation between the radius of a particular lanthanide-ion and its coordination number (10 inI, 11 inII and 9 inIII) and consequently its influence on the composition of the complex is discussed. The possibilities of conformational changes in the B12C4 molecule depending on the type and size of the coordinated moiety (ions Nd(III) and La(III) inI andII and the H2O molecule inIII) are considered.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01066203
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  • 18
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    Electronic Resource
    Chirality of isomers of aldosterone formed in dilute alkali (1991)
    New York, NY [u.a.] : Wiley-Blackwell
    Chirality 3 (1991), S. 71-75 
    Details
    ISSN: 0899-0042
    Keywords: crystal structure ; aldosterone conformation ; correction of assigned configuration ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In the presence of dilute alkali at room temperature aldosterone undergoes rearrangement to form 11β,18:18,21-diepoxy-20,21-dihydroxy-4-pregnen-3-one (V). X-Ray crystallographic analysis demonstrates that isomers of both 18R, 20S, 21S and 18R, 20S, 21R configuration are formed rather than the 18R, 20R, 21R isomer postulated on the basis of examination of 1H-NMR spectra. The spectra appears to be consistent with the major component of the mixture. The 20S configuration observed is in agreement with the chirality assigned to the degradation product obtained when the same alkaline solution of aldosterone is subjected to reflux. The crystals of (V) are monoclinic P21, Z = 4 with a = 20.891(2), b = 6.3848(5), c = 16.067(2)Å, β = 122.09°(1) with two molecules in the asymmetric unit. Molecule A has the 20S,21S configuration and the molecules in the second site are a mixture of the 20S, 21S and 20S, 21R configuration in the ratio of 3:2.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/chir.530030112
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  • 19
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    [t-Bu2P]3P7 und (t-Bu2Sb)3P7 sowie Untersuchungen zur Bildung von Heptaphosphanen(3) mit PMe2-, PF2- und P(CF3)2-GruppenFrau Professor Marianne Baudler zum 70. Geburtstage am 27. April 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 594 (1991), S. 36-46 
    Details
    ISSN: 0044-2313
    Keywords: Tris(di-tert-butylphospha)heptaphosphanortricyclane, (t-Bu2P)3P7 ; Tris(di-tert-butylstiba)heptaphosphanortricyclane, (t-Bu2Sb)3P7 ; syntheses ; crystal structure ; 31{1H} n.m.r. data ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [t-Bu2P]3P7 and (t-Bu2Sb)3P7, as well as Investigations on the Formation of Heptaphosphanes (3) Containing PMe2, PF2, and P(CF3)2 GroupsTris(di-tert-butylphospha)heptaphosphanortricyclane (t-Bu2P)3P7 1 obtained by reacting Li3P7 · 3 DME with t-Bu2PF forms yellow crystals. (t-Bu2Sb)3P7 2 produced similarly from t-Bu2SbCl and Li3P7 · 3 DME didn't form crystals; it decomposes in a solution of toluene above -10°C. Both compounds were identified by their 31P{1H} NMR spectra, and 1 also by elemental analysis and single crystal structure determination (space group) P21/a, a = 1 712.0(9) pm, b = 1 105.1(7) pm, c = 1 854.0(10) pm, β = 94.96(4)°, Z = 4 formula units in the elementary cell).Attempts to synthesize (Me2P)3P7 3, (F2P)3P7 4 and [(F3C)2P]3P7 5 failed as dialkylchlorophosphanes as Me2PCl e. g. with Li3P7 · 3 DME react under Li/Cl exchange, dialkylfluorophosphanes (except t-Bu2PF) disproportionate, and neither PF3 nor (F3C)2PBr with Li3P7 · 3 DME give the desired products 4 or 5, resp.
    Notes: Tris(di-tert-butyl-phospha)-heptaphosphanortricyclan (t-Bu2P)3P7 1 entsteht durch Umsetzung von Li3P7 · 3 DME mit t-Bu2PF und bildet gelbe Kristalle. Das analog aus t-Bu2SbCl und Li3P7 · 3 DME gebildete (t-Bu2Sb)3P7 2 wurde nicht kristallin erhalten. Es zersetzt sich in Lösung (Toluol) oberhalb -10°C. Der Nachweis von 2 erfolgt über das 31P{1H}-NMR-Spektrum, der von 1 anhand des 31P{1H}-NMR-Spektrums, der Analyse und der Kristallstrukturbestimmung. 1 kristallisiert in der Raumgruppe P21/a mit Z = 4 Formeleinheiten; a = 1 712,0(9) pm, b = 1 105,1(7) pm, c = 1 854,0(10) pm, β = 94,96(4)°.Untersuchungen zur Bildung von (Me2P)3P7 3, (F2P)3P7 4, [(F3C)2P]3P7 5 führten nicht zum Ziel, weil Dialkylchlorphosphane wie Me2PCl (zur Bildung von 3) mit Li3P7 · 3 DME unter Li/Cl-Austausch reagieren, Dialkylfluorphosphane (ausgenommen t-Bu2PF) disproportionieren und PF3 sowie (F3C)2PBr mit Li3P7 · 3 DME nicht zu den Verbindungen 4 und 5 führen.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915940105
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  • 20
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    Ternäre intermetallische Phasen des Lithiums mit Elementen der 4. Neben- und 5. Hauptgruppe mit statistischer Metallverteilung im „Kationen“-TeilgitterProfessor Hanskarl Müller-Buschbaum zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 33-39 
    Details
    ISSN: 0044-2313
    Keywords: Intermetallic phases (ternary) ; lithium ; 4A metals ; 5B elements ; preparation ; crystal structure ; X-ray ; neutron scattering ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ternary Intermetallic Phases of Lithium, Transition Metals of the 4th Group and Elements of the 5th Maingroup with Statistical Metal Distribution in the „Cation“-SubstructureThe results of X-ray investigations and neutron diffraction on new and in some cases already known [1, 2] ternary intermetallic phases of Lithium with transition metals of the 4th group (b) and those of the 5th main group (X = P, As, Sb, Bi) will be reported. They crystallize in a partly „filled“ antifluorite type structure with a statistical Li/B-distribution in the tetrahedral sites. The structures are obviously stabilized by small amounts of enclosed d-elements.
    Notes: Es wird über Röntgenstrukturuntersuchungen und Neutronenbeugung an neuen und einigen schon bekannten [1, 2] ternären intermetallischen Phasen des Lithiums mit Elementen der 4. Nebengruppe (B) und Elementen der 5. Hauptgruppe (X = P, As, Sb, Bi) berichtet. Sie kristallisieren in einer teilweise „aufgefüllten“ Antifluorit-Struktur mit statistischer Li/B-Besetzung der Tetraederlücken, die offenbar durch den Einbau von geringen Mengen der Übergangsmetalle stabilisiert wird.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915970106
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  • 21
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    Synthese, Struktur und Eigenschaften der neuen Bromoselenate(II) [Se3Br8]2-, [Se4Br14]2- und [Se5Br12]2- Kristallstrukturen von [Cu(i-PropCN)4]2[Se3Br8], [EtPh3P]2[Se4Br14] und [n-Prop4N]2[Se5Br12]Professor Hanskarl Müller-Buschbaum zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 115-132 
    Details
    ISSN: 0044-2313
    Keywords: Selenium ; bromoselenates(II) ; preparation ; crystal structure ; FIR spectra ; Raman spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Structure, and Properties of the Novel Bromoselenates(II) [Se3Br8]2-, [Se4Br14]2-, and [Se5Br12]2-. Crystal Structures of [Cu(i-PropCN)4]2[Se3Br8], [EtPh3P]2[Se4Br14], and [n-Prop4N]2[Se5Br12]Using the symproportionation of elemental selenium and selenium tetrabromide in polar aprotic solvents a new class of tri-, tetra-, and pentanuclear bromoselenates(II) was obtained. In 2-methylpropionitrile solution the novel ion [Se3Br8]2- was stabilized and isolated as its black solvated copper salt. The crystals of [Cu(i-PropCN)4]2[Se3Br8] are monoclinic (C 2/c, a = 20.753(6), b = 13.344(4), c = 19.149(6) Å, β = 90.09(3)° at 140K, Z = 4) and contain trigonal star-shaped ions [Se3Br8]2- consisting of three edge-sharing square planar SeBr4 units. The mean terminal and μ3-bridging Se—Br bond lengths are 2.408 Å, respectively. [EtPh3P]2[Se4Br14] was obtained from dichloromethane solutions as dark red square-shaped crystals. The X-ray structure analysis (space group P 21/n, a = 11.400(3), b = 11.815(3), c = 20.720(A) Å, β = 92.50(3)° at 140 K, Z = 2) shows the crystals to contain tetranuclear ions [Se4Br14]2- that are built of two parallel planar [Se2Br6] units connected via two linear μBr-bridges. In the interesting delocalized electronic system a formal oxidation number of +1 has to be assigned to the bridging bromine. The mean terminal Se—Br bond length is 2.411 Å, the bridging bond lengths are 2.764 Å in the planar Se2Br6 units 2.594 Å in the linear Se—Br—Se bridges. Dark red [n-Prop4N]2[Se5Br12] was also isolated from CH2Cl2 solutions. It crystallizes in the tetragonal space group P 42/mnm (a = 14.798(3), c = 11.69(2) Å at 140 K, Z = 2) and its structure shows the novel pentanuclear ion [se5Br12]2-, consisting of a central square planar SeBr4 unit with two of its trans-edges being shared with additional pairs of square planar SeBr4, units. The anion can be described as two star-like Se3Br8 fragments with one sharing Se. The mean terminal and μ3-bridging Se—Br bond lengths are 2.343 Å and 2.956 Å, respectively. The vibrational spectra of the novel anions are reported and discussed.
    Notes: Durch Symproportionierung von elementarem Selen und Selentetrabromid in polaren protischen Lösungsmitteln wurde eine neue Klasse tri-, tetra- und pentanuklearer Bromoselenate(II) dargestellt. In 2-Methylpropionitril als Lösungsmittel wurde das strukturell neuartige Ion [Se3Br8]2- stabilisiert und als schwarzes solvatisiertes Kupfersalz isoliert. Kristalle von [Cu(i-PropCN)4]2[Se3Br8] sind monoklin (C2/c, a = 20,753(6), b = 13,344(4), c = 19,149(6) Å, β = 90,09(3)° bei 140K, Z = 4) und enthalten trigonale sternförmige Ionen [Se3Br8]2-, die aus drei kantenverknüpften quadratisch-planaren SeBr4-Einheiten bestehen. Die mittleren endständigen und μ3-verbrückenden Se—Br-Bindungslängen betragen 2,408 Å und 2,911 Å. [EtPh3P]2[Se4Br14] wurde aus Lösungen in Dichlormethan in Form dunkelroter Kristalle erhalten. Wie die Röntgenstrukturanalyse zeigt (Raumgruppe P21/n, a = 11,400(3), b = 11,815(3), c = 20,720(7) Å, β = 92,50(3)° bei 140K, Z = 2), enthalten sie vierkernige Ionen [Se4Br14]2-, die aus zwei parallel angeordneten, über lineare μBr-Brücken verknüpften Se2Br6-Einheiten aufgebaut sind. In diesem bemerkenswerten delokalisierten Elektronensystem muβ für das verbrückende Brom die formale Oxidationszahl + 1 angenommen werden. Die mittlere Se—Brterm-Bindungslängen sind 2,411 Å, die Brückenbindungslängen 2,764 Å in den planaren Se2Br6-Einheiten sowie 2,594 Å in den linearen Se—Br—Se-Brücken. Dunkelrotes [n-Prop4N]2[Se5Br12] konnte ebenfalls aus Lösungen in CH2Cl2 dargestellt werden. Es kristallisiert tetragonal (Raumgruppe P42/mnm, a = 14,798(3), c = 11,169(2) Å bei 140K, Z = 2). Seine Struktur enthält neuartige molekulare Ionen [Se5Br12]2-, die aus einer zentralen quadratisch-planaren SeBr4-Einheit bestehen, die über zwei trans-Kanten mit jeweils zwei weiteren quadratisch-planaren SeBr4-Einheiten verknüpft ist. Das Anion kann als über ein Selenatom verknüpfte Anordnung zweier sternförmiger Se3Br8-Fragmente beschrieben werden. Die mittleren endständigen und μ3-verbrückenden Se—Br-Abstände sind 2,343 Å und 2,956 Å. Über schwingungsspektroskopische Untersuchungen der neuen Anionen wird berichtet.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915970115
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  • 22
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    Kristallstruktur von gelbem K3OBrProfessor Hanskarl Müller-Buschbaum zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 197-200 
    Details
    ISSN: 0044-2313
    Keywords: Tripotassium bromide oxide ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of Yellow K3OBrK3OBr was prepared for the first time and investigated by X-ray methods. The yellow compound crystallizes with cubic symmetry, space group Pm3m, a = 521.3(1) pm, Z = 1 and shows like colourless Na3OCl anti-perovskite structure.
    Notes: K3OBr wurde erstmal dargestellt und an Einkristallen untersucht. Die gelbe Verbindung kristallisiert kubisch, Raumgruppe Pm3m, a = 521,3(1) pm, Z = 1 und weist wie farbloses Na3OCl anti-Perowskitstruktur auf.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915970122
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  • 23
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    Tetraphenylphosphonium-Heptathiacyclo-thioarsenat(III), PPh4[SAsS7]Professor Kurt Dehnicke zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 595 (1991), S. 211-215 
    Details
    ISSN: 0044-2313
    Keywords: Tetraphenylphosphonium heptathiacyclo thioarsenate(III) ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tetraphenylphosphonium Heptathiacyclo Thioarsenate(III), PPh4[SAsS7]From PPh4[As2SCl5] und K2S5 the title compound was obtained in acetonitrile among other products. According to an X-ray crystal structure analysis, it crystallizes in the orthorhombic space group Pna21 with a = 1 826.1(3), b = 1 312.0(2), c = 1 215.9(2) pm, Z = 4. The structure consists of PPh4+ and [SAsS7]- ions, AsS7 rings in the crown conformation as in S8 being present.
    Notes: Aus PPh4[As2SCl5] und K2S5 wurde in Acetonitril unter anderem die Titelverbindung erhalten. Nach der Röntgenstrukturanalyse mit 1474 beobachteten Reflexen (R = 7,1%, wR = 2,7%) kristallisiert sie rhombisch in der Raumgruppe Pna21; a = 1 826,1(3), b = 1 312,0(2), c = 1 215,9(2) pm, Z = 4. Die Struktur besteht aus PPh4+-und [SasS7]-Ionen, wobei AsS7-Ringe in der Kronenform wie beim S8 vorliegen.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915950120
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  • 24
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    Die Kristallstruktur von 2CaCl2 · 11HgCl2 · 16H2O, eines kubischen, quecksilberreichen Chloromercurats mit ikosaedrischen Hg6Cl13- und Hg5Cl13-BaugruppenProfessor Kurt Dehnicke zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 595 (1991), S. 193-202 
    Details
    ISSN: 0044-2313
    Keywords: Bis(octaaquocalcium)-tridecachlorohexamercurate-tridecachloropentamercurate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of 2CaCl2 · 11HgCl2 · 16H2O, a Cubic Mercury-rich Chloromercurate with Icosahedral Hg6Cl13 and Hg5Cl13 GroupsThe mercury-rich chloromercurate 2CaCl2 · 11HgCl2 · 16H2O has been obtained by crystallization from concentrated aqueous solutions of CaCl2 and HgCl2 at room temperature. In the cubic crystal structure (a = 18.170(3) Å, space group F23, Z = 4) a three-dimensional framework is formed by Hg6Cl13- and Hg5Cl133- anions with large cavities, in which the dodecahedral Ca(H2O)82+ cations are accomodated. 96 out of 104 Cl atoms in the cell form a lattice complex cP2[12i] with 8 Cl12 icosahedra, which are centered by Cl atoms. In four of these Hg atoms are situated on 6 edges thus forming Cl(HgCl2)6- anions, while the remaining four icosahedra hold 3 Hg atoms on edges and two on faces. Here the central Cl- anions are coordinated by 3 HgCl2 and 2 HgCl3 groups. The Hg5Cl13 and Ca(H2O)8 polyhedra are crystallographically disordered.
    Notes: Das quecksilberreiche Chloromercurat 2CaCl2 · 11HgCl2 · 16H2O ist durch Kristallisation aus konzentrierten wäßrigen Lösungen von CaCl2 und HgCl2 bei Raumtemperatur zu erhalten. In der kubischen Kristallstruktur (a = 18,170(3) Å, Raumgr. F23, Z = 4) bilden Hg6Cl13-- und Hg5Cl133--Anionen ein Gerüst mit großen Hohlräumen, in denen sich Ca(H2O)82+-Kationen mit dodekaedrischer Konformation befinden. Von den 104 Cl-Atomen in der Zelle bilden 96 einen Bauverband cP2[12i] mit acht Cl12-Ikosaedern, die jeweils durch ein Cl-Atom zentriert sind. Bei vier der Ikosaeder befinden sich 6 Hg-Atome auf Kanten, so daß Cl(HgCl2)6--Anionen resultieren. Bei den Hg5Cl133--Anionen besetzen jeweils 3 Hg-Atome Kanten und 2 Hg-Atome Flächen der Ikosaeder, so daß die zentralen Cl--Anionen von 3 HgCl2- und 2 HgCl3-Gruppen koordiniert sind. Die Hg5Cl13- und Ca(H2O)8-Baugruppen sind kristallographisch fehlgeordnet.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915950118
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  • 25
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    K4BeP2, K4BeAs2 und K4BeSb2-Verbindungen mit linearen [BeX2]4-. Anionen (X = P, As, Sb)Professor Kurt Dehnicke zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 595 (1991), S. 217-223 
    Details
    ISSN: 0044-2313
    Keywords: Tetrapotassium biphosphidoberyllate, -biarsenidoberyllate, -biantimonidoberyllate ; crystal structure ; vibrational spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: K4BeP2, K4BeAs2, and K4BeSb2 Compounds with Linear [BeX2]4- Anions (X = P, As, Sb)The title compounds are synthesized from the elements. K4BeP2 and K4BeAs2 are isostructural and crystallize trigonal rhombohedrally in the space group R3m (No. 166) with Z = 3. The partial structure of the potassium atoms corresponds to a closest packing of rotational ellipsoides, which envelope an elongated K14-polyhedron (combination of rhombohedron and hexagonal prism). The polyhedrons are filled with linear [BeX2]4- anions, which are the analoga to BeCl2 molecules. The bond lengths are: d(Be—P) = 198.2 pm and d(Be—As) = 206.0 pm. IR spectra confirm the presence of [Sb—Be—Sb]4- anionic groups in K4BeSb2, which crystallizes in the hexagonal system with Z = 2. The vibrational spectra of the compounds are measured. The assignment of the observed frequencies is based on the D∞h symmetry of an isolated [X—Be—X]4- unit.
    Notes: Die Titelverbindungen wurden aus den Elementen dargestellt. K4BeP2 und K4BeAs2 sind isotyp und kristallisieren trigonal-rhomboedrisch in der Raumgruppe R3m (Nr. 166) mit Z = 3. Die Teilstruktur der Kaliumatome entspricht einer dichtesten Packung von Rotationsellipsoiden, welche ein gestrecktes K14-Polyeder (Kombination von Rhomboeder und hexagonalem Prisma) einhüllen. Die Polyeder sind durch lineare [BeX2]4--Anionen aufgefüllt, Analoga des BeCl2-Moleküls. Die Bindungslängen sind d(Be—P) = 198,2 qm und d(Be—As) = 206,0 pm. IR-Spektren belegen die Existenz von [Sb—Be—Sb]4--Anionen auch in K4BeSb2, welches im hexagonalen System mit Z = 2 kristallisiert. Die Schwingungsspektren der Verbindungen wurden gemessen. Die Zuordnung der beobachteten Frequenzen basiert auf der D∞h-Symmetrie einer isolierten [X—Be—X]4--Einheit.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915950121
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  • 26
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    Synthese und Struktur der Platin(O)-Verbindungen [(dipb)Pt]2(COD) und (dipb)3Pt2 sowie des clusters Hg6[Pt(dipb)]4 (dipb = (i-Pr)2P(CH2)4P(i-Pr)2)Professor Kurt Dehnicke zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 595 (1991), S. 239-250 
    Details
    ISSN: 0044-2313
    Keywords: Platinum(0) compounds ; syntheses ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of the Platinum(0) Compounds [(dipb)Pt]2(COD) and (dipb)3Pt2 and of the Cluster Hg6[Pt(dipb)]4 (dipb = (i-Pr)2P(CH2)4P(i-Pr)2)The reduction of (dipb)PtCl2 with Na/Hg yields (dipb)Pt as an intermediate which reacts with the amalgam to form the cluster Hg6[Pt(dipb)]4 (3) or decomposes to (dipb)3Pt2 (2) and Pt. In the presence of COD [(dipb)Pt]2(COD) (1) is obtained. 1 crystallizes monoclinicly in the space group P21/c with a = 1596.1(4), b = 996.5(2), c = 1550.4(3) pm, β = 113.65(2)°, Z = 2. In the dinuclear complex two (dipb)Pt units are bridged by a 1,2-η2-5,6-η2 bonded COD ligand. Whereby the C = C double bonds are lengthened to 145 pm. 2 forms triclinic crystals with the space group P1 and a = 1002.0(2), b = 1635.9(3), c = 868.2(2) pm, α = 94.70(2)°, β = 94.45(2)°, σ = 87.95(1)°, Z = 1. In 2 two (dipb)Pt moieties are connected by a μ-dipb ligand in a centrosymmetrical arrangement. 3 is monoclinic with the space group C2/c and a = 1273.8(3), b = 4869.2(6), c = 1660.2(3) pm, β = 95.16(2)°, Z = 4. The clusters Hg6[Pt(dipb)]4 have the symmetry C2. Central unit is a Hg6 octahedron of which four faces are occupied by Pt(dipb) groups. The bonding in the cluster is discussed on the basis of eight Pt—Hg two center bonds of 267.6 pm and two Pt—Hg—Pt three center bonds with Pt—Hg = 288.0 pm.
    Notes: Bei der Reduktion von (dipb)PtCl2 mit Na/Hg entsteht intermediär (dipb)Pt, das mit dem Amalgam den Cluster Hg6[Pt(dipb)]4 (3) bildet oder sich zu (dipb)3Pt2 (2) und Pt zersetzt. Bei Anwesenheit von COD entsteht [(dipb)Pt]2(COD) (1). 1 kristallisiert monoklin in der Raumgruppe P21/c mit a = 1596,1(4), b = 996,5(2), c = 1550,4(3) pm, β = 113,65(2)°, Z = 2. Im zentrosymmetrischen Zweikernkomplex sind zwei (dipb)Pt-Einheiten über das 1,2-η2-5,6-η2-gebundene COD verbrückt. Die C = C-Doppelbindungen werden dabei auf 145 pm aufgeweitet. 2 bildet trikline Kristalle mit der Raumgruppe P1 und a = 1002,0(2), b = 1635,9(3), c = 868,2(2) pm, α = 94,70(2)°, β = 94,45(2)°, σ = 87,95(1)°, Z = 1. In 2 überbrückt ein μ-dipb-Ligand zwei (dipb)Pt-Gruppen in zentrosymmetrischer Anordnung. Monoklines 3 mit der Raumgruppe C2/c und a = 1273,8(3), b = 4869,2(6), c = 1660,2(3) pm, β = 95,16(2)°, Z = 4 ist aus Hg6[Pt(dipb)]4-Clustern mit der Symmetrie C2 aufgebaut. Zentrale Einheit des Clusters ist ein Hg6-Oktaeder, bei dem vier Flächen von (dipb)Pt-Gruppen besetzt sind. Die Bindungsverhältnisse werden auf der Grundlage von acht Pt—Hg-Zweizentrenbindungen mit Pt—Hg = 267,6 pm und zwei Pt—Hg—Pt-Dreizentrenbindungen mit Pt—Hg = 288,0 pm diskutiert.
    Additional Material: 4 Ill.
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  • 27
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    Synthese und Kristallstruktur von Quecksilber(II)-N,N′-bis(trimethylsilyl)benzamidinat, Hg[Ph—C(NSiMe3)2]2 (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 47-53 
    Details
    ISSN: 0044-2313
    Keywords: Mercury-N,N′-bis(trimethylsilyl)benzamidinate ; synthesis ; i.r. spectrum ; 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 Mercury(II)-N,N′-bis(trimethylsilyl)benzamidinate, Hg[Ph—C(NSiMe3)2]2The title compound has been synthesized by the reaction of N,N,N′-tris(trimethylsilyl)benzamidine with mercury(I)-acetate in boiling acetonitrile because of redox disproportionation, forming white crystal needles, which were characterized by IR spectroscopy as well as by an X-ray structure determination. Space group P1; Z = 2; 6846 observed unique reflections; R = 0.048. Lattice dimensions at -90 ° C: a = 1091.9, b = 1212.8, c = 1433.5 pm; α = 106.89°, β = 109.25°, γ = 90.62°. The compound forms a nearly centro-symmetric molecule structure with sp-hybridized Hg atom (r Hg—N = 207 pm).
    Notes: Die Titelverbindung entsteht bei der Reaktion von N,N,N′-tris(trimethylsilyl)-benzamidin mit Quecksilber(I)-acetat in siedendem Acetonitril durch Redox-Disproportionierung in Form weißer Kristallnadeln, die durch das IR-Spektrum und durch eine röntgenographische Kristallstrukturanalyse charakterisiert werden. Raumgruppe P1, Z = 2, 6 846 beobachtete unabhängige Reflexe; R = 4, 8%. Gitterabmessungen bei -90 °C: a = 1091,9; b = 1212,8; c = 1433,5 pm; α = 106,89α β = 109,25°; γ = 90,62°. Die Verbindung bildet eine nahezu zentrosymmetrische Molekülstruktur mit sp-hybridisiertem Hg-Atom (r Hg—N = 207 pm).
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915960107
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  • 28
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    Die Antimonid-Triantimonidometallate(III) Cs6K3Sb[AlSb3] und Cs6K3Sb[GaSb3]Professor Hanskarl Müller-Buschbaum zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 201-208 
    Details
    ISSN: 0044-2313
    Keywords: Antimonide triantimonidometallates(III) ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Antimonide Triantimonidometallates(III) Cs6K3Sb[AlSb3] and Cs6K3Sb[GaSb3]The novel compounds Cs6K3Sb[AlSb3] and Cs6K3Sb[GaSb3] are formed from stoichiometric mixtures of Cs, AlSb (GaSb) and KSb in sealed niobium ampoules at 950 K. The hexagonal structures are especially characterized by one-dimensional rod packings 1∞[Cs6K3Sb] which are formed from columns of condensed (Cs6K6/2) icosahedra. The icosahedra are centered by Sb3-- anions. The trigonal planar anions [AlSb3]6-- and [GaSb3]6-- are embedded between the icosahedra columns, and they are coordinated by alkali metal atoms. The FIR spectra were assigned to the vibrations of the [MSb3]6-- anions, with respect to the 6m2-D3h symmetry.(P63/mmc, No. 194; a = 1101.7 and 1097.2 pm; c = 1158.9 and 1150.1 pm; Z = 2; Single crystal data: 574 and 546 reflections; R = 0.073 and 0.029. Distances:d(Al—Sb) = 265.4 pm; d(Ga—Sb) = 265.1 pm; d(Sb—Cs) = 401.6-423.0 pm; d(Sb—K) = 358.6-367.3 pm).
    Notes: Die neuen Verbindungen Cs6K3Sb[AlSb3] und Cs6K3Sb[GaSb3] entstehen aus stöchiometrischen Gemischen von Cs, AlSb (GaSb) und KSb in verschweißten Niob-Ampullen bei 950 K. Besonderes Merkmal der hexagonalen Strukturen sind eindimensionale Stabpackungen 1∞[Cs6K3Sb], gebildet aus Säulen kondensierter (Cs6K6/2)-Ikosaeder. Die Ikosaeder sind von Sb3---Anionen zentriert. Zwischen den Ikosaedersäulen sind die trigonal-planaren Anionen [AlSb3]6-- bzw. [GaSb3]6-- eingebettet. Sie werden durch die Alkalimetallatome koordiniert. Die FIR-Spektren können den Schwingungen der Anionen [MSb3]6-- mit der Symmetrie 6m2-D3h zugeordnet werden.(P63/mmc, Nr. 194; a = 1101,7 bzw. 1097,2 pm; c = 1158,9 bzw. 1150,1 pm; Z = 2; Einkristalldaten: 574 bzw. 546 Reflexe; R = 0,073 bzw. 0,029. Abstände: d(Al—Sb) = 265,4 pm; d(Ga—Sb) = 265,1 pm; d(Sb—Cs) = 401,6-423,0 pm; d(Sb—K) = 358,6-367,3 pm).
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915970123
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  • 29
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    Zur Kenntnis von (Ba0,5Sr0,5)Cu2V2O8 und Ba(CuMg)V2O8 (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 602 (1991), S. 149-154 
    Details
    ISSN: 0044-2313
    Keywords: Alkaline earth ; copper ; vanadium ; oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On (Ba0,5Sr0,5)Cu2V2O8 and Ba(CuMg)V2O8Single Crystals of (A): (Ba0.5Sr0.5)Cu2V2O8 and (B) Ba(CuMg)V2O8 were prepared by solid state reactions below the melting points of the starting mixtures. Both compounds were examined by X-ray technique. They crystallize in the space groups (A): 142d [No. 122]; a = 12.65; c = 8.18 Å; Z = 8; and (B): 141/acd [No. 142]; a = 12.50; c = 8.33 Å; Z = 8. In (A) are Ba2+ plus Sr2+ and in (B) are Cu2+ plus Mg2+ in statistical distribution. The square pyramidal Cu2+ coordination in (A) is changed to an octahedron in (B), by replacing Cu2+ by Mg2+.
    Notes: Einkristalle von (A): (Ba0,5Sr0,5)Cu2V2O8 und (B): Ba(CuMg)V2O8 wurden durch Feststoffreaktionen dicht unterhalb des Schmelzpunktes der jeweiligen Reaktionsgemenge erhalten. Zellparameter und Atompositionen wurden röntgenographisch bestimmt. Die Verbindungen kristallisieren in den Raumgruppen (A): 142d, [Nr. 122] mit a = 12,65; c = 8,18 Å; Z = 8; (B): 141/acd; [Nr. 142] mit a = 12,50; c = 8,33 Å; Z = 8. In (A) sind Ba2+ und Sr2+, in (B) Cu2+ und Mg2+ statistisch verteilt. Die tetragonal pyramidale Koordination von Cu2+ in (A) ändert sich durch den Einbau von. Mg2+ in (B) in eine gestreckt oktaedrische.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916020116
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  • 30
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    Zinc and cadmium adducts of 2,2′-Bis(pyrazol-1-yl) propane,(L—L), a sterically hindering ligand. Crystal structure of (L—L)Zn[OC(=O)CF3]2(H2O) (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 602 (1991), S. 169-177 
    Details
    ISSN: 0044-2313
    Keywords: Zinc ; Cadmium ; 2,2′-bis(pyrazol-1-yl)propane ; adduct complexes ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zink- und Cadmium-Addukte des 2,2′-Bis(pyrazol-1-yl)propan, (L—L), einem sterisch anspruchsvollen Liganden. Kristallstruktur des (L—L)Zn[OC(=O)CF3]2(H2O)1:1 Addukte zwischen dem Titelliganden und MX2 (M = Zn oder Cd; X = Cl, Br, I oder C2F3O2) bzw. den ionischen Verbindungen [(L—L)5Zn2(H2O)2](ClO4) 4 und [(L—L)2 Cd(H2O)2](ClO4)2 wurden dargestellt. Diese sind stabil im festen Zustand und in Aceton-Lösung, nicht jedoch in Dimethylsulfoxid-Lösung. In der Struktur des (L—L)Zn(H2O)[O—C(=O)CF3]2 liegt, auf Grund einer durch die Methylgruppen verursachten sterischen Behinderung, eine verzerrte trigonale Bipyramide vor, in der zwei Sauerstoffatome (vom Wasser und Trifluoroacetat) und ein Stickstoffatom in der äquatorialen Ebene liegen. Die axialen Zn—X-Bindungen (X = N = 2,125(3) Å; X = O = 2,085(4) Å) sind länger als die äquatorialen.
    Notes: 1:1 adducts between the title ligand and MX2 (M = Zn or Cd; X = Cl, Br, I or trifluoroacetate) as well as ionic compounds [(L—L)5Zn2(H2O)2](ClO4) 4 and [(L—L)2Cd(H2O)2](ClO4) 2 are stable in the solid state and in acetone solution, but not in dimethylsulphoxide. In (L—L)Zn(H2O)[O—C(=O)CF3]2 two oxygen atoms (belonging to water and to one O—C(=O)CF3) at 2.039(4) and 2.008(4) Å from Zn, and one nitrogen atom (Zn—N 2.067(3) Å) from the chelating L—L define the basal plane of a trigonal bipyramid, which is distorted owing to the steric requirements of the bridgehead methyls of L—L; the axial Zn—X bonds (X = N 2.125(3) Å; X = O 2.085(4) Å), are longer than the equatorial Zn—X bonds.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916020118
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  • 31
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    Preparation and crystal structure of Nb6.74 Ta5.26S4 - a new compound in the ternary system Ta—Nb—SDedicated to Professor Hans-Georg von Schnering on his 60th Birthday (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 598 (1991), S. 353-362 
    Details
    ISSN: 0044-2313
    Keywords: Niobium tantalum sulfide ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung und Kristallstruktur von Nb6,74Ta5,26S4 - einer neuen Verbindung im ternären System Ta—Nb—SNb6,74Ta5,26S4 ist mittels Hochtemperaturtechnik dargestellt worden. Die Kristallstruktur wurde aus Einkristall-Röntgenbeugungsdaten bestimmt (R/Rw = 0,0588/0,0655). Die Verbindung kristallisiert orthorhombisch, Raumgruppe Pnma mit a = 959,11 (26), b = 336,37 (10) und c = 3282,51 (74) pm, Z = 4. Die Struktur entspricht eher der von Nb-reichen als der von Ta-reichen Sulfiden. Die Metall-Koordinationen sind bekappte, verzerrte kubische Prismen und pentagonale Prismen während die Schwefelkoordinationen bekappte trigonale Prismen sind.
    Notes: Nb6.74Ta5.26S4 has been prepared by high temperature techniques. The crystal structure has been determined from single crystal X-ray diffraction data (R/Rw = 0.0588/0.0655). The compound crystallizes in the orthorhombic space group Pnma with unit cell dimensions a = 959.11 (26) pm, b = 336.37 (10) pm, and c = 3282.51 (74) pm. The orthorhombic cell contains four formula units. Its structure is similar to that of Nb-rich sulfides, rather than to that of Ta-rich sulfides. The metal coordinations are capped distorted cubic prisms and pentagonal prisms while the coordinations of sulfur are capped trigonal prisms.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915980132
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  • 32
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    Hydrate schwacher und starker Basen. V. Die Kristallstrukturen von KOH · 2H2O (Substruktur) und KOH · 4H2OProfessor Wilhelm Kuchen zum 65. Geburtstage am 27. Mai 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 601 (1991), S. 73-82 
    Details
    ISSN: 0044-2313
    Keywords: Potassium hydroxide dihydrate ; tetrahydrate ; preparation ; 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. V. Crystal Structures of KOH · 2H2O (Substructure) and KOH · 4H2OIn the context of studies on formation and structure of base hydrates the crystal structures of KOH · 2H2O and KOH · 4H2O have been determined. For both structures, Mokα diffractometer data were used, obtained at -150°C, which allowed also the complete set of H atoms to be localized and refined. The dihydrate, melting incongruently at 33°C, crystallizes with a superstructure. The substructure, which is reported here, is tetragonal with space group I41/amd and Z = 8 formula units per unit cell of dimensions a = 7.154 and c = 13.415 Å. With 462 independent observed reflections an R value of 0.026 was obtained. K(H2O)8+ cubes via common faces form rods and these in a tetragonal four-layer packing pattern are further linked into a three-dimensional framework. The OH-ions, hydrogen-bonded by the H2O molecules, are located with a twofold disorder in additional cubes of this frame-work, not occupied by K+ ions. The tetrahydrate, melting congruently at -33.7°C, is monoclinic with space group P21/c and Z = 4. The unit cell dimensions are a = 6.951, b = 11.530, c = 7.080 Å and β = 99.19°. With 2198 independent observed reflections the final R value is 0.025. Trigonal K(H2O)6+ prisms across common edges form layers, which are linked with each other via OH- ions and only loosely cation-bonded H2O molecules.
    Notes: Im Rahmen von Untersuchungen zu Bildung und Struktur von Basehydraten wurden die Kristallstrukturen von KOH · 2H2O und KOH · 4H2O bestimmt. Benutzt wurden hierzu bei -150°C mit Mokα-Strahlung erhaltene Diffraktometerdaten, mit denen auch sämtliche H-Atome lokalisiert und verfeinert werden konnten. Das bei 33°C inkongruent schmelzende Dihydrat kristallisiert mit einer Überstruktur. Die Substruktur, über die hier berichtet wird, ist tetragonal mit der Raumgruppe 141/amd und Z = 8 Formeleinheiten pro Elementarzelle sowie den Gitterkonstanten a = 7,154 und c = 13,415 Å. Mit 462 unabhängigen beobachteten Reflexen wurde ein R-Wert von 0,026 erreicht. K(H2O)8+ -Würfel bilden über gemeinsame Flächen Stäbe und durch weitere Verknüpfung ein nach dem Muster einer tetragonalen Vierschichtpackung aufgebautes dreidimensionales Gerüst. Die OH- -Ionen befinden sich, durch Wasserstoffbrücken von den H2O-Molekülen gebunden, mit zweifacher Fehlordnung in weiteren, nicht mit K+ -Ionen besetzten Würfeln dieses Gerüsts. Das bei -33,7°C kongruent schmelzende Tetrahydrat ist monoklin mit der Raumgruppe P21/c und Z = 4. Die Gitterkonstanten betragen a = 6,951, b = 11,530, c = 7,080 Å und β = 99,19°. Mit 2198 unabhängigen beobachteten Reflexen liegt der abschließende R-Wert bei 0,025. Trigonale K(H2O)6+ -Prismen bilden über gemeinsame Kanten Schichten, die durch Wasserstoffbrücken über OH- -Ionen und nur locker an die Kationen gebundene H2O-Moleküle miteinander verbunden sind.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916010109
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    Synthese und Kristallstrukturen der Alkali-Tetraiodoindate(III), Alnl4 (A = Li, K, Rb, Cs)Professor Klaus Brodersen zum 65. Geburtstage am 12. August 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 602 (1991), S. 31-37 
    Details
    ISSN: 0044-2313
    Keywords: Alkali-iodoindates(III) ; indium ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structures of the Alkali-tetraiodoindates(III), AInI4 (A = Li, K, Rb, Cs)Single crystals of the yellow alkaliiodoindates(III), AInI4 (A = Li, K, Rb, Cs), are obtained from mixtures of the binary components by slow cooling of the melts. LiInI4 is isotypic with LiAlCl4: monoclinic, P21/c, Z = 4; a = 838.9(4); b = 751.2(3); c = 1526,7(8) pm; β = 92.67(4)°. KInI4 belongs to the ATIX4 type of structure (A = NH4, K, Rb; X = Br, I): cubic, F4 3c, Z = 24; a = 1990.8(1) pm. RbInI4 crystallizes with the β-GaBr2 type: trigonal, R3c, Z = 18; a = 2452.6(6); c = 978.6(4) pm. CsInI4 is isostructural with CsTII4: monoclinic, P21/c, Z = 4; a = 738.4(1); b = 1875.7(3); c = 853.6(2) pm; β = 105.75(2)°. In all structures almost regular tetrahedral polyhedra [InI4]- occur. The coordination numbers of the alkali cations cover the wide range from 6 (Li+) via 9 (Rb+) and 11 (Cs+) to 12 (K1+).
    Notes: Einkristalle der gelben Iodoindate(III) der Alkalimetalle, AInI4 (A = Li, K, Rb, Cs), erhält man aus Gemengen der binären Komponenten durch langsames Abkühlen der Schmelzen. LiInI4 ist isotyp mit LiAlCl4: monoklin, P21/c, Z = 4; a = 838,9(4); b = 751,2(3); c = 1526,7(8) pm; β = 92,67(4)°. KInI4 gehört zum ATIX4-Typ (A= NH4, K, Rb; X= Br, I): kubisch, F4 3c, Z = 24; a = 1990,8(1) pm. RbInI4 kristallisiert im β-Ga[GaBr4]-Typ: trigonal, R3c, Z = 18; a = 2452,6(6); c = 978,6(4) pm. CsInI4 ist isotyp mit CsTII4: monoklin, P21/c, Z = 4; a = 738,4(1); b = 1875,7(3); c = 853,6(2) pm; β = 105,75(2)°. Stets liegen annähernd tetraedrische Baugruppen [InI4]- vor. Die Koordinationszahlen der Alkali-Kationen überstreichen das Spektrum von 6 (Li+) über 9 Rb+, 11 (Cs+) bis 12 (K1+).
    Additional Material: 6 Tab.
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  • 34
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    Synthese und Kristallstruktur von PbMo5O8; ein reduziertes Oxomolybdat mit Mo10O28-Oktaederdoppeln (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 602 (1991), S. 49-63 
    Details
    ISSN: 0044-2313
    Keywords: Oxomolybdates ; cluster ; crystal structure ; HRTEM ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of PbMo5O8; a reduced Oxomolybdate with Mo10O28 Double OctahedraThe crystal structure of the new phase PbMo5O8 contains oligometric Mo clusters which consist of two edge-sharing Mo6 octahedra connected according to Mo10O6iO4/2i-iO16/2i-a. The compound is isotypic with LaMo5O8. Isolated, divalent Pb atoms are located in the “channels” of the monoclinic structure (a = 999.3(2) pm, b = 924.7(1) pm, c = 753.6(2) pm, β = 109.39(2)°, P21/a. Compared to the compound In 11Mo40O62 the Mo—O distances (average 206 pm) and the Mo—Mo distances within the octahedral units (average 275 pm) are slightly decreased by 1 and 4 pm, respectively. The very short Mo—Mo distances (278 pm) between the cluster units which are not observed in In11Mo40O62 (320 pm) are due to excess electrons in these inter-cluster bonds which would otherwise occupy antibonding cluster states.
    Notes: Mit der neuen Phase PbMo5O8 wurde ein weiteres Beispiel für oligomere Mo-Cluster aus zwei kantenverknüpften Mo6-Oktaedern gefunden, die nach Mo10O6iO4/2i-iO16sol;2i-a verknüpft sind. Die Verbindung ist isotyp zu LaMo5O8. In den „Kanälen“ der monoklinen Struktur a = 999,3(2) pm, b = 924,7(1) pm, c = 753,6(2) pm, β = 109,39(2)°, P21/a) findet man isolierte, zweiwertige Pb-Atome. Gegenüber der Verbindung In11Mo40O62 sind die Mo—O-Abstände mit durchschnittlich 206 pm nur gering um 1 pm und die Mo—Mo-Abstände innerhalb der oktaedrischen Baueinheiten mit durchschnittlich 275 pm ebenfalls nur schwach um 4 pm verkürzt. Allerdings findet man mit 278 pm sehr kurze Mo—Mo-Abstände zwischen den Clustereinheiten, die so nicht bei In11Mo40O62 (320 pm) beobachtet werden können. An diesen inter-Cluster-Bindungen sind überschüssige Elektronen beteiligt, die andernfalls antibindende Clusterzustände besetzen würden.
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    URL: http://dx.doi.org/10.1002/zaac.19916020106
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  • 35
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    Über die Kronenetherkomplexe [K(15-Krone-5)2]3[Sb3I12], [TeCl3(15-Krone-5)][TeCl5] und [TeCl3(15-Krone-5)]2[TeCl6] (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 55-61 
    Details
    ISSN: 0044-2313
    Keywords: Crown ether complexes ; tellurium ; antimony ; syntheses ; i.r. spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Crown Ether Complexes [K(15-Crown-5)2]3[Sb3I12], [TeCl3(15-Crown-5)][TeCl5], and [TeCl3(15-Crown-5)]2[TeCl6]Orange-coloured crystals of [K(15-crown-5)2]3[Sb3I12] are formed in the reaction of potassium iodide with antimony triiodide and 15-crown-5 in acetonitrile solution. An X-ray structure determination reveals severe disorder of the crown ether molecules, which coordinate to the potassium atoms in a sandwich array; so only the [Sb3I12]3- ion and the potassium positions were ascertained. The anion is a centrosymmetric trimer (symmetry C2h), which can be understood as central SbI63- ion, coordinated by two SbI3 molecules. (Space group C2/m), Z = 2, 3263 observed, independent reflections, R = 0.06, lattice dimensions at 20°C: a = 2541.1 pm, b = 1441.7 pm, c = 1588.4 pm, β = 113.33°.The tellurium complexes [TeCl3(15-crown-5)] [TeCl5] and [TeCl3(15-crown-5)]2[TeCl6] are prepared by reaction of TeCl4 with 15-crown-5 in acetonitrile solution, forming yellow-green crystals sensitive to moisture. They are characterized by their i.r. spectra.
    Notes: Orange Kristalle [K(15-Krone-5)2]3[Sb3I12] entstehen durch Einwirkung von Kaliumiodid auf Antimontriiodid bei Anwesenheit von 15-Krone-5 in Acetonitrillösung. Wegen Fehlordnung der die Kaliumionen sandwichartig koordinierenden Kronenethermoleküle konnten röntgenogrpahisch in der Struktur nur das [Sb3I12]3--Ion sicher aufgeklärt werden. Es bildet ein zentrosymmetrisches Trimer (Symmetrie C2h), das sich als zentrales SbI63--Ion mit zwei koordinierten SbI3-Molekülen auffassen läßt. Raumgruppe C2/m, Z = 2, 3263 unabhängige beobachtete Reflexe, R = 6,2%. Gitterabmessungen bei 20 °C: a = 2541,1; b = 1441,7; c = 1588,4 pm, β = 113,33°.Die Tellurokomplexe [TeCl3(15-Krone-5)] [TeCl5] und [TeCl3(15-Krone-5)]2[TeCl6] entstehen aus TeCl4 und 15-Krone-5 in Acetonitrillösung als gelbgrüne, feuchtigkeitsempfindliche Kristalle, die durch ihre IR-Spektren charakterisiert werden.
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    URL: http://dx.doi.org/10.1002/zaac.19915960108
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  • 36
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    Über ein Oxidchlorid des Calciums: Ca4OCl6 (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 89-92 
    Details
    ISSN: 0044-2313
    Keywords: Calcium oxychloride ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: An Oxychloride of Calcium: Ca4OCl6Ca4OCl6 (hexagonal, P63mc, Z = 2), a = 905.8(3), c = 686.3(4) pm, (R = 0.031) crystallizes as colourless needles from reducing melts (CaCl2, Ca) that contain small amounts of „oxygen“. It contains „isolated“ tetrahedral units [Ca4O] and is isotypic with e.g., Ba4OCl6, Yb4OCl6 and K6HgS4. Ca4OCl6 does not form in the dehydration process of, for example, CaCl2 · 6 H2O.
    Notes: Ca4OCl6 (hexagonal, P63mc, Z = 2, a = 905.8(3)); c = 686.3(4) pm, (R = 0,031) kristallisiert in Form farbloser Nadeln aus „reduzierenden Schmelzen“ (CaCl2, Ca), die wenig „Sauerstoff“ enthalten. Es enthält „isolierte“ tetraedrische [Ca4O]-Einheiten und ist isotyp mit z. B. Ba4OCl6, Yb4OCl6 oder K6HgS4. Ca4OCl6 entsteht nicht beim Entwässern von z. B. CaCl2 · 6 H2O.
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    URL: http://dx.doi.org/10.1002/zaac.19915960112
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  • 37
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    Untersuchungen über Polythiocuprate(I) [Cu(Sx)]-. 3. Kristallstruktur von [H3N—C2H4—NH3][Cu(S5)]2 · 4 H2O (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 111-119 
    Details
    ISSN: 0044-2313
    Keywords: Polythiocuprates(I) ; ethylenediammonium bis(pentathiocuprate(I)) tetrahydrate ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Studies on Polythiocuprates(I) [Cu(Sx)]-. 3. Crystal Structure of [H3N—C2H4—NH3][Cu(S5)]2 · 4 H2OThe title compound crystallizes with Z = 2 in the monoclinic space group P21/c (Nr. 14) with cell dimensions a = 8.820(1) Å, b = 15.532(3) Å, c = 6.999(2) Å and β = 96.92(4)°. For 2368 independent reflections the structure was refined to R = 0.070 and Rw = 0.045.The structure contains endless [Cu(S5)]nn- anion-chains ∥c and is stabilized by hydrogen bonds N—H…S, N—H…O, O—H…S, and O—H…O. Each copper atom is tetrahedrally coordinated by four sulfur atoms from three different (S5)2- chains. There are CuS4 and Cu2S3 five-ring systems, which are linked together by common edges forming the one-dimensional chains.
    Notes: Die Titelverbindung kristallisiert monoklin in der Raumgruppe P21/c (Nr. 14) mit den Gitterdimensionen a = 8,820(1) Å, b = 15,532(3) Å, c = 6,999(2) Å, β = 96,92(4)° und zwei Formeleinheiten in der Elementarzelle. Unter Verwendung von 2368 symmetrieunabhängigen Reflexen konnte die Struktur bis auf Zuverlässigkeitsfaktoren von R = 0,070 und Rw = 0,045 verfeinert werden.Die Struktur ist aus polymeren [Cu(S5)]nn--Anionenketten ∥c aufgebaut und wird durch Wasserstoffbrückensysteme N—H…S, N—H…O, O—H…S und O—H…O stabilisiert. Jedes Cu-Atom ist tetraedrisch von 4 S-Atomen umgeben, die aus drei aus drei verschiedenen (S5)2--Ketten stammen. Dabei liegen über Kanten zu Ketten verknüpfte CuS4- und Cu2S3-Fünfringsysteme vor.
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    URL: http://dx.doi.org/10.1002/zaac.19915960116
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  • 38
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    Benzamidinium-Hexachlorostannat Synthese und Kristallstruktur (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 133-138 
    Details
    ISSN: 0044-2313
    Keywords: Benzamidinium hexachlorostannate ; synthesis ; crystal structure ; i.r. spectrum ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Benzamidinium Hexachlorostannate: Synthesis and Crystal Structure[Ph—C(NH2)2SnCl6] has been prepared by the reaction of hydrogen chloride with the amidinato complex [Ph—C(NSiMe3)2SnCl3] in CH2Cl2 solution, forming colourless crystals. which were characterized by IR spectroscopy as well as by an X-ray structure determination. Space group P21/c, Z = 4, 3070 observed unique reflexions, R = 0.029. Lattice dimensions at -50°C: a = 892.5, b = 1076.7, c = 1175.6 pm, β = 109.3°. The compound consists of benzamidinium ions C6H5—C(NH2)2+ and anions SnCl62-, which are connected by a network of N—H…Cl hydrogen bridges.
    Notes: [Ph—C(NH2)2]2SnCl6 entsteht in Form farbloser Einkristalle durch Einwirkung von Chlorwasserstoff auf eine Lösung des Amidinatokomplexes [Ph—C(NSiMe3)2SnCl3] in Dichlormethan. Die Verbindung wird durch das IR-Spektrum und durch eine röntgenographische Strukturanalyse charakterisiert. Raumgruppe P21/c, Z = 4, 3070 beobachtete unabhängige Reflexe, R = 2,9%. Gitterabmessungen bei -50°C: a = 892,5; b = 1076,7; c = 1175,6 pm; β = 109,3°. Die Verbindung besteht aus Benzamidinium-Kationen C6H5—C(NH2)2+ und SnCl62--Ionen, in denen ein Netz von N—H…Cl-Wasserstoffbrücken besteht.
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    URL: http://dx.doi.org/10.1002/zaac.19915960118
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  • 39
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    Über die Bildung und Kristallstruktur von Mg(HSO4)2 · H2O (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 167-171 
    Details
    ISSN: 0044-2313
    Keywords: Magnesium bis(hydrogensulfate) hydrate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Formation and Structure of Mg(HSO4)2 · H2OMg(HSO4)2 reacts with water under formation of its monohydrate, Mg(HSO4)2 · H2O. This reaction proceeds crystallographically oriented and is reversible. Mg(HSO4)2 · H2O crystallized monoclinic in the space group P21/n, with the unit cell parameters a = 8.623(2), b = 5.014(1), c = 15.428(3) Å, β = 101.32(2)°, V = 654 Å3, Z = 4. The crystal structure of Mg(HSO4)2 · H2O consists of two types of SO3OH-tetrahedra connected over three common oxygen atoms with three different MgO6-octahedra. This motif forms layers parallel to the xy-plane. The layers are arranged at a distance of c/2 and are linked via hydrogen bonds which start from the water of crystallization situated between the layers.
    Notes: Mg(HSO4)2 bildet durch Wasseraufnahme das Monohydrat Mg(HSO4)2 · H2O. Diese Reaktion verläft kristallographisch orientiert und ist reversibel. Mg(HSO4)2 · H2O kristallisiert in der monoklinen Raumgruppe P21/n mit den Gitterkonstanten a = 8,623(2), b = 5,014(1), c = 15,428(3) Å, β = 101,33(2)°, V = 654 Å3, Z = 4. Die Kristallstruktur des Mg(HSO4)2 · H2O ist charakterisiert durch 2 Sorten von SO3OH-Tetraedern, die jeweils über drei gemeinsame Sauerstoffatome mit drei verschiedenen MgO6-Oktaedern verknüpft sind. Dieses Strukturmotiv bildet Schichten parallel zur xy-Ebene. Die Schichten folgen im Abstand von c/2 aufeinander und werden über H-Brücken miteinander verknüpft, die vom Hydratwasser ausgehen, das zwischen den Schichten positioniert ist.
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    URL: http://dx.doi.org/10.1002/zaac.19915960122
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  • 40
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    Li3Sr3Ni4N4: Ein Niedervalentes Nitridoniccolat mit ∞1[NiN]-KettenProfessor Hanskarl Müller-Buschbaum zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 61-67 
    Details
    ISSN: 0044-2313
    Keywords: Lithium strontium nitridoniccolate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Li3Sr3Ni4N4: An Low-Valency Nitridoniccolate with ∞1[NiN]-ChainsIsometric black-reflecting crystals of Li3Sr3Ni4N4 (orthorhombic, Immm; a = 401.1(1) pm, b = 708.8(3) pm, c = 1663.0(8) pm; Z = 2) were obtained by wall-reaction of Li4SrN2 in closed nickel tubes (heating rate 50°C/h; reaction at 800°C for 20 h; cooling rate 10°C/h). The crystal structure contains ∞1[NiN]-chains (Ni—N: 177.3(1) pm and 177.8(1) pm) which run parallel to the [010] direction. Lithium and strontium are arranged in planes (010) perpendicular to the [NiN]-chains and interconnect the chains via the nitrogen atoms. Lithium is in a two-fold (linear; Li—N: 200.7(1) pm and 200.4(7) pm), strontium is in three-and four-fold (distorted trigonal-and square-planar) N-coordination (Sr—N: 264.5(5) pm, 268.0(7) pm and 277.6(6) pm, resp.). Nitrogen is in an octahedral surrounding by Ni, Li and Sr; the coordination-octahedra NNi2Sr4 and NNi2Li3Sr are condensed by sharing common edges and apices. The three-dimensional framework contains one-dimensional fragments of the (inverse) octahedral structures of the ReO3 and Rutile structure types.
    Notes: Isometrische, schwarz-glänzende Einkristalle von Li3Sr3Ni4N4 (orthorhombisch, Immm; a = 401,1(1) pm, b = 708,8(3) pm, c = 1663,0(8) pm; Z = 2) wurden in geschlossenen Nickelampullen durch Reaktion von Li4SrN2 mit dem Tiegelmaterial dargestellt (Aufheizraten 50°C/h; 20 h bei 800°C; Abkühlrate 10°C/h). Die Kristallstruktur enthält parallel [010] verlaufende ∞1[NiN]-Ketten (Ni—N: 177,3(1) pm und 177,8(1) pm). Lithium und Strontium sind in Ebenen (010) senkrecht zu den [NiN]-Ketten angeordnet und verknüpfen diese über die Stickstoffatome. Lithium ist zweifach (linear; Li—N: 200,7(1) pm und 200,4(7) pm), Strontium ist sowohl verzerrt trigonal-planar (Sr—N: 264,5(5) pm und 268,0(7) pm) als auch planar-quadratisch (Sr—N: 277,6(6) pm) von Stickstoff koordiniert. Stickstoff selbst ist oktaedrisch von Ni, Li und Sr umgeben; die Koordinationsoktaeder NNi2Sr4 und NNi2Li3Sr werden über gemeinsame Ecken und Kanten miteinander verknüpft. Der insgesamt dreidimensionale Strukturverband enthält eindimensionale (inverse) Fragmente der Oktaederstrukturen des ReO3- und Rutil-Typs.
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    URL: http://dx.doi.org/10.1002/zaac.19915970109
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  • 41
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    Ag18(SiO4)2(Si4O13), das erste Silbersilicat mit gemischten AnionenProfessor Hanskarl Müller-Buschbaum zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 79-86 
    Details
    ISSN: 0044-2313
    Keywords: Silver silicate ; mixed-anion silicate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ag18(SiO4)2(Si4O13), the First Mixed-Anion Silver(I) SilicateThe system Ag2O/SiO2 has been investigated at Ag : Si = 3 : 1 by solid state reactions. Ag6Si2O7(II) forms from the binary components applying elevated oxygen pressures (p(O2) = 0.2 GPa) at 560-580°C. By adding conc. NH3-solution to the same starting mixtures Ag6Si2O7(I) forms at 500-550°C. Hitherto unknown (Ag4SiO4)2 · Ag10Si4O13 is the product if the temperature is kept below 470°C. (Ag4SiO4)2 · Ag10Si4O13 transforms in an irreversible phase transition to Ag6Si2O7(I) at T = 495 ± 10°C. The crystal structure of (Ag4SiO4)2 · Ag10Si4O13 (C2/m; a = 1201.7(1), b = 1060.7(1), c = 607.4(1) pm, β = 106.7(1)°; 1927 independent reflections; R = 0.06; Rw = 0.05) is constituted from orthosilicate and catena-tetrasilicate anions. The catena-tetrasilicate anions exhibit 2/m point symmetry. The intense red colour indicates the existence of weak Ag—Ag bonding interactions (shortest Ag+—Ag+ separation: 282.1 pm).
    Notes: Das System Ag2O/SiO2 wurde bei dem Schnitt Ag : Si = 3 : 1 präparativ untersucht. Aus den binären Komponenten entsteht in einer Festkörperreaktion unter Sauerstoffdrucken 〉 0,2 GPa und im Temperaturbereich von 560-580°C Ag6Si2O7(II) als offensichtlich thermodynamisch stabile Phase. Bei Zusatz von konz. NH3 bildet sich zwischen 500 und 550°C Ag6Si2O7(I) und unterhalb 470°C (Ag4SiO4)2 · Ag10Si4O13. Diese neu erhaltene Verbindung wandelt sich bei 495 ± 10°C irreversibel in Ag6Si2O7(I) um. Die Kristallstruktur von (Ag4SiO4)2 · Ag10Si4O13 (C2/m; a = 1201,7(1), b = 1060,7(1), c = 607,4(1) pm, β = 106,7(1)°; Z = 2; 1927 unabhängige Reflexe; R = 0,06; RW = 0,05) enthält nebeneinander Orthosilicat- und catena- Tetrasilicatanionen. Letztere haben die Lagesymmetrie 2/m. Die intensiv rote Eigenfarbe wird auf schwache Ag—Ag-Wechselwirkungen (kürzester Ag—Ag-Abstand: 282, 1 pm) zurückgeführt.
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    URL: http://dx.doi.org/10.1002/zaac.19915970111
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  • 42
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    Rb[Re3Br10]  -  das erste ternäre Rhenium(III)-Halogenid mit KettenstrukturProfessor Hanskarl Müller-Buschbaum zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 107-113 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium bromides ; cluster ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Rb[Re3Br10]  -  the First Ternary Rhenium(III) Halide with a Chain StructureRb[Re3Br10] crystallizes on evaporation of a hydrobromic acid solution of rhenium tribromide and rubidium bromide as dark red-brown single crystals. The crystal structure (monoclinic; C2/m; a = 1469.09(10); b = 1085.75(8); c = 1019.15(8) pm; β = 91.81(1)°; Vm = 245.1(2) cm3mol-1; Z = 4) is built up of chains along [010] of [Re3Br12] units that are connected via two edges. The anionic chains are held together by rubidium ions. Each cation is surrounded by eight bromide ions at distances between 332 and 368 pm with four additional bromide ions at 401 to 427 pm. This is the first example of a ternary rhenium halide with a chain structure. Only salts with isolated cluster anions [Re3X12-y(H2O)y](3-y)- (X = Cl, Br; y = 0-3) have been known so far.
    Notes: Aus bromwasserstoffsaurer Lösung von Rheniumtribromid und Rubidiumbromid kristallisieren beim Eindunsten dunkelrotbraune Einkristalle von Rb[Re3Br10] aus. Die Kristallstruktur (monoklin; C2/m; a = 1469,09(10); b = 1085,75 (8); c = 1019,15(8) pm; β = 91,81(1)°; Vm = 245,1(2) cm3mol-1; Z = 4) baut sich aus Ketten doppelt kantenverknüpfter [Re3Br12]-Baugruppen entlang [010] auf. Die anionischen Stränge kantenverknüpfter Cluster werden von Rubidiumionen zusammengehalten. Dabei ist jedes Kation von acht Bromid-Ionen in einem Abstand von 332-368 pm umgeben sowie von vier weiteren in einem Abstand zwischen 401 und 427 pm. Dies ist das erste Beispiel eines ternären Rhenium(III)-halogenids mit Kettenstruktur. Bislang waren nur Salze mit isolierten Clustern [Re3X12-y(H2O)y](3-y)- (X = Cl, Br; y = 0-3) bekannt.
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    URL: http://dx.doi.org/10.1002/zaac.19915970114
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    Das erste Gadoliniumcarbidfluorid: Gd2CF2Professor Hanskarl Müller-Buschbaum zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 145-150 
    Details
    ISSN: 0044-2313
    Keywords: Gadolinium carbide fluoride ; condensed clusters ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The First Gadolinium Carbide Fluoride: Gd2CF2Gd2CF2, the first gadolinium carbide fluoride is prepared by reaction of stoichiometric amounts of GdF3, Gd, and C at 1250°C in sealed Ta-capsules. It is isotypic with Gd2CBr2 (space group P3m1; a = 373.11(4) and c = 642.5(1) pm). The Gd atoms surround the C atoms octahedrally. Such Gd6C octahedra are condensed via edges to form octahedral sheets, which are separated by double slabs of F-- ions.
    Notes: Mit Gd2CF2 konnte erstmals ein Gadoliniumcarbidfluorid dargestellt werden. Man erhält Gd2CF2 durch Reaktion von stöchiometrischen Mengen GdF3, Gd und C bei 1250°C in verschweißten Ta-Ampullen. Es ist isotyp mit Gd2CBr2 (Raumgruppe P3m1; a = 373,11(4) und c = 642,5(1) pm). Die C-Atome sind von Gd-Atomen oktaedrisch umgeben. Diese Gd6C-Oktaeder sind zweidimensional zu Oktaederschichten kondensiert, die durch F---Doppelschichten voneinander getrennt sind.
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    URL: http://dx.doi.org/10.1002/zaac.19915970117
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  • 44
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    Darstellung und Kristallstruktur von Kupfer(II)-monofluorophosphat-Dihydrat CuPO3F · 2H2OProfessor Helmut Köhler in memoriam (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 600 (1991), S. 231-238 
    Details
    ISSN: 0044-2313
    Keywords: Copper(II) monofluorophosphate dihydrate ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Salts of Halogenophosphoric Acids. XVII. Preparation and Crystal Structure of Copper(II) Monofluorophosphate Dihydrate CuPO3F · 2H2OCopper(II) monofluorophosphate dihydrate, CuPO3F · 2H2O 1 was obtained by the reaction of aqueous NH4HPO3F and acid (NH4)2PO3F solutions, respectively, using acetone or ethanol as precipitating agents. The thermal dehydration of 1 gives the water-free copper monofluorophosphate CuPO3F (2). 1 crystallizes in the monoclinic space group P21/c with a = 761,44, b = 780,97, c = 921,02 pm, β = 112,94° and Z = 4.
    Notes: Bei der Reaktion von wäßrigen NH4HPO3F- bzw. sauren (NH4)2PO3F-Lösungen mit Kupfer(II)-Salzen wird unter Zusatz von Aceton bzw. Ethanol als Fällungsmittel Kupfer(II)-monofluorophosphat-Dihydrat CuPO3F · 2H2O 1 als kristalliner Niederschlag gebildet. Aus 1 läßt sich durch thermische Entwässerung wasserfreies Kupfer(II)-monofluorophosphat CuPO3F 2 herstellen.1 kristallisiert in der monoklinen Raumgruppe P21/c mit a = 761,44, b = 780,97, c = 921,02 pm, β = 112,94° und Z = 4.
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    PdSCl, ein molekulares Palladium(II)-disulfidchlorid mit achtkernigen Pd8(S2)4Cl8-Komplexen und vierfach überbrückenden DisulfidgruppenProfessor Hans Georg von Schnering zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 598 (1991), S. 253-258 
    Details
    ISSN: 0044-2313
    Keywords: Palladium(II) disulfidechloride ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: PdSCl, a Molecular Palladium(II) Disulfidechloride with Octanuclear Pd8(S2)4Cl8 Groups and with Tetra Metal-coordinated bridging Disulfide GroupsBlack crystals of PdSCl have been obtained by reaction of Pd with S2Cl2 in closed quartz ampoules at 200°C. The compound is to be formulated as a Palladium(II)-disulfidechloride consisting of Pd8(S2)4Cl8 molecules with approximately D4h symmetry. In the octanuclear complexes Pd atoms form a cube, where bridging disulfide groups are found in front of 4 faces and μ2-bridging Cl atoms on 8 edges. In the monoclinic crystal structure (a = 8.763(2) Å; b = 9.082(2) Å; c = 13.662(4) Å; β = 91.748(23)°; V = 1086.8 Å3; Z = 16 PdSCl; Space gr. P21/n) the molecules form a cubic closed arrangement.
    Notes: Schwarze Kristalle von PdSCl wurden durch Umsetzung von Pd-Metall mit S2Cl2 in geschlossenen Ampullen bei 200°C erhalten. Die Verbindung ist ein Palladium(II)-disulfidchlorid, aufgebaut aus molekularen Pd8(S2)4Cl8-Gruppen mit annähernd D4h-Symmetrie. In den achtkernigen Komplexen bilden Pd-Atome einen Würfel mit S2-Gruppen vor vier Flächen und Cl-Atomen vor 8 Kanten. In der monoklinen Kristallstruktur (a = 8,763(2) Å; b = 9,082(2) Å; c = 13,662(4) Å; β = 91,748(23)°; V = 1086,8 Å3; Z = 16 PdSCl; Raumgr. P21/n) sind die Moleküle kubisch dichtest gepackt.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915980122
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    Untersuchungen über Zinn(IV)-alkoxide. I Kristall- und Molekülstruktur des Zinn(IV)-isopropanolat-Isopropanolsolvats, Sn(OiPr)4 · i-PrOHProfessor Hans-Georg von Schnering zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 598 (1991), S. 259-268 
    Details
    ISSN: 0044-2313
    Keywords: Tin(IV)-isopropoxide-isopropanol solvate ; preparation ; 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. I. Crystal and Molecular Structure of Tin(IV)-isopropoxide-Isopropanol Solvate, Sn(OiPr)4 · i-PrOHThe isopropanol complex of tin(IV)-isopropoxide has been prepared by the reaction of tin tetrachloride with sodium isopropoxide. The compound forms colourless, moisture sensitive crystals, which in dry air easily release the coordinated solvent molecules. The crystal and molecular structure of Sn(OiPr)4 · i-PrOH has been determinated by single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P21/c with a = 1174.2(5), b = 1428.5(3), c = 1234.1(3) pm, β = 95.37(1)° and Z = 4. The crystal structure consists of discrete, dimeric molecules in which the two tin atoms are bridged by two alkoxide groups. The octahedral coordination sphere of each tin atom is completed by one solvent molecule which, in addition, forms one hydrogen bridge to an alkoxide group of the neighboring tin atom.
    Notes: Der Isopropanolkomplex des Zinn(IV)-isopropanolats wurde durch Reaktion von Zinntetrachlorid mit Natriumisopropanolat in Isopropanol hergestellt. Die Verbindung bildet farblose, feuchtigkeitsempfindliche Kristalle, die an trockener Luft das koordinierte Lösungsmittelmolekül sehr leicht abgeben. Die Kristall- und Molekülstruktur von Sn(OiPr)4 · i-PrOH wurde durch Röntgenstrahlbeugung an einem Einkristall bestimmt. Die Verbindung kristallisiert in der monoklinen Raumgruppe P21/c mit den Gitterkonstanten a = 1174,2(5), b = 1428,5(3), c = 1234,1(3) pm, β = 95,37(1)° und Z = 4. Die Kristallstruktur besteht aus diskreten, dimeren Molekülen, in denen die beiden Zinnatome über zwei Alkoxidreste verbrückt werden. Die oktaedrische Koordinationssphäre an den Zinnatomen wird durch jeweils ein Lösungsmittel-Molekül vervollständigt, das zusätzlich eine Wasserstoffbrücke zu einem Alkoxidrest am benachbarten Zinnatom bildet.
    Additional Material: 3 Ill.
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    Synthesis, structure, and properties of LaSrCuGaO5Dedicated to Professor Hans-Georg von Schnering on his 60th Birthday (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 598 (1991), S. 327-338 
    Details
    ISSN: 0044-2313
    Keywords: Lanthanum strontium copper gallate ; preparation ; crystal structure ; magnetic susceptibility ; electrical resistivity ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Präparation, Struktur und Eigenschaften von LaSrCuGaO5Die neue Brownmillerit-verwandte Verbindung, LaSrCuGaO5, wird dargestellt und charakterisiert. Sie kristallisiert in der orthorhombischen nicht-zentrosymmetrischen Raumgruppe Ima2.Die Gitterparameter sind a = 16,383(1) Å, b = 5,5293(7) Å, c = 5,3275(6) Å. Die Struktur ist der des Perowskits verwandt, enthält aber geordnete Sauerstoffleerstellen in den zweidimensionalen Gallium-Sauerstoff-Schichten, was zur tetraedrischen Koordination der Gallium-Kationen führt. Andere wichtige Strukturmerkmale sind die gewellten Kupfer-Sauerstoff-Ebenen und die statische Verteilung der Lanthan- und Strontium-Kationen über die A-Lage. Genaue Gitterkonstanten-Bestimmungen zeigen eine Dehnung der a-Achse um 0,17 Å bei Dotierung mit Strontium La1-xSr1-xCuGaO5 (xmax = 0,13). Messungen der magnetischen Suszeptibilität zeigen, daß die Verbindung bis zu 4 K paramagnetisch bleibt.
    Notes: The new brownmillerite-related compound, LaSrCuGaO5, has been synthesized and characterized. It crystallizes in the orthorhombic non-centrosymmetric space group Ima2. The unit cell dimensions are a = 16.383(1) Å, b = 5.5293(7) Å, c = 5.3275(6) Å. The structure is related to perovskite but contains ordered oxygen vacancies within the two-dimensional gallium oxygen layers resulting in tetrahedral coordination of the gallium cations. Other important structural features include buckled copper-oxygen planes, and disorder of the lanthanum and strontium cations over the A-site. Accurate lattice constant measurements reveal an a-axis expansion of 0.17 Å when doped with strontium La1-xSr1+xCuGaO5 (xmax = 0.13). Magnetic susceptibility measurements demonstrate that the compound remains paramagnetic to 4 K.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915980130
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    Darstellung und Struktur der Tetrafluoroaurate(III) MI[AuF4] mit MI = Li, RbProfessor Hans Georg von Schnering zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 598 (1991), S. 103-110 
    Details
    ISSN: 0044-2313
    Keywords: Lithium, rubidium tetrafluoroaurate(III) ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of Tetrafluoroaurates(III) MI[AuF4] with MI = Li, RbSingle crystal investigations on Rb[AuF4], light yellow, confirm the tetragonal unit cell (K[BrF4]-type) with a = 618.2(1) and c = 1191(1) pm, Z = 4, space group I 4/mcm-D4h18 (No. 140).Li[AuF4], light yellow too, crystallizes monoclinic with a = 485.32(7), b = 634.29(8), c = 1004.43(13) pm, β = 92.759(12), Z = 4; space group P 2/c-C2h4 (No. 13). The structure of Li[AuF4] is related to the Rb[AuF4]-type of structure.
    Notes: Einkristalluntersuchungen an Rb[AuF4], hellgelb, bestätigen die tetragonale Elementarzelle (K[BrF4]-Typ) mit a = 618,2(1) und c = 1191(1) pm, Z = 4, Raumgruppe I 4/mcm-D4h18 (Nr. 140).Ebenfalls hellgelbes Li[AuF4] hingegen kristallisiert monoklin (eigener Typ) in der Raumgruppe P 2/c-C2h4 (Nr. 13) mit a = 485,32(7), b = 634,29(8), c = 1004,43(13) pm, β = 92,759(12), Z = 4 und ist mit der Rb[AuF4]-Struktur verwandt.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915980110
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    Darstellung und Kristallstruktur von TICu[CuO2] (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 605 (1991), S. 157-162 
    Details
    ISSN: 0044-2313
    Keywords: TICu[CuO2] ; synthesis ; crystal structure ; lattice energy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of TlCu[CuO2]By reaction of Tl2O3 and Cu2O in a sealed copper-type TlCu[CuO2] was synthesized; the orthorhombically bodycentered crystallizing compound forms a new structure type, space group Imma (no. 74), with the lattice constants a = 552.5 pm, b = 605.2 pm, c = 896.4 pm. The Madelung Part of Lattice Energy, MAPLE, as well as Effective Coordination Numbers, ECoN, these via Mean Effective Ionic Radii, MEFIR, were calculated.
    Notes: Durch Umsetzung von Tl2O3 und Cu2O im verschweißten Kupfertiegel gelang die Darstellung von TlCu[CuO2]; die Verbindung kristallisiert orthorhombisch innenzentriert in einem neuen Strukturtyp, Raumgruppe Imma (Nr. 74), mit den Gitterkonstanten a = 552,5 pm, b = 605,2 pm, c = 896,4 pm. Der Madelunganteil der Gitterenergie, MAPLE, sowie Effektive Koordinationszahlen, ECoN, diese über Mittlere Effektive Ionenradien, MEFIR, wurden berechnet.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916050119
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    Synthese und Kristallstruktur von [Li(12-Krone-4)2][ReCl5(CH3CN)] · CH3CNHerrn Professor Joseph Grobe zum 60. Geburtstage am 2. November 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 606 (1991), S. 109-117 
    Details
    ISSN: 0044-2313
    Keywords: Pentachlorohenate(IV)-acetonitrile solvate ; synthesis ; IR spectrum ; 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 [Li(12-Crown-4)2][ReCl5(CH3CN)] · CH3CNThe title compound has been prepared by the reaction of lithium chloride with rhenium pentachloride in the presence of 12-crown-4 in acetonitrile solution.[Li(12-crown-4)2][ReCl5(CH3CN)] · CH3CN has been characterized by IR spectroscopy as well as by an X-ray structure determination. Space group P1, Z = 2, 4 450 observed unique reflections, R = 0.047, Lattice dimensions at 20°C: a = 1 445.8, b = 1 463.2, c = 1 580.2 pm, α = 89.28°, β = 114.19°, γ = 89.40°. The compound is ionic, the cation being formed by a lithium ion coordinated by the eight oxygen atoms of two crown ether molecules 12-crown-4 in sandwich fashion. In the anions [ReCl5(CH3CN)]- the rhenium atoms are in a distorted octahedral shape by the five chlorine atoms and by the N atom of the acetonitrile molecule. The two crystallographically independent cations and anions, respectively, are only slightly different.
    Notes: Die Titelverbindung wurde durch Reaktion von Lithiumchlorid mit Rheniumpentachlorid in Gegenwart von 12-Krone-4 in Acetonitrillösung hergestellt und durch ihr IR-Spektrum und durch eine röntgenographische Strukturanalyse charakterisiert.[Li(12-Krone-4)2][ReCl5(CH3CN)] · CH3CN kristallisiert triklin in der Raumgruppe P1 mit zwei Formeleinheiten pro Elementarzelle, 4 450 beobachtete unabhängige Reflexe, R = 4,7%. Gitterabmessungen bei 20°C: a = 1 445,8; b = 1 463,2; c = 1 580,2 pm; α = 89,28°; β = 114,19°; γ = 89,40°. Die Verbindung hat einen ionischen Aufbau, in dem die Lithiumionen sandwichartig von den acht Sauerstoffatomen zweier Kronenethermoleküle 12-Krone-4 koordiniert sind. In den Anionen [ReCl5(CH3CN)]- sind die Rheniumatome verzerrt oktaedrisch von den fünf Chloratomen und von dem N-Atom des Acetonitrilmoleküls umgeben. Die beiden kristallographisch unabhängigen Kationen bzw. Anionen unterscheiden sich nur wenig voneinander.
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    URL: http://dx.doi.org/10.1002/zaac.19916060112
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    LiSmAlF6  -  das erste Fluoroaluminat mit zweiwertigem Samarium (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 606 (1991), S. 169-176 
    Details
    ISSN: 0044-2313
    Keywords: Lithium samarium hexafluoroaluminate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: LiSmAlF6  -  the First Fluoroaluminate with Divalent SamariumLiSmAlF6, the first quaternary fluoride with Sm2+ that has been obtained as red transparent single crystals, is formed while heating corresponding mixtures of the starting materials in niobium or tantalum crucibles under argon after 7-10 d at about 800°C. Orange-red, microcrystalline powder samples of LiSmAlF6 could be prepared at T ≤ 700°C after 1-2 d under the same conditions.LiSmAlF6, crystallizes as a new structure type in P6322 (Nr. 182) with a = 507.9(1), c = 1 040.5(1) pm and Z = 2 (CAD4, 2 512 Io, Rw = 2,3%). The crystal structure of LiSmAlF6 is related to the LiCaAlF6 structure type whereby the essential difference lies in the coordination of the M2+ ions. Ca2+, as well as Sr2+ in LiSrAlF6, exhibit octahedral coordination, whereas Sm2+ has, surprisingly, trigonal prismatic coordination to F-. The two triangles of the SmF6 prism are twisted by 8.3° with respect to each other.Measurements of the magnetic susceptibility show the temperature dependence typically found for Sm2+. The Madelung part of the lattice energy has been calculated and is discussed.
    Notes: LiSmAlF6, das erste in Form roter, transparenter Einkristalle erhaltene quaternäre Fluorid mit Sm2+, bildet sich beim Erhitzen geeigneter Ausgangsmenge in Niob- oder Tantaltiegln unter Ar nach 7-10 d bei ca. 800°C. Orangerote, mikrokristalline Pulverproben von LiSmAlF6 können bei T ≤ 700°C bereits nach 1-2 Tagen unter sonst gleichen Bedingungen dargestellt werden.LiSmAlF6 kristallisiert in einem neuen Strukturtyp in P6322 (Nr. 182) mit a = 507,9(1), c = 1 040,5(1) pm und Z = 2(CAD4, 2 512 Io, Rw = 2,3%). Die Kristallstruktur von LiSmAlF6 ist dem LiCaAlF6-Typ verwandt, zeigt aber den wesentlichen Unterschied in der Umgebung für M2+ : Ca2+, wie auch Sr2+ in LiSrAlF6, werden oktaedrisch, Sm2+ jedoch überraschenderweise trigonal-prismatisch von F- koordiniert. Die beiden Dreiecke des SmF6-Prismas sind um 8,3° gegeneinander verdreht.Messungen der magnetischen Suszeptibilität zeigen die für Sm2+ typische Temperaturabhängigkeit. Der Madelunganteil der Gitterenergie wurde berechnet und diskutiert.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916060117
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    Molekül- und Kristallstrukturen des dimeren Strontium-bis[bis(trimethylsilyl)amids] und des Strontium-bis[bis(trimethylsilyl)amids] · 2DME (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 606 (1991), S. 177-190 
    Details
    ISSN: 0044-2313
    Keywords: Strontium bis[bis(trimethylsilyl)amide] ; strontium bis[bis(trimethylsilyl)amide] · 2DME ; preparation ; 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 the Dimeric Strontium Bis[bis(trimethylsilyl)amide] and Strontium Bis[bis(trimethylsilyl)amide] · 2DMEThe dimeric strontium bis[bis(trimethylsilyl)amide] 1 crystallizes from toluene in the triclinic space group P1 {a = 983,5(6); b = 1 238,1(7); c = 2 890(2) pm; α = 99,65(1)°; β = 91,67(1)°; γ = 96,03(2); Z = 3 dimers}. The characteristic moiety of this base-free strontium diamide is the planar, four-membered Sr2N2-ring with SrN-bond lenghts of 264 pm and a NSrN-angle of 84°. The bond distance between the strontium and the terminal, planar nitrogen atom is approximately 20 pm shorter. The strontium bis[bis(trimethylsilyl)amide] · 2DME 2 crystallizes in the monoclinic space group C2/c {a = 1 333,5(3); b = 1 715,0(3); c = 1 490,8(3) pm; β = 93,64(1)°; Z = 4}. This molecule includes the crystallographic C2-symmetry. The six-coordinate strontium shows bond distances to the nitrogen atoms of 254 pm and to the ether oxygen atoms of approximately 265 pm with a NSrN-angle of 136°.
    Notes: Das dimere Strontium-bis[bis(trimethylsilyl)amid] 1 kristallisiert aus Toluol in der triklinen Raumgruppe P1 {a = 983,5(6); b = 1 238,1(7); c = 2 890(2) pm; α = 99,65(1)°; β = 91,67(1)°; γ = 96,03(2); Z = 3 Dimere}. Das charakteristische Bauelement dieses basenfreien Strontium-diamids ist der planare, viergliedrige Sr2N2-Ring mit SrN-Bindungslängen von durchschnittlich 264 pm und einem NSrN-Winkel von 84°. Die Bindung vom Strontiumatom zum terminal gebundenen, planaren Stickstoffatom ist um 20 pm kürzer. Das Strontium-bis[bis(trimethylsily)amid] · 2DME 2 kristallisiert in der monoklinen Raumgruppe C2/c (a = 1 333,5(3); b = 1 715,0(3); c = 1 490,8(3) pm; β = 93,64(1)°; Z = 4). Die kristallographische C2-Achse verläuft durch das Molekül. Das sechsfach koordinierte Strontiumatom weist mittlere SrN- bzw. SrO-Bindungslängen von 254 bzw. 265 pm und einen NSrN-Winkel von 136° auf.
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    URL: http://dx.doi.org/10.1002/zaac.19916060118
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    Bis(dichlor-N-trimethylsily)cycloaminoalan Kristallstruktur und thermischer Abbau zu Aluminiumnitrid (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 603 (1991), S. 119-127 
    Details
    ISSN: 0044-2313
    Keywords: Dimeric aminoalane ; preparation ; crystal structure ; thermal decomposition ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Bis(dichloro-N-trimethylsilyl)cycloaminoalane - Crystal Structure and Thermal Decomposition to AluminiumnitrideThe dimeric aminoalane II, (me3SiNHAlCl2)2, is obtained in the reaction of aluminium trichloride and HN(Sime3)2. A crystal structure analysis and the pyrolysis with formation of AlN were carried out with II. The decomposition products were measured and characterized as a function of the temperature.
    Notes: Das dimere Aminoalan II, (me3SiNHAlCl2)2, entsteht in der Reaktion von Aluminiumtrichlorid und HN(Sime3)2. Von II wurde eine Kristallstrukturanalyse und eine Pyrolyse unter Bildung von AlN durchgeführt. Die Abspaltprodukte der Pyrolyse wurden temperaturabhängig gemessen und charakterisiert.
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    URL: http://dx.doi.org/10.1002/zaac.19916030116
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    Synthese und Strukturuntersuchungen von Ba2H[α-FeO4W12O36] · 26 H2O (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 594 (1991), S. 191-201 
    Details
    ISSN: 0044-2313
    Keywords: Dibarium-α-dodecawolframatoferrate(III)-26-hydrate ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure Studies of Ba2H[α-FeO4W12O36] · 26 H2OThe heteropolyanion compound Ba2H[α-FeO4W12O36] · 26 H2O (I) crystallizes in the tetragonal space group P4n2 with the lattice parameters a = 12.398(6), c = 18.721(6) Å; Z = 2; Dx = 4.128 g · cm-3. The structure was solved on a twinned crystal from 1029 observed reflections and refined to an index R of 7.6%. The calculations were done by means of a modified ORFLS-programme by Eitel and Bärnighausen. The heteropolyanion [α-FeO4W12O36]5- has the well known α-Keggin structure. The average distance of the four central oxygen atoms to the FeIII position (0, 0, 0) is 1.84 Å. The angles ∢ O—Fe—O are 112.3° (4X) and 103.9 (2X), respectively, which leads to an disphenoidal distortion of the FeO4 tetrahedron.The powder and single crystal ESR spectra of I show the anisotropy of the FeIII fine structure transition 1/2 ↔ -1/2. The Mößbauer spectra confirm the tetragonal distortion of the central FeO4 tetrahedron (quadrupole splitting Δ ≈ 0.50 mm · s-1).
    Notes: Die erstmalig in einkristalliner Form dargestellte Heteropolyanionenverbindung Dibarium-α-dodekawolframatoferrat(III)-26-Hydrat, Ba2H[α-FeO4W12O36] · 26 H2O (I), kristallisiert tetragonal mit den Gitterkonstanten a = 12,398(6), c = 18,721(6) Å; Z = 2; Dx = 4,128 g α cm-3. Für den vorliegenden Inversionszwilling mit einem Heteropolyanion vom α-Keggin-Typ wurde zur Verfeinerung der Kristallstruktur in der Raumgruppe P4n2 ein von Eitel und Bärnighausen modifiziertes ORFLS-Programm benutzt (R-Wert 7,6%). Der mittlere Abstand der vier zentralen Sauerstoffatome zur FeIII-Position (0, 0, 0) beträgt 1,84 Å. Die Winkel ∢ O—Fe—O weichen mit 112,3(4X) bzw. 103,9°(2X) deutlich von 109,5° ab, wodurch das Tetraeder zu einem tetragonalen Disphenoid verzerrt wird.Die Mößbauer-Spektren von I weisen eine deutliche Quadrupolaufspaltung von Δ; ≈ 0,50 mm · s-1 auf, die durch die Asymmetrie in der Umgebung von FeIII hervorgerufen wird. Damit in Übereinstimmung zeigen die EPR-Spektren sowohl für Pulver als auch für einen Einkristall von I ein Signal bei g ≃ 2, das im wesentlichen aus dem Feinstrukturübergang 1/2 ↔ - 1/2 des FeIII-Ions herrührt und eine deutliche Anisotropie aufweist.
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    URL: http://dx.doi.org/10.1002/zaac.19915940122
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    Neue Komplexe des Titans mit Bis(trimethylsilyl)amido-LigandenProfessor Kurt Dehnicke zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 595 (1991), S. 21-26 
    Details
    ISSN: 0044-2313
    Keywords: Titanium complex compounds ; cyclopentadienyl titanium bis(trimethylsilyl)amido compounds ; syntheses ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Complexes of Titanium with Bis(trimethylsilyl)amido LigandsThe reaction of cp′TiCl3 with LiN(SiMe3)2 · Et2O 1 yield the compounds cp′TiCl2N(SiMe3)2 (cp′ = C5H5 2, C5H4SiMe3 3, C5H3(SiMe3)2 4, C5Me5 5) and cp′TiCl[N(SiMe3)2]2 (cp′ = C5H5 6). Compound 2 was characterized by an X-ray structural analysis with space group P21/n and unit cell dimensions of a = 1 660.9(7), b = 688.6(3), c = 1 739.1(8) pm and β = 117.18(3)°.
    Notes: Die Reaktion von cp′TiCl3 mit LiN(SiMe3)2 · Et2O 1 führt zu den Verbindungen cp′TiCl2N(SiMe3)2 (cp′ = C5H5 2, C5H4SiMe3 3, C5H3(SiMe3)2 4, C5Me5 5) und cp′TiCl[N(SiMe3)2]2 (cp′ = C5H5 6). Verbindung 2 wurde durch eine Einkristall Röntgenstrukturanalyse charakterisiert. 2 kristallisiert in der Raumgruppe P21/n mit a = 1 660,9(7), b = 688,6(3), c = 1 739,1(8) pm und β = 117,18(3)°.
    Additional Material: 1 Ill.
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    Zur Reaktion von [Cp2TiCl]2 und TiCl4 mit LiE(SiMe3)2 (E = P, As) und P(SiMe3)3 Die Kristallstrukturen von [Cp2TiP(SiMe3)2], [(Cp2Ti)2ClAs(SiMe3)2] und [TiCl3 {P(SiMe3)3}2]Professor Kurt Dehnicke zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 595 (1991), S. 57-66 
    Details
    ISSN: 0044-2313
    Keywords: Dicyclopentadienyl [bis(trimethylsilyl)phosphanido]titanium, [Cp2TiP(SiMe3)2] ; μ-chloro-μ-bis(trimethylsilyl)arsanido-bis(dicyclopentadienyl)titanium, [(Cp2Ti)2ClAs(SiMe3)2] ; trichloro-bis[tris(trimethylsilyl)phosphane]titanium, [TiCl3{P(SiMe3)3}2] ; syntheses ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of [CpTiCl]2 and TiCl4 with LiE(SiMe3)2 (E = P, As) and P(SiMe3)3. The Crystal Structures of [Cp2TiP(SiMe3)2], [(Cp2Ti)2ClAs(SiMe3)2], and [TiCl3 {P(SiMe3)3}2][Cp2TiCl]2 reacts with LiP(SiMe3)2 to form the mono nuclear complex [Cp2TiP(SiMe3)2] (3). 3 has been characterized by X-ray crystal structure analysis. 3 is paramagnetic and Ti is coordinated by two Cp ligands and a P(SiMe3)2 group. The geometry about the phosphorus atom is nearly trigonal planar. As a result of π-interactions one can find a short Ti—P bond length of about 246.7 pm. In contrast to the formation of 3, the reaction of [Cp2TiCl]2 with LiAs(SiMe3)2 yields the dinuclear Ti complex [(Cp2Ti)2ClAs(SiMe3)2] (4). TiCl4 and P(SiMe3)3 react to from the complex [TiCl3{P(SiMe3)3}2] (2). The Ti atom in 2 is coordinated to three Cl1- and two P(SiMe3)3 ligands.
    Notes: [Cp2TiCl]2 reagiert mit LiP(SiMe3)2 zu dem einkernigen Komplex [Cp2TiP(SiMe3)2] (3). Die Struktur des paramagnetischen 3 konnte mit Hilfe einer Kristallstrukturanalyse aufgeklärt werden. Danach wird das Titanatom von 2 Cp-Liganden und einer P(SiMe3)2-Gruppe koordiniert. Die an P gebundenen Atome liegen dabei in einer Ebene mit dem P-Atom. Als ein Ergebnis der π-Wechselwirkung zwischen Ti und P beobachtet man eine kurze Ti—P-Bindungslänge von 246,7 pm. Dagegen reagiert [Cp2TiCl]2 mit LiAs(SiMe3)2 zu dem zweikernigen Komplex [(Cp2Ti)2ClAs(SiMe3)2] (4). Setzt man TiCl4 mit P(SiMe3)3 um, erhält man weiße Kristalle der Zusammensetzung [TiCl3 {P(SiMe3)3}2] (2). In 2 ist Ti trigonal bipyramidal an die Cl1-- und P(SiMe3)3-Liganden gebunden.
    Additional Material: 3 Ill.
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    [Rb2(H2O)2][Re3(μ-Cl)3Br7(H2O)2]2 · H2O, ein gemischtes Halogenid-Hydrat mit anionischen Dimeren {[Re3(μ-Cl)3Br7(H2O)2]2 · H2O}2-Professor Kurt Dehnicke zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 595 (1991), S. 131-137 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium ; rubidium rhenium halide hydrates ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Rb2(H2O)2][Re3(μ-Cl)3Br7(H2O)2]2 · H2O, a Mixed Halide-Hydrate with the Anionic Dimer {[Re3(μ-Cl)3Br7(H2O)2]2 · H2O}2-[Rb2(H2O)2][Re3(μ-Cl)3Br7(H2O)2]2 · H2O crystallizes as dark redbrown single crystals from an hydrobromic-acid solution of ReCl3 and RbBr at 0°C. An important feature of the crystal structure (monoclinic, C2/c; a = 1494.61(8); b = 835.71(4); c = 3079.96(19) pm; β = 97.801(4)°; Vm = 573.9(4) cm3mol-1; R = 0.060; Rw = 0.038) is the connection of two anions [Re3(μ-Cl)3Br7(H2O)2]- via a water molecule to dimers, {[Re3(μ-Cl)3Br7(H2O)2]2 · H2O}2-. These dimeric units are contained in slabs that are stacked in the [001] direction and held together by Rb+ cations and crystal water.
    Notes: [Rb2(H2O)2][Re3(μ-Cl)3Br7(H2O)2]2 · H2O kristallisiert in dunklen, rotbraunen Einkristallen aus bromwasserstoffsaurer Lösung von Rheniumtrichlorid und Rubidiumbromid bei 0°C. Ein wichtiges Merkmal der Kristallstruktur (monoklin; C2/c; a = 1494,61(8); b = 835,71(4); c = 3079,96(19) pm; β = 97,801(4)°; Vm = 573,9(4) cm3mol-1; R = 0,060; Rw = 0,038) ist die Verknüpfung zweier Anionen [Re3(μ-Cl)3Br7(H2O)2]- über ein Wassermolekül zu Dimeren {[Re3(μ-Cl)3Br7(H2O)2]2 · H2O}2-. Diese dimeren Baugruppen sind zu Schichtpaketen zusammengefaßt, die längs [001] gestapelt und über die Rb+-Ionen in Gemeinsamkeit mit Kristallwasser verbunden sind.
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    Strukturen caesiumhaltiger Fluoride. IX. CsCu2F5, eine Verbindung mit den Koordinationszahlen 4, 5 und 6 für Kupfer(II)Professor Kurt Dehnicke zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 595 (1991), S. 139-149 
    Details
    ISSN: 0044-2313
    Keywords: Cesium copper(II) fluoride, CsCu2F5 ; crystal structure ; magnetism ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structure of Cesium-containing Fluorides. IX. CsCu2F5, a Compound exhibiting Coordination Numbers 4, 5, and 6 for Copper(II)Single crystals of the monoclinic compound CsCu2F5 (a = 713.5, b = 738.6, c = 950.2 pm, β = 97.19°; P21/n, Z = 4) were prepared and their structure determined by X-ray methods (wR = 0.045 for 2140 independent reflections). Besides of square planar and elongated octahedral [CuFn] units (average Cu—F = 190.3 resp. 195.0/221.9 pm), the structure exhibits the first example of [CuF5] coordination, which is a distorted square pyramide (Cu—F = 190.7/221.6 pm). Relations to the pyrochlore structure are discussed, as well as the linking of polyhedra and the bridge angles Cu—F—Cu in context with the antiferromagnetic properties (TN = 54 K), which were found by powder susceptibility measurements.
    Notes: Einkristalle der monoklinen Verbindung CsCu2F5 (a = 713,5, b = 738,6, c = 950,2 pm, β = 97,19°; P21/n, Z = 4) wurden dargestellt und ihre Struktur röntgenographisch bestimmt (wR = 0,045 für 2140 unabhängige Reflexe). Neben quadratisch planaren und gestreckt oktaedrischen [CuFn]-Baugruppen (Mittelwerte Cu—F = 190,3 bzw. 195,0/221,9 pm) zeigt die Struktur das erste Beispiel einer [CuF5]-Koordination in Form einer verzerrten quadratischen Pyramide (Cu—F = 190,7/221,6 pm). Beziehungen zur Pyrochlorstruktur werden diskutiert, sowie die Vernetzung der Polyeder und die Brückenwinkel Cu—F—Cu im Zusammenhang mit den antiferromagnetischen Eigenschaften (TN = 54 K), die durch Suszeptibilitätsmessungen an Pulvern ermittelt wurden.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915950114
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    Kristallstruktur einer neuen Modifikation von Sb8F30 (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 605 (1991), S. 109-116 
    Details
    ISSN: 0044-2313
    Keywords: Antimony(III)fluoride,(Sb2F5+)(Sb3F72+)(SbF6-)3 ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of a new Modification of Sb8F30The modification of Sb8F30, described here, crystallizes in the orthorhombic space group Pca21 (No. 29) with a = 1115.7(1), b = 1100.2(1), c = 1917.8(3) pm and Z = 4. Within this complex molecule, the Sb3F72+-cation was identified besides a heavily distorted form of the mixed valent Sb4F17--anion.
    Notes: Die hier beschriebene Modifikation von Sb8F30 kristallisiert in der orthorhombischen Raumgruppe Pca21 (Nr. 29) mit a = 1115,7(1), b = 1100,2(1), c = 1917,8(3) pm und Z = 4. Innerhalb dieses komplexen Moleküls werden ein Sb3F72+-Kation und eine stark verzerrte Form des gemischt valenten Sb4F17--Anions identifiziert.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916050112
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    Die Kristallstruktur der geordneten Phase der Verbindung TlSbSe2 (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 606 (1991), S. 51-58 
    Details
    ISSN: 0044-2313
    Keywords: Thallium antimony selenide ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of the Ordered Phase of the Compound TlSbSe2Single crystals of the RT-phase of the compound TlSbSe2, which are stable at room temperature, were prepared by sublimation at 350°C. The crystals are monoclinic, space group P21 (No. 4), a = 9.137(1) Å, b = 4.097(1) Å, c = 12.765(2) Å, β = 111.75(1)°, Z = 4. Contrary to the high temperature (HT) phase the cation distribution of the RT-phase is strongly ordered. The lattice forms a layer structure parallel (001), where the Sb atoms have a (3 + 2) and the Tl atoms a (1 + 4) coordination of Se atoms within the layer. The crystal structure of the RT-phase of the compound TlSbSe2 can be described as a superstructure of the HT-phase. The order of the superstructure and a model of the twinning are discussed.
    Notes: Einkristalle der bei Raumtemperatur stabilen (RT) Phase der Verbindung TlSbSe2 wurden durch Sublimation bei 350°C erhalten. Die Kristalle sind monoklin, Raumgruppe P21 (No. 4), a = 9,137(1) Å, b = 4,097(1) Å, c = 12,765(2) Å, β = 111,75(1)°, Z = 4. Im Gegensatz zu der Hochtemperaturphase (HT) weist die RT-Phase eine streng geordnete Kationenverteilung auf. Das Kristallgitter bildet eine Schichtstruktur parallel (001), bei der die Sb-Atome von (3 + 2), die Tl von (1 + 4) Se-Atomen innerhalb einer Schicht koordiniert sind. Die Kristallstruktur der RT-Phase der Verbindung TlSbSe2 kann als Überstruktur der HT-Phase beschrieben werden. Die Überstrukturordnung und ein Modell der Verzwillingung werden diskutiert.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916060105
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    [Li(12-Krone-4)]Cl: Kristallstruktur und IR-Spektrum (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 606 (1991), S. 91-96 
    Details
    ISSN: 0044-2313
    Keywords: Lithium chloride crown ether complex ; I.R. spectrum ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Li(12-Crown-4)]Cl: Crystal Structure and I.R. SpectrumColourless single crystals of [Li(12-crown-4)]Cl were obtained from acetonitrile solutions of LiCl in the presence of 12-crown-4. They were characterized by i. r. spectroscopy as well as by an X-ray structure determination. Space group P4/n, Z = 2, 1 080 observed unique reflections, R = 0.034. Lattice dimensions at -50°C; a = 837.8(5), c = 752.0(2) pm. [Li(12-crown-4)]Cl forms ion pairs with tetragonal symmetry and bond lengths Li—O of 212.8 pm and Li—Cl of 229.0 pm.
    Notes: [Li(12-Krone-4)]Cl wurde aus LiCl-Lösungen in Acetonitril in Gegenwart von 12-Krone-4 in farblosen Einkristallen erhalten, die durch das IR-Spektrum und eine röntgenographische Strukturanalyse charakterisiert werden. Raumgruppe P4/n, Z = 2, 1080 beobachtete unabhängige Reflexe, R = 3,4%. Gitterabmessungen bei -50°C: a = 837,8(5), c = 752,0(2) pm. [Li(12-Krone-4)]Cl bildet Ionenpaare mit tetragonaler Symmetrie und Abständen Li—O von 212,8 pm und Li—Cl von 229,0 pm.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916060109
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    Fe(OTeF5)3, Darstellung, Struktur und Reaktivität (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 606 (1991), S. 201-207 
    Details
    ISSN: 0044-2313
    Keywords: Iron tris(pentafluorooxotellurate(VI)) ; trigonal planar iron ; preparation ; crystal structure ; nonachloriditellurate (IV) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Fe(OTeF5)3, Preparation, Structure, and ReactivityFeCl3 reacts with ClOTeF5 under formation of Fe(OTeF5)3. From SO2ClF solutions an adduct Fe(OTeF5)3 · 3SO2ClF can be crystallized. This has a distorted octahedral iron oxygen co-ordination. The solvate-free compound is trigonal-planar, according to its Mößbauer spectrum. It has an extreme reactivity towards bases. Only alkanes and perfluoro-alkanes remain unaffected. Attempts to coordinate P(OC2H5)3 in SO2ClF solution result in a complex reaction under formation of [P(OC2H5)4]+ [Te2Cl9]- and iron fluoride(s).
    Notes: FeCl3 reagiert mit ClOTeF5 unter Bildung von Fe(OTeF5)3. Aus der Lösung in SO2ClF kristallisiert ein Addukt Fe(OTeF5)3 · 3SO2ClF mit verzerrt oktaedrischer Eisen-Sauerstoff-Koordination. Die solvatfreie Verbindung ist nach Mößbauermessungen anscheinend trigonal planar aufgebaut und zeigt ein extremes Reaktionsverhalten gegenüber Basen: Nur Alkane und Perfluoralkane werden nicht angegriffen. Versuche zur Komplexierung der freien Koordinationsstellen z. B. mittels P(OC2H5)3 in SO2ClF-Lösung ergaben in komplexer Reaktion [P(OC2H5)4]+[Te2Cl9]- und Eisenfluorid.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916060120
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    Über die Kristallstruktur von Barium-Acetylendicarboxylat Monohydrat - Ba[C2(COO)2] · H2O (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 149-155 
    Details
    ISSN: 0044-2313
    Keywords: Barium acetylenedicarboxylate monohydrate ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Crystal Structure of Barium Acetylene Dicarboxylate Monohydrate - Ba[C2(COO)2] · H2OBa[C2(COO)2] · H2O crystallizes in the monoclinic space group P21/a. The lattice constants are a = 753.4(2), b = 921.8(2), c = 881.8(2) pm and β = 102.00(2)°. The crystal structure is characterized by an intricate three-dimensional framework made up by Ba2+ and [C2(COO)2]2- ions. Ba2+ has coordination number 9 and is bound to two water molecules and seven oxygen atoms belonging to carboxylate groups of the dianion. The [C2(COO)2]2- ion does not merely act like a multiple monodentate ligand, but coordinates Ba2+ in a chelate-like manner as well. The carboxylate groups of the dianion are inclined to each other by 65°.
    Notes: Ba[(C2(COO)2)2] · H2O kristallisiert in der monoklinen Raumgruppe P21/a mit den Gitterkonstanten a = 753,4(2), b = 921,8(2), c = 881,8(2) pm und β = 102,00(2)°. Es liegt ein kompliziert gebautes dreidimensionales Gerüst aus Ba2+- und [C2(COO)2]2--Ionen vor. Ba2+ besitzt Koordinationszahl 9 und ist von zwei Wassermolekülen und sieben Sauerstoffatomen aus den Dianionen umgeben. Das [C2(COO)2]2--Ion wirkt nicht nur als mehrfach einzähniger Ligand, sondern bindet Ba2+ mit einer Carboxylatgruppe auch chelatartig. Die Carboxylatgruppen des Dianions sind um etwa 65° gegeneinander verdreht.
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    NaHg: A variant of the cesiumchloride structure structural relations and electronic structureProfessor Hanskarl Müller-Buschbaum zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 41-50 
    Details
    ISSN: 0044-2313
    Keywords: Sodium mercury compound ; mercury cluster unit ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: NaHg: Eine Variante der Caesiumchloridstruktur. Strukturelle Beziehungen und elektronische StrukturDie bereits früher untersuchte Kristallstruktur des gold-bronzefarbenen NaHg ist gekennzeichnet durch nahezu quadratische Hg4-Gruppen, die über gemeinsame Kanten zu Zickzack-Ketten kondensiert sind. Die bislang unbemerkte Beziehung der orthorhombischen Realstruktur von NaHg zum Caesiumchloridtyp (B2) wird diskutiert. Außerdem werden die elektronischen Strukturen sowohl für die hypothetische B2-als auch für die orthorhombische Realstruktur mittels des relativistischen LMTO-Verfahrens berechnet. Dabei zeigt sich eine klare Tendenz zur Population der im Grundzustand des freien Atoms leeren 6 p-Zustände am Quecksilber. Diese Auffüllung liefert, in Übereinstimmung mit der intuitiven chemischen Vorstellung, wonach ein partieller Elektronenübertrag vom elektropositiven Natrium auf das Quecksilber stattfinden sollte, den entscheidenden Beitrag zur chemischen Bindung zwischen den Quecksilberatomen.
    Notes: The crystal structure of the gold-bronce coloured, metallic NaHg, which was already determined earlier, is characterized by nearly square planar Hg4 clusters condensed to zig-zag chains via common edges. We discuss the hitherto unknown relation of the orthorhombic NaHg structure to the CsCl type (B2). and present calculations of the electronic structures for the hypothetical B2 structure as well as for the real orthorhombic structure by means of the relativistic LMTO method. A clear tendency is observed towards a population of the mercury 6 p-states, which are empty in the free atom in its ground state. This population is the most important contribution to the bonding between the mercury atoms in the cluster chains. Thus the simple chemical picture, whereafter a partial electron transfer should take place from the electropositive sodium to mercury, is in accordance with the calculation results.
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    Zweikernige Aniongruppen [Fe2F10]4- in der Kristallstruktur von Sr5Fe3F19Professor Hanskarl Müller-Buschbaum zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 51-59 
    Details
    ISSN: 0044-2313
    Keywords: Pentastrontium-trifluoride-{di-μ-fluoro-bis[tetrafluoroferrate(III)]}-hemafluoroferrate(III), Sr5F3[Fe2F10][FeF6] ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Dinuclear Anion Groups [Fe2F10]4- in the Crystal Structure of Sr5Fe3F19At single crystals of Sr5Fe3F19 a X-ray structure determination in the tetragonal space group 14/m was performed (a = 1429.4(3), c = 730.7(3) pm; Z = 4. wR = 0.019 for 502 independent reflections). Within the structure there are isolated, but disordered dimeric anion groups of edge-sharing octahedra [Fe2F10]4- (average Fe—F = 193.3 pm, Fe—Fe = 319.1 pm). They are embedded in a framework of strontium ions (C.N. 8-10) and single FeF63- octahedra (Fe—F = 191.0 resp. 192.7 pm, if corrected for thermal motion). The strong relations to the crystal structure of BaTiF5 and to further related fluoride compounds are discussed.
    Notes: An Einkristallen von Sr5Fe3F19 wurde eine röntgenographische Strukturbestimmung in der tetragonalen Raumgruppe 14/m durchgeführt (a = 1429,4(3), c = 730,7(3) pm; Z = 4. wR = 0,019 für 502 unabhängige Reflexe). In der Struktur treten isolierte, aber fehlgeordnete dimere Aniongruppen kantenverknüpfter Oktaeder [Fe2F10]4- auf (Mittelwert Fe—F = 193,3 pm, Fe—Fe = 319,1 pm). Sie sind eingebettet in ein Gerüst von Strontiumionen (KZ 8-10) und FeF63--Einzeloktaedern (Fe—F = 191,0 bzw. 192,7 pm, wenn für die thermische Schwingung korrigiert wird). Die engen Beziehungen zur Kristallstruktur von BaTiF5 und zu weiteren verwandten Fluorverbindungen werden diskutiert.
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    URL: http://dx.doi.org/10.1002/zaac.19915970108
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    Ungewöhnliche H-Brückenbindungen in Natriumhydroxidmonohydrat: Röntgen- und Neutronenbeugung an NaOH · H2O bzw. NaOD · D2OProfessor Hanskarl Müller-Buschbaum zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 97-106 
    Details
    ISSN: 0044-2313
    Keywords: Sodium hydroxide monohydrate ; monodeuterate ; crystal structure ; neutron diffraction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Unusual H-Bonds in Sodium Hydroxide Monohydrate: X-Ray and Neutron Diffraction on NaOH · H2O and NaOD · D2O, respectivelyX-ray data revealed the structure of NaOH · H2O including the H positions. Neutron diffraction on microcrystalline NaOD · D2O was used for comparison of H with D positions: \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{l}{\rm NaOH} \cdot {\rm H}_2 {\rm O}:{\rm Pbca},\,{\rm Z} = 8,\,{\rm a} = 11.825(2){\rm {\AA}},\,{\rm b} = 6.213(2){\rm {\AA}},\,{\rm c} = 6.069(2){\rm {\AA}}\\{\rm Z}({\rm F}_\circ)\,{\rm mit}\,({\rm F}_\circ)^2 \ge 1{\rm \sigma}({\rm F}_\circ)^2 = 635,\,{\rm Z}\,({\rm Parameter}) = 40,\,{\rm R}/{\rm R}_{\rm w} = 0.022/0.024\\{\rm NaOD} \cdot {\rm D}_2 {\rm O}:{\rm \lambda} = 2.016{\rm {\AA}},\,10^\circ \le 2\Theta \le 86^\circ,\,{\rm R} = 0.049\,({\rm nur}\,{\rm D - Lagen variiert})\\\end{array} $$\end{document}The compound crystallizes in a layer-type structure with the sequence … /O Na O O Na O/ … closely related to that of hydrargillite Al(OH)3 with … /O 2/3 Al O O 2/3 Al O/ …. Between OH- ions as acceptors and H2O molecules mäandric, one-dimensional infinite strong H-bonds occur with d(O…O) = 2.66 Å and 2.69 Å. These lie within O-layers that coordinate Na+ ions. Bridge-bonds between OH- ions as donors and H2O molecules as acceptors connect the /O Na O/-layers with d(O…O) = 3.18 Å.
    Notes: An NaOH · H2O wurde röntgenographisch die Atomanordnung einschließlich der H-Lagen bestimmt und Neutronenbeugungsmessungen an feinkristallinem NaOD · D2O vergleichend ausgewertet: \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{l}{\rm NaOH} \cdot {\rm H}_2 {\rm O}:{\rm Pbca},\,{\rm Z} = 8,\,{\rm a} = 11,825(2){\rm {\AA}},\,{\rm b} = 6,213(2){\rm {\AA}},\,{\rm c} = 6,069(2){\rm {\AA}}\\{\rm Z}({\rm F}_\circ)\,{\rm mit}\,({\rm F}_\circ)^2 \ge 1{\rm \sigma}({\rm F}_\circ)^2 = 635,\,{\rm Z}\,({\rm Parameter}) = 40,\,{\rm R}/{\rm R}_{\rm w} = 0,022/0,024\\{\rm NaOD} \cdot {\rm D}_2 {\rm O}:{\rm \lambda} = 2,016{\rm {\AA}},\,10^\circ \le 2\Theta \le 86^\circ,\,{\rm R} = 0,049\,({\rm nur}\,{\rm D - Lagen variiert})\\\end{array} $$\end{document}Die Verbindung kristallisiert in einer Schichtstruktur der Abfolge … /O Na O O Na O/ … verwandt zu der von Hydrargillit, Al(OH)3 mit … /O 2/3 Al O O 2/3 Al O/ …. Zwischen Hydroxidionen als Akzeptoren und H2O-Molekülen treten mäanderförmig eindimensional unendliche starke H-Brücken auf mit d(O…O) = 2,66 Å und 2,69 Å. Diese liegen in O-Schichten, die Na+-Ionen koordinieren. Weitere Brückenbindungen zwischen OH--Ionen als Donatoren und H2O-Molekülen als Akzeptoren verknüpfen die /O Na O/-Schichtpakete mit d(O…O) = 3,18 Å.
    Additional Material: 5 Ill.
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    AgPbOBr  -  ein neuer Sillén-Typ? Darstellung und KristallstrukturProfessor Hanskarl Müller-Buschbaum zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 151-161 
    Details
    ISSN: 0044-2313
    Keywords: Silver lead oxybromide ; crystal structure ; layer structure ; crystal chemistry ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: AgPbOBr  -  a New Sillén Type? Preparation and Crystal StructureAgPbOBr was prepared for the first time. Its crystal structure was explored by single crystal X-ray diffraction. AgPbOBr crystallizes with tetragonal symmetry in space group P 4/nmm - No. 129 with a = 3.891(1) Å, c = 11.07(1) Å and two formulas per unit cell. Least squares refinement yields an weighted R-value of 0.065. AgPbOBr shows a layered structure with components of the crystal structure of red PbO as well as AgBr. Emphasized differences between the crystal structures of AgPbOBr and the X2-types after Sillén's notation [1] are characteristic. AgPbOBr is the first member of a new structure type, arranged between Sillén- and Aurivilliusphases [2].
    Notes: AgPbOBr wurde erstmalig dargestellt und die Kristallstruktur an Einkristallen aufgeklärt. Es kristallisiert tetragonal (Raumgruppe P4/nmm  -  No. 129) mit a = 3,891(1) Å, c = 11,07(1) Å und z = 2. Die Verfeinerung (LSQ) der Einkristallmessung liefert Rw = 0,065. AgPbOBr ist schichtförmig aufgebaut mit aus PbO und AgBr bestehenden Bereichen, die nahezu unverändert dem Bau von PbO und AgBr gleichen. Die Unterschiede zur Kristallstruktur der Sillén-Phasen vom X2-Typ [1] sind charakteristisch. AgPbOBr nimmt kristallchemisch eine Stellung zwischen den Sillén- und den Aurivillius-Phasen [2] (z. B. BiOCl und γ-Bi2 WO6) ein.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915970118
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    Ternäre Nickelphosphide und -arsenide mit einem Metall: Nichtmetall-Verhältnis von 2:1Professor Hanskarl Müller-Buschbaum zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 173-182 
    Details
    ISSN: 0044-2313
    Keywords: (strontium, europium, barium, uranium) nickel phosphides ; arsenides ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ternary Phosphides and Arsenides of Nickel with a Metal: Non-Metal Ratio of 2:1Several new ternary phosphides and arsenides of nickel were prepared by reaction of the elements. SrNi5P3, SrNi5As3, and EuNi5As3 crystallize in the LaCo5P3 structure with the following lattice constants [Å]: \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{*{20}c}{} \hfill & {\rm a} \hfill & {\rm b} \hfill & {\rm c} \hfill\\{{\rm SrNi}_{\rm 5} {\rm P}_3 :} \hfill & {3.618(1)} \hfill & {11.789(2)} \hfill & {11.597(2)} \hfill\\{{\rm SrNi}_5 {\rm As}_3 :} \hfill & {3.759(1)} \hfill & {12.239(2)} \hfill & {11.890(2)} \hfill\\{{\rm EuNi}_{\rm 5} {\rm As}_3 :} \hfill & {3.742(1)} \hfill & {12.215(2)} \hfill & {11.839(2)} \hfill\\\end{array} $$\end{document}BaNi9P5 (a = 6.534(1) Å, c = 10.847(2) Å) and BaNi9As5 (a = 6.760(1) Å, c = 11.226(2) Å) crystallize in a new type of structure (P63/mmc, Z = 2). The characteristic polyhedra are trigonal Ni-antiprisms centered by P or As atoms and trigonal Ni-prisms with vacant centres and sides capped by non-metal atoms. U2Ni12P7 (a = 9.077(2) Å, c = 3.694(1) Å) has a Zr2Fe12P7 structure (P6, Z = 1).
    Notes: Durch Erhitzen der jeweiligen Elemente konnten einige neue ternäre Nickelphosphide und -arsenide dargestellt werden. SrNi5P3, SrNi5As3 und EuNi5As3 kristallisieren im LaCo5P3-Typ (Cmcm, Z = 4) mit folgenden Gitterkonstanten [Å]: \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{*{20}c}{} \hfill & {\rm a} \hfill & {\rm b} \hfill & {\rm c} \hfill\\{{\rm SrNi}_{\rm 5} {\rm P}_3 :} \hfill & {3,618(1)} \hfill & {11,789(2)} \hfill & {11,597(2)} \hfill\\{{\rm SrNi}_5 {\rm As}_3 :} \hfill & {3,759(1)} \hfill & {12,239(2)} \hfill & {11,890(2)} \hfill\\{{\rm EuNi}_{\rm 5} {\rm As}_3 :} \hfill & {3,742(1)} \hfill & {12,215(2)} \hfill & {11,839(2)} \hfill\\\end{array} $$\end{document}BaNi9P5 (a = 6,534(1) Å, c = 10,847(2) Å) und BaNi9As5 (a = 6,760(1) Å, c = 11,226(2) Å) bilden einen neuen Strukturtyp (P63/mmc, Z = 2), bei dem trigonale Ni-Antiprismen mit je einem P-bzw. As-Atom in der Mitte sowie allseitig überdachte trigonale Ni-Prismen mit unbesetzten Zentren strukturbestimmend sind. U2Ni12P7 (a = 9,077(2) Å, c = 3,694(1) Å) kristallisiert in der Zr2Fe12P7-Struktur (P6, Z = 1).
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915970120
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    Ein neuer Strukturtyp der Oxovanadate MV2O6: NiV2O6 (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 23-28 
    Details
    ISSN: 0044-2313
    Keywords: Nickel ; vanadium ; oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A New Structure of Oxovanadates MV2O6 : NiV2O6Single crystals of NiV2O6 were prepared by solid state reactions below the melting point of the compound. It crystallizes with triclinic symmetry, space group Ci1 - P1; a = 7.128; b = 8.820; c = 4.793 Å; α = 90.24; β = 94.10 und γ = 102.15°; Z = 3. Ni2+ and two of the three vanadium point positions show an octahedral surrounding by O2- ions. The third V5+ position is tetrahedrally coordinated. The crystal structure will be shown and discussed.
    Notes: Einkristalle von NiV2O6 wurden mit Feststoffreaktionen nahe am Schmelzpunkt dieser Verbindung dargestellt. Mit Röntgen-Einkristalltechnik wurde die Struktur aufgeklärt. NiV2O6 kristallisiert triklin, Raumgruppe Ci1 - P1 mit a = 7,128; b = 8,820; c = 4,793 Å; α = 90,24; β = 94,10 und γ = 102,15° Z = 3. Ni2+ und zwei der drei Vanadiumpunktlagen sind oktaedrisch von O2- koordiniert. Die dritte V5+-Punktlage zeigt tetraedrische Koordination. Die Kristallstruktur wird vorgestellt und diskutiert.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915960104
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    Der Ba3In2O6-Typ mit Sc3+ In tetragonal pyramidaler Koordination Zur Kenntnis von BaSr2ScInO6 (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 29-33 
    Details
    ISSN: 0044-2313
    Keywords: Alkaline earth ; indium ; oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Ba3In2O6-Type with Sc3+ in Square Pyramidal Coordination. About BaSr2ScInO6Single crystals of BaSr2ScInO6 were prepared by CO2 laser technique. X-ray investigations show tetragonal symmetry: space group D4h17-I4/mmm; a = 4.1020; c = 20.685 Å; Z = 2. It is isotypic to Ba3In2O6 and the phases Ln2-xSr1+xCu2O6-x/2, respectively. In3+ and Sc3+ are in statistically distribution and coordinated by square pyramids of oxygen.
    Notes: Mit CO2-Laser-Technik wurden Einkristalle von BaSr2ScInO6 dargestellt. Röntgenuntersuchungen führen zu tetragonaler Symmetrie: Raumgruppe D4h17 - I4/mmm; a = 4,1020; c = 20,685 Å; Z = 2. BaSr2ScInO6 ist mit Ba3In2O6 bzw. den Phasen Ln2-xSr1+xCu2O6-x/2 isotyp. In3+ und Sc3+ sind statistisch verteilt und werden von Sauerstoff tetragonal pyramidal koordiniert.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915960105
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    2-Pyridinamin-Addukte von Übergangsmetall-bis(acetyl-acetonaten) und ihre Reaktionen. Hydrogencarbonat als Chelatligand in cis-(Ampy)2Co(acac)(HCO3)Professor Hans-Georg von Schnering zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 598 (1991), S. 71-82 
    Details
    ISSN: 0044-2313
    Keywords: Cobalt (nickel) complexes ; bis(2-pyridinamine) adducts of MII bis(acetylacetonate) ; carbonate ; acetylacetonate hydrogencarbonate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 2-Pyridinamine Adducts of Transition Metal Bis(acetylacetonates) and their Reactions. Hydrogencarbonate as a Chelating Ligand in cis-(Ampy)2Co(acac)(HCO3)The reaction of cobalt(II) salts, acetylacetone (acacH), 2-pyridinamine (Ampy), and the carbon dioxide of the air in methanol affords a mixture of (Ampy)2Co(acac)2(II) and (Ampy)2Co(CO3)(H2O)2. On heating in toluene, appropriately in the presence of carbon dioxide, these complexes are converted into cis-(Ampy)2Co(acac)(HCO3) (III). Characteristic of compound III is a four-membered ring with the hydrogencarbonate as a bidentate ligand. The two Co—O distances are distinctly different (215.9 and 224.4 pm).In the complexes II and III 2-pyridinamine is a bidentate ligand coordinating by the endo-nitrogen. The Co-n-N bond lengths vary between 210.9 and 225.3 pm. Reasons are both the different trans-influence of the hydrogencarbonate or the acetylacetonato donor atoms and the π-interaction between cobalt(II) and the pyridine ring. This interaction is more significant in the cis-complex III. II and III are stabilized by a system of N—H … O- and O—H …O-bridges.With nickel(II) complexes analogous to II and III were obtained, while only the type II was characterized for manganese(II).
    Notes: Die Umsetzung von Cobalt(II)-Salzen mit Acetylaceton (acacH), 2-Pyridinamin (Ampy) und dem Kohlendioxid der Luft in Methanol gibt ein Gemisch von trans-(ampy)2Co(acac)2(II) und (Ampy)2Co(CO3)(H2O)2. Beim Erhitzen in Toluen, zweckmäßigerweise unter Durchleiten von Kohlendioxid, setzen sich diese Komplexe zu cis-(Ampy)2Co(acac)(HCO3)(III) um.Für III ist ein viergliedriger Chelatring mit dem Hydrogencarbonat als zweizähligem Liganden charakteristisch, die beiden Co—O-Abstände sind deutlich verschieden (215,9 und 224,4 pm).In II und III ist Ampy einzählig und koordiniert über den endo-Stickstoff. Die Co—N-Abstände variieren von 210,9 bis 225,3 pm. Differenzierende Faktoren sind der unterschiedliche Transeinfluß von Hydrogencarbonat-bzw. Acetylacetonathaftatomen, aber auch die π-Wechselwirkung zwischen dem Zentralatom und dem Pyridinring, die beim cis-Komplex III stärker als beim trans-Komplex II ausgeprägt ist. Die Verbindungen II und III werden durch ein System von N—H … O-und O—H … O-Brücken stabilisiert.Im Falle des Nickels wurden die zu II und III analogen Komplexe erhalten, bei Mangan(II) konnte dagegen nur der Typ II realisiert werden.
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    URL: http://dx.doi.org/10.1002/zaac.19915980107
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    Trimethylsilyl-substituierte Amidinatokomplexe von Thallium(III). Die Kristallstruktur von [Ph—C(NHSiMe3)2] [Ph—C(NSiMe3)2 TICI3]Herrn Professor Eberhard Hoyer zum 60. Geburtstage am 26. Mai 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 600 (1991), S. 7-14 
    Details
    ISSN: 0044-2313
    Keywords: Amidinato complexes of thallium(III) ; syntheses ; i.r. spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Trimethylsilyl Substituted Amidinato Complexes of Thallium(III). The Crystal Structure of [Ph—C(NHSiMe3)2] [Ph—C(NSiMe3)2TlCl3]The amidinato complexes [Ph—C(NSiMe3)2TlCl3] and [Ph—C(NHSiMe3)2] [Ph—C(NSiMe3)2TlCl3] have been prepared by the reaction of TlCl3 with N,N,N′-tris(trimethylsilyl)benzamidine in THF solution. They were characterized by IR spectroscopy, [Ph—C(NHSiMe3)2] [Ph—C(NSiMe3)2TlCl3] additionally by an X-ray structure determination. Space group P21/c, Z = 4, 4300 observed unique reflexions, R = 0.053. Lattice dimensions at -43°C: a = 1157.2, b = 2346.3, c = 1536.9 pm, β = 105.98°. The structure consists of amidinium cations, and of anions [Ph—C(NSiMe3)2TlCl3]-, in which the thallium atom is fivefold surrounded by three chlorine atoms and by two nitrogen atoms of the amidinato chelate.
    Notes: Die Amidinatokomplexe [Ph—C(NHSiMe3)2TlCl2] und [Ph—C(NHSiMe3)2TlCl2] [Ph—C(NSiMe3)2TlCl3] entstehen bei der Einwirkung von Thallium(III)-chlorid auf N,N,N′-Tris(trimethylsilyl)benzamidin in Tetrahydrofuranlösung. Sie werden durch ihre IR-Spektren, und [Ph—C(NHSiMe3)2] [Ph—C(NSiMe3)2TlCl3] zusätzlich durch eine Kristallstrukturanalyse charakterisiert. Raumgruppe P21/c, Z = 4, 4300 unabhängige beobachtete Reflexe, R = 5,3%. Die Gitterkonstanten betragen bei -43°C: a = 1157,2; b = 2346,3; c = 1536,9 pm; β = 105,98°. Die Verbindung besteht aus einem Amidiniumkation und einem [Ph—C(NSiMe3)2TlCl3]--Anion, in dem das Thalliumatom verzerrt trigonal-bipyramidal von drei Cl-Atomen und chelatartig von den beiden N-Atomen des Amidinatoliganden umgeben ist.
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    Das Cyclotetraphosphan P4[P(tBu)2]4 (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 602 (1991), S. 73-78 
    Details
    ISSN: 0044-2313
    Keywords: 1,2,3,4-Tetrakis(di-tert-butylphosphanyl)-cyclo-tetraphosphane ; 31P n.m.r. ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Cyclotetraphosphane P4[P(tBu)2]4P4[P(tBu)2]4 1 is obtained by thermal decomposition (20°C) of (tBu)2P—P = P(tBu)2Br which is formed from [(tBu)2P]2PLi and 1,2-dibromoethane. The 31P NMR spectrum of 1 shows two complex signal patterns of the AA′ A″ A‴ XX′X″X‴ type; δ = +63 ppm (exocyclic) and δ = -43 ppm (cyclic).1 crystallizes monoclinic in the space group C2/c, (a = 2240.8(17) pm, b = 885.6(7) pm, c = 2221.8(14) pm, β = 101.72(5)°) with Z = 4 molecules in the elementary cell. The molecule has E conformation. The four-membered ring is folded (dieder angle 61°) to give the P(tBu)2 groups nearly equatorial and the lone pairs nearly axial positions.
    Notes: P4[P(tBu)2]4 1 entsteht bei der thermischen Zersetzung des (tBu)2P—P = P(tBu)2Br bei 20°C, das sich aus [(tBu)2P]2PLi und 1,2-Dibromethan bildet. Das 31P-NMR-Spektrum von 1 enthält zwei komplexe Signalgruppen; δ = +63 ppm (exocyclisch) und δ = -43 ppm (cyclisch). Es liegt ein AA′ A″ A‴ XX′X″X‴ Spinsystem vor. 1 kristallisiert monoklin in der Raumgruppe C2/c, a = 2240,8(17) pm, b = 885,6(7) pm, c = 2221,8(14) pm, β = 101,72(5)° mit Z = 4 Molekülen in der Elementarzelle. Das Molekül besitzt E-Konformation. Der Vierring ist gefaltet, Diederwinkel 61°. Dadurch nähern sich die P(tBu)2-Gruppen einer äquatorialen und die nichtbindenden Elektronenpaare am Phosphor einer axialen Position.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916020108
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    SmTiO3Cl: Präparation und Struktur - das erste Oxochlorotitanat der „mittleren“ Seltenen Erden (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 602 (1991), S. 119-128 
    Details
    ISSN: 0044-2313
    Keywords: Samarium oxochlorotitanate, SmTiO3Cl ; 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 SmTiO3ClThe compound SmTiO3Cl has been prepared by reaction of SmOCl/TiO2 (1:1) (with an admixture of small amounts of SmCl3) in evacuated silica ampoules (3 d, 800°C). Single crystals of SmTiO3Cl were obtained by chemical transport reaction (T2 → T1; T2 = 1000°C, T1 = 900°C) using chlorine (p(Cl2, 298 K) = 1 atm) as transport agent with a sintered mixture SmOCl/TiO2 (2:3) (800°C, 5d, evacuated silica ampoule) as starting material.SmTiO3Cl crystallizes in the monoclinic space group C2/m (No. 12) with cell dimensions a = 9.716(3) Å, b = 3.942(2) Å, c = 10.100(4) Å, β = 106.63(3)° and Z = 4. The structure was refined to give R = 3.8%, Rw = 3.9%. Main building units are TiO32--layers (parallel to the (110) plain) which are connected by eightfold coordinated Sm-atoms. The relationship of this new structure type with Nd2Ta2O7Cl2 and ThTi2O6 is considered.
    Notes: Die neue Verbindung SmTiO3Cl wurde durch Umsetzung von Gemengen SmOCl/TiO2 (1:1) (unter Zusatz geringer Mengen SmCl3) in evakuierten Quarzglasampullen dargestellt (3d, 800°C). Einkristalle wurden durch chemischen Transport (T2 → T1; T2 = 1000°C, T1 = 900°C) mit einem getemperten (800°C, 5d; evakuierte Quarzglasampulle) Gemenge SmOCl/TiO2 (2:3) als Startbodenkörper bei T2 sowie mit Chlor (p(Cl2, 298K) = 1 atm) als Transportmittel erhalten.SmTiO3Cl kristallisiert monoklin: RG: C2/m (No. 12) mit den Gitterkonstanten a = 9.716(3) Å, b = 3.942(2) Å, c = 10.100(4) Å, β = 106.63(3)° und Z = 4. Die Struktur wurde bis zu R = 3.8% bzw. Rw = 3.9% verfeinert. Die Koordination der Metallteilchen läßt sich durch TiO6-Oktaeder und durch 8-fach koordinierte Sm-Atome beschrieben. Parallel zur (110)-Ebene sind Schichten mit der Zusammensetzung TiO32- zu erkennen. Die Strukturverwandtschaft zu Nd2Ta2O7Cl2 und ThTi2O6 wird aufgezeigt.
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    URL: http://dx.doi.org/10.1002/zaac.19916020113
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    Zur Darstellung und Struktur neuer Niobate LnNb7O19(Ln = La, Ce) (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 602 (1991), S. 105-117 
    Details
    ISSN: 0044-2313
    Keywords: Lanthanum niobate, LaNb7O19 ; cerium niobate, CeNb7O19 ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Structure of LnNb7O19 (Ln = La, Ce)Two new ternary compounds, LaNb7O19 and CeNb7O19, could be prepared and characterized. At temperatures about 900°C already decomposition of both compounds will be initiated, but at lower temperatures (800°C) no reaction between the binary components occured. Single crystals could be obtained by chemical transport reactions (T2 → T1; T2 = 800°C; T1 = 780°C). Chlorine for mineralization or as transport agent is absolutely indispensable for preparation. Single crystal investigations on LaNb7O19 (R = 4.4%; Rw = 4.19%) result in the trigonal space group P3. The cell dimensions are a = 6.2531(2) A; c = 20.0685(10) Å; Z = 2. The structure can be described as to be build up by layers of 8-coordinated La and 6-coordinated Nb, alternating with layers of edge-sharing pentagonal NbO7-bipyramids. Corresponding to the unusual sequence of layers the structure of LnNb7O19 (Ln = La,Ce) is the first example of a trigonal member of a family of structures, which has been described in detail by Jahnberg. The most examples are represented by tantalates, but only a few niobates related to these structures are known.
    Notes: LaNb7O19 und CeNb7O19 wurden erstmals dargestellt und charakterisiert. Beide Verbindungen sind oberhalb 900 °C nicht mehr beständig; unterhalb dieser Temperatur gelang die Darstellung nur in Gegenwart eines Mineralisators (z. B. Cl2), jedoch nicht durch unmittelbare Umsetzung der binären Oxide („Festkörperreaktion“ bei z. B. 800 °C). Einkristalle wurden durch chemischen Transport (T2 → T1; T2 = 800 °C; T1 = 780 °C) mit dem Transportmittel Chlor (p(Cl2; 298 K) = 0,1 atm) zugänglich. Wie eine Strukturbestimmung (Einkristalldaten) zeigt (R = 4,4%; Rw= 4,19%), kristallisiert LaNb7O19 trigonal (RG:P3) mit a = 6,2531(2) Å; c = 20,0685(10) Å;Z = 2. In Richtung der c-Achse folgen unterschiedliche Schichten aufeinander, in denen einerseits La (CN = 8) und Nb (CN = 6) und andererseits kantenverknüpfte, pentagonale NbO7-Bipyramiden vorliegen. Orangerotes CeNb7O19 ist nach Guinierdaten mit LaNb7O19 istotyp. Beide sind aufgrund der Schichtfolge als erste Vertreter einer bisher unbekannten trigonalen Variante der von Jahnberg beschriebenen Strukturfamilie anzusehen, welcher bereits zahlreiche Tantalate, aber nur wenige Niobate angehören.
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    Ein Halogenooxoruthenat (IV, V): Ba6Ru2, 5Mn0, 5O12Cl2 mit neuem Strukturtyp (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 602 (1991), S. 143-147 
    Details
    ISSN: 0044-2313
    Keywords: Halogenooxoruthenate(IV, V) ; ruthenium ; oxygen ; chlorine ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: About a Halogenooxoruthenat (IV, V): Ba6Ru2,5Mn0,5O12Cl2 with a New Structure TypeBa6Ru2.5Mn0.5O12Cl2 was prepared and investigated by single crystal X-ray work (space group D3d3 - P3m1; a = b = 5.799; c = 14.853 Å; Z = 1). This structure type is characterized by «isolated», face-sharing (Ru/Mn)3O12-octahedratriple. Calculations of the Coulomb term of lattice energy support the charge distribution (5+/4+/5+) within the groups (Ru/Ru0.5Mn0.5/Ru)3O1210-. The coordination of barium by oxygen and chlorine within three different polyhedra is discussed in detail.
    Notes: Ba6Ru2, 5Mn0, 5O12Cl2 wurde dargestellt und mit Röntgenmethoden an Einkristallen untersucht (Raumgruppe D3d3 - P3m1; a = b = 5, 799; c = 14, 853 Å; Z = 1). Der neu gefundene Strukturtyp wird durch „isolierte“, flächenverknüpfte (Ru/Mn)3O12-Oktaedertripel charakterisiert. Berechnungen der Coulombenergie zeigen, daß; in den (Ru/Ru0,5Mn0,5/Ru)3O1210--Gruppen eine Ladungsverteilung (5+/4+/5+) vorliegt. Ba2+ zeigt drei verschiedene Koordinationspolyeder, die ausführlich diskutiert werden.
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    Darstellung und Kristallstruktur von Na28In14Sn15 (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 606 (1991), S. 79-90 
    Details
    ISSN: 0044-2313
    Keywords: Na28In14Sn15 Zintl compound ; 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 Na28In14Sn15Na28In14Sn15 was prepared from the elements. The crystal structure was determined by single crystal X-Ray and neutron diffraction methods (aro = 2299.3(3) pm, F43m, Z = 8). The structure elements can be explained in terms of the Zintl concept together with the valence rules of electron deficiency compounds as derivates of the arachno-Borane B3H9.
    Notes: Na28In14Sn15 wurde aus den Elementen dargestellt und strukturell über Röntgen- und Neutronenbeugungsmethoden an Einkristallen charakterisiert (aro = 2299,3(3) pm, F43m, Z = 8). Die Strukturelemente lassen sich über das Zintl-Konzept deuten bzw. als Abkömmlinge des arachno-Borans B3H9 nach den Valenzregeln der Elektronenmangelverbindungen interpretieren.
    Additional Material: 5 Ill.
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    Darstellung und Kristallstruktur von Cs2HgPdCl6, eine Verzerrungsvariante der ChloroperowskiteProfessor Hans-Joachim Seifert zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 603 (1991), S. 69-76 
    Details
    ISSN: 0044-2313
    Keywords: Dicesium mercury(II) palladium(II) hexachloride ; preparation ; crystal structure ; group-subgroup relation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of Cs2HgPdCl6, a Distorted Variant of ChloroperovskitsCs2HgPdCl6 single crystals show tetragonal symmetry with the space group I 4/m m m (No. 139) with 2 formular units per unit cell. The lattice parameters are a = 7.432(4) Å, c = 10.874(7) Å. The atomic arrangement of Cs2HgPdCl6 is explored by X-ray crystal structure analysis. The important polyhedrons are square-planar PdCl4 groups and HgCl2 dumbbells. The PdCl4 group is completed by two further chlorine atoms to a elongated octahedron and four further chlorine atoms form with the HgCl2 dumbbell a compressed octahedron. The crystal structure of Cs2HgPdCl6 is compared with the arrangement in halogenoperovskits and in Rb2PdCl4 [3].
    Notes: Die Verbindung Cs2HgIIPdIICl6 läßt sich durch Festkörperreaktion phasenrein darstellen. Sie kristallisiert in der Raumgruppe I 4/m m m (No. 139) mit a = 7,432(4) Å, c = 10,874(7) Å, Z = 2. Die Kristallstruktur wurde mit röntgenographischen Methoden an Einkristallen ermittelt. Pd2+ ist quadratisch-planar und Hg2+ hantelförmig von Cl-umgeben. In zweiter Nachbarschaft ergänzen weitere Cl- zu gestreckten bzw. gestauchten Oktaedern. Dieses Bauprinzip entspricht dem Aufbau von Cs2AuIAuIIICl6 [1, 2]. Es besteht direkte kristallchemische Beziehung zur Kristallstruktur der Halogenoperowskite bzw. des K2PdCl4-Typs.
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    Polysulfonylamine XXVI. Ein polymeres Lithiumamid mit alternierend tetra- und hexakoordinierten Lithiumatomen: Kristallstruktur von Lithiumdimesylamid-Monohydrat (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 604 (1991), S. 47-51 
    Details
    ISSN: 0044-2313
    Keywords: Polysulfonyl amines ; lithium dimesylamide monohydrate ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Polysulfonyl Amines. XXVI. A Polymeric Lithium Amide with Alternating Tetra- and Hexacoordinate Lithium Atoms: Crystal Structure of Lithium Dimesylamide MonohydrateLiN(SO2CH3)2 · H2O crystallizes in the orthorhombic space group Cmc21. The lithium atoms and the water molecules form infinite zigzag chains —Li(2)—OH2—Li(1)—OH2—Li(2)—. The dimesylamide anion acts as a tridentate bridging ligand, using N and one O atom of each sulfonyl group as donor atoms. In the chain depicted above, Li(1) is additionally coordinated by two N atoms, Li(2) by four O atoms of four different dimesylamide groups. Thus, Li(1) attains a nearly ideal tetrahedral (N2O2)-coordination, Li(2) a distorted octahedral (O6)-coordination. The overall result of the coordination pattern is a string with a repeat unit consisting of four condensed six-membered rings. The repeat units are linked in a spirane-like fashion at Li(2) as the spiro atom. The strings are three-dimensionally interconnected by hydrogen bonds. Two extremely short (S = O) bonds (137pm) are observed in the repeat unit.
    Notes: LiN(SO2CH3)2 · H2O kristallisiert in der orthorhombischen Raumgruppe Cmc21. Die Li-Atome und die Wassermoleküle sind zu unendlichen Zickzack-Ketten —Li(2)—OH2—Li(1)—OH2—Li(2)— verknüpft. Das Dimesylamid-Anion fungiert als dreizähniger Brückenligand mit dem N-Atom und je einem O-Atom der beiden Sulfonylgruppen als Donoratomen. Außer von den Wassermolekülen wird jedes Li(1) von zwei N-Atomen, jedes Li(2) von vier O-Atomen aus vier verschiedenen Dimesylamid-Gruppen koordiniert. Auf diese Weise erreicht Li(1) eine nahezu ideale tetraedrische (N2O2)-Koordination, Li(2) eine verzerrt oktaedrische (O6)-Koordination. Das Ergebnis des Koordinationsmusters ist ein Strang, dessen Repetiereinheit aus vier kondensierten Sechsringen besteht. Die Repetiereinheiten sind über Li(2) spiranartig verknüpft. Die Stränge sind über Wasserstoffbrücken dreidimensional quervernetzt. In der Repetiereinheit werden zwei extrem kurze (S = O)-Bindungen (137 pm) beobachtet.
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    Konformation von 2-Amino-4-methoxy-6-methyl-1,3,5-triazin (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 604 (1991), S. 53-62 
    Details
    ISSN: 0044-2313
    Keywords: 1, 3, 5-triazine ; 2-amino-4-methoxy-6-methyl-1,3,5-triazine ; preparation ; crystal structure ; ir, Raman spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Conformation of 2-Amino-4-methoxy-6-methyl-1,3,5-triazineThe title compound AMMT (formula see „Inhaltsübersicht“) has been produced by reaction of N-(methoxycarbimidoyl) guanidine with acetic anhydride and characterized by different methods.AMMT crystallizes at 20°C with Z = 4 orthorhombic with lattice constants a = 6.709(1) Å, b = 7.971(1) Å, c = 12.303(2) Å, α = β = γ = 90.0(1)°. The crystal structure has been approximately determined by X-ray methods in the triclinic space group P1 (R = 0.28, Rw = 0.27).The arrangement of the 1, 3, 5-triazine ring atoms and those of the substituents is exactly plane. The molecules are oriented in a typical layer structure with layers perpendicular to the crystallographic a-axis in agreement with the observed cleavage. The vibrational data from powder infrared and single crystal Raman measurements confirm this special conformational situation in the solid state. Concerning the Raman experiments the orientation of the laser beam along the crystallographic axis b or c causes no inplane ring vibrations to occur in the resulting spectra.
    Notes: Die Titelverbindung AMMT wurde durch Umsetzung von N-(Methoxycarbimidoyl) guanidin mit Essigsäureanhydrid hergestellt und mit verschiedenen Methoden charakterisiert.AMMT kristallisiert bei 20°C mit Z = 4 orthorhombisch mit den Gitterkonstanten a = 6,709(1) Å, b = 7,971(1) Å, c = 12,303(2) Å, α = β = γ = 90,0(1)°. Die Kristallstruktur wurde unter der Annahme des Vorliegens der triklinen Raumgruppe P1 näherungsweise aufgeklärt (R = 0,28, Rw = 0,27).Die 1,3,5-Triazin-Ringatome und die der Substituenten sind exakt planar angeordnet. AMMT besitzt eine typische Schichtstruktur mit Schichten senkrecht zur kristallographischen a-Achse in Übereinstimmung mit der beobachteten Spaltbarkeit. Die Schwingungsspektren (Pulver-Infrarot und Einkristall-Raman) bestätigen diese spezielle Anordnung. Bei Einstellung des Laserstrahls parallel zur kristallographischen b- oder c-Achse werden keine in-plane Ring-Schwingungen registriert.
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    URL: http://dx.doi.org/10.1002/zaac.19916040108
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    Guanidiniumhexafluorometallate von Titan, Silicium, Germanium und Zinn. Guanidiniumpentafluorooxoniobat und Guanidiniumtetrafluorodioxowolframat (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 604 (1991), S. 77-83 
    Details
    ISSN: 0044-2313
    Keywords: Guanidinium hexafluorometallates ; guanidinium pentafluorooxoniobate ; guanidinium tetrafluorodioxowolframate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Guanidinium Hexafluorometallates of Titanium, Silicon, Germanium, and Tin. Guanidinium Pentafluorooxoniobate and Guanidinium TetrafluorodioxowolframateThe title compounds were crystallized from the aqueous solutions of their fluorometallate respectively oxofluorometallate acids by adding of guanidinium fluoride solution. Their unit cells were determined and for [C(NH2)3]2 TiF6 its crystal structure was determined: s. g. Cm, a = 12.869 Å, b = 7.378 Å, c = 6.243 Å, β = 114.45°, layer structure, R = 0.0257. The unit cell parameters of [C(NH2)3]2 SiF6: a = 12.612 Å, b = 7.272 Å, c = 6.171 Å, β = 114.30°, of [C(NH2)3]2 GeF6: a = 12.773 Å, b = 7.343 Å, c = 6.202 Å, β = 114.38°, of [C(NH2)3]2 SnF6 : a = 12.972 Å, b = 7.439 Å, c = 6.356 Å, β = 114.14°, of [C(NH2)3]2 NbOF5:a = 12.987 Å, b = 7.425 Å, c = 6.326 Å, β = 114,25°, of [C(NH2)3]2 WO2F4:a = 12.941 Å, b = 7.396 Å, c = 6.256 Å, β = 114.33°.
    Notes: Die Titelverbindungen wurden aus den wässrigen Lösungen der jeweiligen Fluorometallat-bzw. oxofluorometallatsäuren nach Zugabe von Guanidiniumfluoridlösung als kristalline Verbindungen erhalten und ihre Gitterkonstanten bestimmt. Vom [C(NH2)3]2 Tif6 wurde die Kristallstruktur bestimmt: R.Gr. Cm, a = 12,869 Å, b = 7,378 Å, c = 6,243 Å, β = 114,45°, Schichtstruktur, R = 0,0257. Kristallographische Daten von [C(NH2)3]2 SiF6:a = 12,612 Å, b = 7,272 Å, c = 6,171 Å, β = 114,30°, von [C(NH2)3]2 GeF6:a = 12,773 Å, b = 7,343 Å, c = 6,202 Å, β = 114,38°, von [C(NH2)3]2 SnF6:a = 12,972 Å, b = 7,439 Å, c = 6,356 Å, β = 114,14°, von [C(NH2)3]2 NbOF5:a = 12,987 Å, b = 7,425 Å, c = 6,326 Å, β = 114,25°, von [C(NH2)3]2 WO2F4:a = 12,941 Å, b = 7,396 Å, c = 6,256 Å, β = 114,33°.
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    URL: http://dx.doi.org/10.1002/zaac.19916040111
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    Komplexchemie P-reicher Phosphane und Silylphosphane. IV. Bildung und Struktur der Chromcarbonylkomplexe des Tris(di-tert-butylphospha)heptaphosphanortricyclans, (t-Bu2P)3P7Professor Kurt Dehnicke zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 595 (1991), S. 67-94 
    Details
    ISSN: 0044-2313
    Keywords: Tris(di-tert-butylphospha)heptaphosphanortricyclane chromium carbonyl complexes ; syntheses ; 31P(1H) n.m.r. spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Transition Metal Complexes of P-rich Phosphanes and Silylphosphanes. IV. Formation and Structure of the Chromium Carbonyl Complexes of Tris(di-tert-butylphospha)heptaphosphanortricyclane (t-Bu2P)3P7The reaction of (t-Bu2P)3P7 1 with Cr(CO)5 · THF in a molar ratio of 1:1 yields yellow crystals of (t-Bu2P)3P7[Cr(CO)5] 2 having the Cr(CO)5 group coordinated to a Pb atom (basal) of the three membered ring. With a molar ratio of 1:2 compounds 2, (t-Bu2P)3P7[Cr(CO)5]2 3, (t-Bu2P)3P7[Cr(CO)5][Cr(CO)4] 4 and (t-Bu2P)3P7[Cr(CO)4]2 5 were obtained. In 3 (yellow crystals) one Cr(CO)5 group is linked to a Pb atom, the other one to an exocyclic Pexo atom. On irradiation 3 loosing one CO group generates 4 (orange red crystals) with an unchanged Cr(CO)5 group linked to the Pb atom and a five membered chelate-like ring containing an apical Pa atom, two equatorial Pa atoms, one Pexo atom and the Cr atom of the carbonyl group. Compound 5 (orange red crystals) contains two such five membered rings. (t-Bu2P)3P7[Cr(CO)4]3 6 (red needles) is formed with Cr(CO)5 · THF in a molar ratio of 1 : 1. However, even with higher amounts of Cr(CO)5 · THF and after extended reaction times, only 6 is formed; no further Cr carbonyl group could be attached to the P skeleton. With Cr(CO)5 · NBD in a molar ratio of 1 : 1, (t-Bu2P)3P7[Cr(CO)4] 7 is produced from 1, and 5 with a molar ratio of 2 : 1. As in 4, the Cr(CO)4 group in 7 (orange crystals) participates in a five membered chelate-like ring. It was not possible to generate 6 from 5 with an excess of Cr(CO)4 · NBD and with extended reaction times.The molecular structures of the compounds were identified by investigating the 31P[1H] NMR spec-tra and considering especially the coordination shift, and by crystal structure determinations of 2 and 4. Compound 2 crystallizes in the space group PI (no.2) with a = 1566.2(4) pm, b = 2304.1(5) pm, c = 1563.3(4) pm,α = 95.57(3)°, β = 108.79(3)°, γ = 109.82(4)° and Z = 4 formula units in the elementary cell. Compound 4 crystallizes in the space group P 21 /n (no. 14) with a = 1416.6(5) pm, b = 2573.6(5) pm, c = 1352.9(4) pm,β = 99.17(5)° and Z = 4 formula units in the elementary cell.
    Notes: Die Umsetzung von (t-Bu2P)3P7 1 mit Cr(CO)5 · THF im Molverhältnis 1:1 führt zu (t-Bu2P)3P7[Cr(CO)5] 2 (gelbe Kristalle), in dem die Cr(CO)5-Gruppe an ein Pb-Atom des P-Dreirings koordiniert ist. Bei Umsetzung im Molverhältnis 1:2 bilden sich die Verbindungen 2, 3, 4 sowie 5: (t-Bu2P)3P7[Cr(CO)5]2 3; (t-Bu2P)3P7[Cr(CO)5][Cr(CO)4] 4; (t-Bu2P)3P7[Cr(CO)4]2 5. In 3 (gelbe Kristalle) ist eine Cr(CO)5-Gruppe an einem Pb-Atom (basal), die andere an einem Pexo-Atom (exocyclisch) gebunden. Bei Lichteinwirkung geht 3 unter Verlust einer CO-Gruppe in Verbindung 4 (orangerote Kristalle) über, in der die Cr(CO)5-Gruppe am Pb-Atom steht und die folgenden Atome einen Chelatfünfring bilden: ein Pa- (apikal), zwei Pe-, ein Pexo-, das Cr-Atom der Cr(CO)4-Gruppe. Verbindung 5 (orangerote Kristalle) enthält einen zweiten Chelatfünfring. (t-Bu2P)3P7[Cr(CO)4]3 6 (rote Nadeln) bildet sich aus 5 mit Cr(CO)5 · THF (Molverhältnis 1:1). Auch bei höheren Konzentrationen an Cr(CO)5 · THF und längeren Reaktionszeiten entsteht 6, und es gelingt nicht die Einführung einer weiteren Cr(CO)5-Gruppe an einem Pb-Atom. Mit Cr(CO)4NBD reagiert 1 (Molverhältnis 1:1) zu (t-Bu2P)3P7[Cr(CO)4] 7, im Molverhältnis 2:1 zu 5. In 7 (orange Kristalle) ist die Cr(CO)4-Gruppe analog zu 4 in den Chelatfünfring eingebunden. Verbindung 5 bildet auch bei höheren Konzentrationen an Cr(CO)4NBD und längeren Reaktionszeiten nicht Verbindung 6. Die Molekülstrukturen der Verbindungen folgen aus der Untersuchung der 31P{1H}-NMR-Spektren (Koordinationsverschiebung) und der Kristallstrukturuntersuchung der Verbindungen 2 und 4. 2 kristallisiert in der Raumgruppe P1 (Nr. 2) mit a = 1 566,2(4) pm, b = 2304,1(5) pm, c = 1 563,3(4) pm, α = 95,57(3)°, β = 108,79(3)°, γ = 109,82(4)° und Z = 4 Formeleinheiten. 4 kristallisiert in der Raumgruppe P21/n (Nr. 14) mit a = 1 416,6(5)pm, b = 2 573,6(5) pm, c = 1 352,9(4) pm, β = 99,17(5)° mit Z = 4 Formeleinheiten.
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    Ca3Cl2CBN, eine Verbindung mit dem neuen Anion CBN4- (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 594 (1991), S. 113-118 
    Details
    ISSN: 0044-2313
    Keywords: Ca3Cl2CBN ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ca3Cl2CBN, a Compound with the New CBN4- UnitThe new compound Ca3Cl2CBN was obtained from the reaction of Ca and CaCl2 with CaCN2, B and C or with BN and C, in sealed tantalum containers at 900°C. The crystal structure is related with the structure of Ca3Cl2C3 whereas the C34- units (C2v symmetry) are substituted by isoelectronic CBN4- anions (Cs symmetry): Ca3Cl2CBN, Pnma, a = 1 386.7(9) pm, b = 384.7(3) pm, c = 1 124.7(6) pm, Z = 4; R = 0.055, Rw = 0.036 for 380 independent intensities.The CBN4- units are located between layers of Ca2+ that are interconnected by Cl-. The bond angle (C—B—N) is 176° and bond distances are dC—B = 144 pm and dB—N = 138 pm, respectively.
    Notes: Die neue Verbindung Ca3Cl2CBN bildet sich bei der Reaktion von Ca und CaCl2 mit CaCN2, B und C oder mit BN und C in verschweißten Tantalkapseln bei 900°C. Die Kristallstruktur ist mit der Struktur von Ca3Cl2C3 verwandt, wobei statt den C34--Ionen (C2v-Symmetrie) isoelektronische CBN4--Einheiten (Cs-Symmetrie) vorliegen. Ca3Cl2CBN kristallisiert orthorhombisch (Pnma) mit: a = 1 386,7(9) pm, b = 384,7(3) pm, c = 1 124,7(6) pm, Z = 4; R = 0,055, Rw = 0,036 für 380 unabhängige Intensitäten. Die CBN4--Einheiten liegen zwischen Schichten aus Ca2+, die durch Cl- verbrückt sind. Der Bindungswinkel (C—B—N) beträgt 176°, die Bindungslängen dC—B = 144 pm und dB—N = 138 pm.
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    Li2MnBr4(o-rh.) - eine geordnete NaCl-Defektstruktur des SnMn2S4-TypsProfessor Hans-Joachim Seifert zum 60. Geburtstag am 9. November 1990 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 592 (1991), S. 106-114 
    Details
    ISSN: 0044-2313
    Keywords: Dilithium manganese tetrabromide, Li2MnBr4 ; crystal structure ; neutron diffraction data ; MAPLE calculations ; Raman spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Li2MnBr4(o-rh.) - an Ordered NaCl Defect Structure of the SnMn2S4 TypeNeutron diffraction data of Li2MnBr4 at 25°C are presented. The orthorhombic room-temperature polymorph of Li2MnBr4 (space group Cmmm, Z = 2, a = 777.78(4), b = 1106.58(5), and c = 388.18(2) pm, RI = 6.7%) crystallizes in an ordered NaCl defect structure (SnMn2S4 type). The tetragonally distorted MBr6 octahedra are elongated in the case of LiBr6 and compressed for MnBr6 owing to the different sharing of these units. The crystal structure of Li2MnBr4 oC14 (and those of alternative structure models with a larger pseudotetragonal cell) are discussed with respect to X-ray intensities, Madelung part of lattice energy (MAPLE), and the Raman spectra. The symmetry coordinates and vibrational modes of the \documentclass{article}\pagestyle{empty}\begin{document}$ (\mathop {\rm k}\limits^ \to = 0) $\end{document} phonons of Li2MnBr4 oC14 are given.
    Notes: Die Kristallstruktur der Raumtemperaturmodifikation von Li2MnBr4 wurde mit Hilfe von Neutronenpulvermessungen bestimmt. Li2MnBr4(o-rh.) (Raumgruppe Cmmm, Z = 2, a = 777,78(4), b = 1106,58(5) und c = 388,18(2) pm, RI = 6,7%) kristallisiert in einer geordneten NaCl-Defekt-(bzw. Über-)struktur (SnMn2S4-Typ). Die MBr6-Oktaeder sind (mit unterschiedlicher Verknüpfung) tetragonal gestaucht (Mn) bzw. gestreckt (Li). Die Kristallstruktur von Li2MnBr4 oC14 (sowie von alternativen Strukturmodellen einer größeren pseudotetragonalen Zelle) wird unter Einbeziehung der Röntgenintensitäten, von Madelungenergien (MAPLE) sowie der Ramanspektren diskutiert. Die Symmetriekoordinaten und Schwingungsformen der Gitterschwingungen \documentclass{article}\pagestyle{empty}\begin{document}$ (\mathop {\rm k}\limits^ \to = 0) $\end{document} des Li2MnBr4 oC14 werden mitgeteilt.
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    URL: http://dx.doi.org/10.1002/zaac.19915920112
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    Thallium(I)-Thiolate: Darstellung, Struktur und Eigenschaften von TlSC6H5, TlS-t-C4H9 und TlSC7H7Professor Kurt Dehnicke zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 595 (1991), S. 167-182 
    Details
    ISSN: 0044-2313
    Keywords: Thallium(I) thiolates ; syntheses ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thallium(I) Thiolates: Synthesis, Structure, and Properties of TlSC6H5, TlS-t-C4H9, and TlSC7H7By reaction of thallium(I) salts with sodium thiolates in organic solvents it is possible to synthesize and crystallize polymeric and oligomeric neutral thallium(I) thiolate complexes. The polymeric crystal structure of yellow benzenethiolato thallium(I) TlSC6H5 (space group P213, a = 19.943(3) Å at 143 K) is built up by the two novel structure units [Tl7(SC6H5)6]+ and [Tl5(SC6H5)6]-. Yellow tert.-butanethiolato thallium(I) TlS-t-C4H9 (space group P1, a = 11.490(3), b = 11.490(3), c = 12.698(4) Å, α = 108.31(3), β = 91.21(2), σ = 116.99(3)° at 143 K) consists of [Tl8(S-t-C4H9)8] molecules, the thallium atoms being either in trigonal pyramidal or ψ-trigonal bipyramidal coordination. Yellow phenylmethanethiolato thallium(I) TlSC7H7 crystallizes as thin plates (space group: Pbcn, a = 31.215(9), b = 7.173(2), c = 7.184(2) Å at 293 K). The crystal structure contains chains of fourmembered Tl2S2 rings which are linked through trans edges to form a ladder-like arrangement. Each thallium atom is coordinated trigonal-pyramidally by three sulfur atoms. The vibrational spectra of the compounds are reported.
    Notes: Durch Umsetzung von Thallium(I)-Salzen mit Natriumthiolaten in organischen Lösungsmitteln gelang die Synthese und Kristallisation von polymeren und oligomeren neutralen TlI-Thiolat-Komplexen. Das gelbe Benzolthiolatothallium(I) TlSC6H5 (Raumgruppe P213, a = 19,943(3) Å bei 143 K) enthält in der polymeren Kristallstruktur die zwei neuartigen Strukturelemente [Tl7(SC6H5)6]+ und [Tl5(SC6H5)6]-. Die Thallium-Atome sind entweder trigonal-pyramidal oder ψ-trigonal-bipyramidal koordiniert. Das gelbe tert.-Butanthiolato-thallium(I) TlS-t-C4H9 (Raumgruppe P1, a = 11,490(3), b = 11,490(3), c = 12,698(4) Å, α = 108,31(3), β = 91,21(2), σ = 116,99(3)° bei 143 K) wird aus [Tl8(S-t-C4H9)8]-Molekülen aufgebaut, wobei die Thallium-Atome wieder trigonal-pyramidal und ψ-trigonal-bipyramidal koordiniert sind. Phenylmethanthiolato-thallium(I) TlSC7H7 kristallisiert in Form dünner gelber Plättchen (Raumgruppe: Pbcn, a = 31,215(9), b = 7,173(2), c = 7,184(2) Å bei 293 K). Die Kristallstruktur enthält Thallium-Thiolat-Ketten, die strickleiterartig aus trans-verknüpften Tl2S2-Vierringen bestehen. Jedes Thallium-Atom ist trigonal-pyramidal von drei Schwefel-Atomen koordiniert. Über schwingungsspektroskopische Untersuchungen wird berichtet.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915950116
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    Silber(I)-catena-Polysilicat Kristallzüchtung und Strukturanalyse (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 601 (1991), S. 5-11 
    Details
    ISSN: 0044-2313
    Keywords: Silver(I)-catena-polysilicate ; crystal growth ; crystal structure ; uv/vis absorption ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Silver(I)-catena-Polysilicate, Crystal Growth, and Structure DeterminationAg2SiO3 has been synthesized as powder and single crystals from the binary components applying hydrothermal conditions. According to the results of an X-ray crystal structure analysis (P212121; a = 452.7(1), b = 710.8(1), c = 995.9(1) pm; Z = 4; 1387 reflexions, 57 refined parameters; R = 0.060) the title compound contains a ‘zweier single chain’ catena-polysilicate anion. The UV/VIS absorption spectrum shows an absorption edge at 19700 cm-1.
    Notes: Ag2SiO3 wurde unter hydrothermalen Bedingungen aus den binären Komponenten als Pulver und Einkristalle dargestellt. Nach der Röntgenstrukturanalyse (P212121; a = 452,7(1), b = 710,8(1), c = 995,9(1) pm; Z = 4; 1387 Reflexe, 57 Parameter; R = 0,06) handelt es sich um ein catena-Polysilicat mit einer Zweiereinfachkette. Das UV/VIS-Spektrum zeigt eine Absorptionskante bei 19 700 cm-1.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916010102
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    Neue Untersuchungen zu Präparation und Struktur von Rb4O6Professor Hans-Georg von Schnering zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 598 (1991), S. 163-173 
    Details
    ISSN: 0044-2313
    Keywords: Rubidiumsesquioxide ; Rb4O6 ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reinvestigation of Rubidiumsesquioxide, Rb4O6Rb4O6 was prepared as a pure substance by solid state reaction between Rb2O2 and RbO2; it proves to be thermodynamically stable. The suggested structure was confirmed and refined by X-ray powder and single crystal methods (I43d; a = 932,42(4) pm; Rb4(O2-)2(O22-); Z = 4). Rb4O6 melts at 461°C followed by exothermic decomposition. The fact that O2- and O22- cannot be distinguished is discussed.
    Notes: Rb4O6 wurde durch Festkörperreaktion zwischen Rb2O2 und RbO2 erstmals röntgenrein dargestellt; es ist thermodynamisch stabil. Der bestehende Strukturvorschlag konnte durch röntgenographische Pulver- und Einkristalluntersuchungen bestätigt und verfeinert werden (I43d; a = 932,42(4) pm, Rb4(O2-)2(O22-), Z = 4). Rb4O6 schmilzt bei 461°C mit anschließender exothermer Zersetzung. Das Problem der Ununterscheidbarkeit von O2- und O22- wird diskutiert.
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    URL: http://dx.doi.org/10.1002/zaac.19915980116
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    Über Cs2Li2[GeO4]Professor Heinrich Puff zum 70. Geburtstage am 1. November 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 605 (1991), S. 43-50 
    Details
    ISSN: 0044-2313
    Keywords: Cesium lithium orthogermanate ; preparation ; crystal structure ; MAPLE calculation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: About Cs2Li2[GeO4]By heating of a well-ground mixture of the binary oxides CsO0.55, Li2O and GeO2 (Cs:Li:Ge=2,6:2,2:1; Ni-tube; 600 °C; 49d) we got single crystals of Cs2Li2[GeO4] for the first time. Cs2Li2[GeO4] is isotypic to Rb2Li2[MO4] [M = Si, Ti, Ge] [2] and Cs2Li2[MO4] (M = Si, Ti) [3]: according to this Cs2Li2[GeO4] crystallizes triclinic, in the spacegroup P1 with a = 968.7(4) pm, b = 586.0(2) pm, c = 571.4(2) pm, α = 92.71(4)°, β = 110.95(3)° and γ = 94.34(4)° (Guinier-Simon data), Z = 2. The structure was determined by four-circle diffractometer data (Ag—Kα; 2381 Io(hkl); R = 8,4%; Rw = 5.0%), parameters see text. Further the Madelung Part of Lattice Energy (MAPLE), Effective Coordination Numbers (ECoN) and the Mean Fictive Ionic Radii (MEFIR), have been calculated.
    Notes: Durch Tempern inniger Gemenge der binären Oxide CsO0,55, Li2O und GeO2 (Cs:Li:Ge = 2,6:2,2:1; Ni-Bömbchen; 600°C; 49d) wurden erstmals Kristalle von Cs2Li2[GeO4] erhalten. Cs2Li2[GeO4] ist zu Rb2Li2[MO4] (M = Si, Ti, Ge) [2] und Cs2Li2[MO4] (M = Si, Ti) [3] isotyp; hiernach kristallisiert Cs2Li2[GeO4] triklin, in der Raumgruppe P1 mit a = 968,7(4) pm, b = 586,0(2) pm, c = 571,4(2) pm, α = 92,71(4)°, β = 110,95(3)° und γ = 94,34(4)° (Guinier-Simon Daten), Z = 2. Die Struktur wurde mittels Vierkreisdiffraktometer (Ag-Kα; 2381 I0(h k l); R = 8,4%; Rw = 5,0%) bestimmt, Parameter siehe Text. Weiterhin wurden der Madelunganteil der Gitterenergie (MAPLE), Effektive Koordinationszahlen (ECoN) und die Mittleren Fiktiven Ionenradien (MEFIR) berechnet.
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    URL: http://dx.doi.org/10.1002/zaac.19916050105
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    Das erste quinquinäre Orthoborat der Alkalimetalle: Cs3Na {Li2[BO3]2}Professor Joseph Grobe zum 60. Geburtstage am 2. November 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 605 (1991), S. 25-34 
    Details
    ISSN: 0044-2313
    Keywords: Alkali metal orthoborate, Cs3NA{Li2[BO3]2} ; preparation ; crystal structure ; MAPLE calculation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The First Quinquinary Orthoborate of the Alkali Metals: Cs3Na{Li2[BO3]2}For the first time Cs3NaLi2B2O6 was obtained by ‘exchange reaction’ from an intimate mixture of NaLi2[BO3] and Cs2O (Cs:B = 2:1) in the form of colourless lamellar single crystals. The structure determination (four-circle diffractometer AED 2, MoKα, 3213 Io(hkl), R = 6.3%, Rw = 4.9%) confirms the space group P1;a = 1026.7(7) pm, b = 733.4(4) pm, c = 673.3(5) pm, α = 103.92(5)°, α = 101.41(6)°, β = 96.68(5)°; Z = 2.The characteristic structure units are chains ∞11{Li2B2O6} consisting of approximately trigonal planar [BO3] groups and distorted [LiO4] tetrahedra.Effective Coordination Numbers (ECoN), Mean Fictive Ionic Radii (MEFIR) and the Madelung Part of Lattice Energy (MAPLE) are calculated.
    Notes: Erstmals wurde Cs3NaLi2B2O6 durch ‚Austauschreaktion‘ aus einem Gemenge von NaLi2[BO3] und Cs2O (Cs:B = 2:1) in Form von farblosen, plättchenförmigen Einkristallen erhalten. Die Strukturaufklärung (Vierkreisdiffraktometer AED 2, MoKα, 3213 I0(h k l), R = 6,3%, Rw = 4,9%) bestätigt die Raumgruppe P1; a = 1026,7(7) pm, b = 733,4(4) pm, c = 673,3(5) pm, α = 103,92(5)°, β = 101,41(6)°, γ = 96,68(5)°; Z = 2.Charakteristische Strukturelemente sind Ketten ∞1{Li2B2O6} aus annähernd trigonal planaren [BO3]-Gruppen und verzerrten [LiO4]-Tetraedern.Effektive Koordinationszahlen (ECoN), Mittlere Fiktive Ionenradien (MEFIR) und der Madelunganteil der Gitterenergie (MAPLE) werden berechnet.
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    URL: http://dx.doi.org/10.1002/zaac.19916050103
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    Das erste quaternäre Alkalioxoarsenat(V): Cs2Na[AsO4] (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 605 (1991), S. 67-74 
    Details
    ISSN: 0044-2313
    Keywords: Alkali metal orthoarsenate, Cs2Na[AsO4] ; crystal structure ; MAPLE calculation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The First Quaternary Alkalioxoarsenate (V): Cs2Na[AsO4]By heating of well-ground mixtures of the binary oxides (“Cs2O”, Na2O2, As2O3; Cs:Na:As = 2:1:1; Ni-tube, 500 °C, 21d) bright, colourless single crystals were obtained for the first time. The new arsenate crystallices monoclinic (space group P21/m) with a = 827,5(2), b = 615,7(2), c = 605,6(2) pm, β = 91,98(2)° (Guinier-Simon powder data), Z = 2. It is isotypic with Cs2Na[VO4] [2]. The structure was determined by four-circle-diffractometer data [Siemens AED II, MoKα, 1155 Io (hk1), R = 5.1%, Rw = 4.4%, parameters see text]. The Madelung Part of Lattice Energy, MAPLE, and Effective Coordination Numbers, ECoN, these calculated via Mean Fictive Ionic Radii, MEFIR, are calculated and discussed.
    Notes: Erstmals wurde Cs2Na[AsO4] beim Tempern inniger Gemenge der binären Oxide („Cs2O“, Na2O2, As2O3; Cs: Na : As = 2:1:1; Ni-Bombe, 500° C, 21 d) in Form prachtvoller, farbloser Einkristalle erhalten. Das neue Orthoarsenat(V) kristallisiert monoklin (Raumgruppe P21/m) mit a = 827,5(2), b = 615,7(2), c = 605,6(2) pm, β = 91,98(2)° (Guinier-Simon-Pulverdaten), Z = 2, Es ist isotyp mit Cs2Na[VO4][2]. Die Struktur wurde mittels Vierkreisdiffraktometerdaten [Siemens AED II, MoKα, 1151 Io (hkl), R = 5,1%, Rw = 4,4%, Parameter siehe Text]; aufgeklärt. Der Madelunganteil der Gitterenergie, MAPLE, und Effektive Koordinationszahlen, ECoN, diese über Mittlere Fiktive Ionenradien, MEFIR, werden berechnet und diskutiert.
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    URL: http://dx.doi.org/10.1002/zaac.19916050108
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    [La2Cl3(OAc)2(H2O)7]Cl: Das erste Lanthanid-Acetat-Halogenid-Hydrat mit Chlorid in innerer KoordinationssphäreProfessor Hans-Georg von Schnering zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 598 (1991), S. 299-306 
    Details
    ISSN: 0044-2313
    Keywords: Lanthanides ; crystal structure ; acetate halides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [La2Cl3(OAc)2(H2O)7]Cl: The First Lanthanide-Acetate-Halide-Hydrate with Chloride in Inner-Sphere Coordination[La2Cl3(OAc)2(H2O)7]Cl has been obtained as single crystals through the reaction of LaCl3 · 7H2O with diluted acetic acid or from La2O3 with acetyl chloride. In the crystal structure (triclinic, Z = 2, P1 (no. 2), a = 919.6(2), b = 950.7(2), c = 1178.9(2) pm, α = 82.52(1), β = 84.14(1), γ = 64.69(1)°, R = 0.021, Rw = 0.020), La3+ is surrounded by nine ligands (O, Cl). La1 has two chloride and seven oxygen ligands whereas La2 has one chloride and eight oxygen atoms as nearest neighbours. Four of the oxygen ligands of each lanthanum cation originate from a „tetradentate“ acetate anion, the others from crystal water molecules. The „tetradentate“ acetate groups are coordinated not only to one central La3+ as chelate ligands, but also to the „left“ and „right“ La3+ neighbours. Thereby, a one-dimensional infinite cationic chain, 1∞[La2Cl3(OAc)2(H2O)7]+, is formed that runs in the [011] direction. These chains are held together by „lonesome“ chloride ions which are surrounded by (4 + 1) water molecules and connected to the chains via hydrogen bonds.
    Notes: [La2Cl3(OAc)2(H2O)7]Cl wurde in einkristalliner Form durch Umsetzung von LaCl3 · 7H2O mit und in verdünnter Essigsäure oder von La2O3 mit Acetylchlorid erhalten. In der Kristallstruktur (triklin, Z = 2, P1 (Nr. 2); a = 919,6(2); b = 950,7(2); c = 1178,9(2) pm; α = 82,52(1), β = 84,14(1); γ = 64,69(1)°; R = 0,021; Rw = 0,020) ist La3+ von jeweils neun Liganden (O, Cl) umgeben. Dabei weist La1 zwei Chlorid- und sieben Sauerstoff-, La2 dagegen nur einen Chlorid-, jedoch acht Sauerstoff-Liganden als nächste Nachbarn auf. Je vier der Sauerstoff-Liganden in der Koordinationssphäre des Lanthans stammen von einer „vierzähnigen“ Acetatgruppe, die übrigen von Hydratwasser-Molekülen. Die Acetatgruppen koordinieren sowohl am zentralen (chelatisierend) als auch zu den „rechts“ und „links“ benachbarten La3+-Kationen. Hierdurch entstehen eindimensional unendliche, kationische Ketten 1∞[La2Cl3(OAc)2(H2O)7]+, die in Richtung [011] verlaufen. Diese Ketten werden durch „einsame“ Chlorid-Ionen zusammengehalten, die ihrerseits von (4 + 1) Hydratwasser-Molekülen umgeben sind, zu denen Wasserstoffbrücken-Bindungen ausgebildet werden.
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    URL: http://dx.doi.org/10.1002/zaac.19915980127
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    Über EisengallustinteProfessor Hans-Georg von Schnering zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 598 (1991), S. 371-376 
    Details
    ISSN: 0044-2313
    Keywords: Iron gallic ink ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Iron Gallic InkFrom Iron(III) chloride and gallic acid in gels single crystals could be obtained which will be the dye-stuff of iron gallic ink. The structure consists of a hexagonal iron gallic acid 1:1 framework. The oxidation state three of the iron could be confirmed by Mössbauer and XANES spectroscopy.
    Notes: Durch Kristallisation in Gelen erhält man aus Gallussäure und Eisen(III)-chlorid Einkristalle, die einen der wesentlichen Farbstoffe der Eisengallustinte darstellen dürften. Die Struktur besteht aus einem hexagonalen Gallussäure-Eisen-1: 1-Gerüst, in dessen Kanälen Hydronium-Ionen den Ladungsausgleich bewirken. Die Oxidationsstufe drei des Eisens wurde mit Mössbauer- und XANES-Spektroskopie bestätigt.
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    URL: http://dx.doi.org/10.1002/zaac.19915980134
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    (NH4)3[Re3Cl12]: Synthese, Kristallstruktur und Thermolyse (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 604 (1991), S. 7-15 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium ; crystal structure ; thermolysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: (NH4)3[Re3Cl12]: Synthesis, Crystal Structure, and Thermolysis(NH4)3[Re3Cl12] may be obtained by reaction of ReCl3 with liquid ammonia and subsequent reaction of the solid product with hydrochloric acid solution or, less pure, directly from ReCl3 and NH4Cl in hydrochloric acid. The crystal structure (monoclinic, P21/m, Z = 2, a = 946.82(6), b = 1138.37(6), c = 912.30(4)pm, β = 93.840(5)°) contains the isolated building units [Re3Cl12]3-. The anions are connected via the NH4+ cations (symbolized by N1 and N2) that have coordination numbers of 10(N1) and 9(N2). Thermal decomposition was investigated by simultaneous DSC/TG-MS measurements. It leads, finally, to metallic rhenium and the gases HCL and N2, but consists of three steps at 320, 420 and 480°C, respectively, with (NH4)2[ReCl6] and ReCl3 as intermediate products.
    Notes: Bisher unbekanntes (NH4)3[Re3Cl12] erhält man durch Behandeln von ReCl3 mit fl. NH3 und anschließender Umsetzung des Reaktionsproduktes mit Salzsäure oder, weniger rein, direkt aus ReCl3 und NH4Cl in Salzsäure. In der Kristallstruktur (monoklin, P21/m, Z = 2; a = 946,82(6); b = 1138,37(6); c = 912,30(4) pm; β = 93,840(5)°) liegen isolierte Baueinheiten [Re3Cl12]3- vor. Die Anionen werden durch die Kationen NH4+ (repräsentiert durch N1 und N2) miteinander verknüpft, sie weisen Koordinationszahlen von 10 (N1) bzw. 9 (N2) auf. Der thermische Abbau wurde mittels simultaner DSC/TG-MS untersucht. Er führt letztlich zu metallischem Rhenium und den Gasen HCl und N2 und erfolgt in drei Stufen bei 320, 420 und 480°C, wobei als Zwischenprodukte (NH4)2[ReCl6] und ReCl3 auftreten.
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    URL: http://dx.doi.org/10.1002/zaac.19916040102
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    Synthese und Kristallstrukturen der methylsubstituierten Ammonium-μ-trichlorononachloro-trirhenate(III), (NH4-xMex)3 [Re3Cl12] (1 ≤ X ≤ 3) (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 604 (1991), S. 17-26 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium ; crystal structure ; syntheses ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structures of Methyl-Substituted Ammonium-μ-trichloro-nonachloro-trirhenates(III), (NH4-xMex)3[Re3Cl12] (1 ≤ x ≤ 3)The chlorides (NH3Me)3[Re3Cl12] (1), (NH2Me2)3[Re3Cl12] (2) and (NHMe3)3[Re3Cl12] (3) are obtained from the binary components, for example (NH3Me)Cl and ReCl3, by slow evaporation of the hydrochloric-acid solutions as brick red single crystals. The crystal structures were determined from four-circle diffractometer data.1:orthorhombic, Pnma, Z = 4; a = 1667.93(9); b = 1197.01(5); c = 1110.44(5) pm; R = 0,115; Rw = 0,062.2:monoklin, P21/n, Z = 4; a = 1563,03(12); b = 1648,73(10); c = 984,34(7) pm; β = 93,422(8)°; R = 0,054; Rw = 0,035.3:monoklin, P21/n, Z = 4; a = 1651,7; b = 1679,5; c = 1014,2pm; β = 90,3°; R = 0,107; Rw = 0,075.
    Notes: Die Chloride (NH3Me)3[Re3Cl12] (1), (NH2Me2)3[Re3Cl12] (2) und (NHMe3)3 [Re3Cl12] (3) erhält man aus den binären Komponenten, z. B. (NH3Me)Cl und ReCl3, beim langsamen Eindunsten der salzsauren Lösungen als ziegelrote Einkristalle. Die Kristallstrukturen wurden aus Vierkreis-Diffraktometer-Daten bestimmt.1:orthorhombisch, Pnma, Z = 4; a = 1667,93(9); b = 1197,01(5); c = 1110,44(5)pm; R = 0,115; Rw = 0,062.2:monoklin, P21/n, Z = 4; a = 1563,03(12); b = 1648,73(10); c = 984,34(7)pm; β = 93,422(8)°; R = 0,054; Rw = 0,035.3:monoklin, P21/n, Z = 4; a = 1651,7; b = 1679,5; c = 1014,2pm; β = 90,3°; R = 0,107; Rw = 0,075.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19916040103
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  • 95
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    (NMe4)[Re3Cl10(H2O)2] · 2H2)  -  Kein 5/3-Hydrat gemäß [Re3Cl9(H2O)3] · 2H2O (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 604 (1991), S. 27-33 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium ; crystal structure ; ir, nmr spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: (NMe4)[Re3Cl10(H2O)2] · 2H2O  -  not a 5/3-Hydrate according to [Re3Cl9(H2O)3] · 2H2ONew investigations of the so-called 5/3-hydrate, “[Re3Cl9(H2O)3] · 2H2O”, revealed that it is in fact (NMe4)[Re3Cl10(H2O)2] · 2HO. Low temperature (173 K) single crystal diffractometry confirms the main features of the previously determined crystal structure (hexagonal, P62c, No. 190; a = 937.3(2), c = 1461.2(3) pm; z = 2; Vm = 334.8 cm3/mol; R = 0.030, Rw = 0.022). There are, however, two important differences. First, the channels in the [00.1] direction contain cations NMe4+.These are disordered in a way that their orientation is “up and down” parallel to [00.1]. Infrared and solid-state 13C-NMR spectra confirm the appearance of the NMe4+ cation. Secondly, the in plane, terminal (i, t) positions at the Re3 triangle are not occupied by H2O ligands alone. Rather, the anion [Re3Cl10(H2O)2]- occurs, with statistical distribution of two water molecules (dRe—o = 224(2) pm) and one chloride ion (dRe—cl = 248(1) pm) over the three i,t positions.
    Notes: Neue Untersuchungen an dem als 5/3-Hydrat beschriebenen „[Re3Cl9(H2O)3] · 2H2O“ ergaben, daß es sich hierbei um (NMe4) [Re3Cl10(H2O)2] · 2H2O handelt. Tieftemperaturmessungen (173 K) am Einkristall bestätigen weitgehend die früher bestimmte Kristallstruktur (hexagonal. P62c, Nr. 190; a = 937,3(2), c = 1461,2(3) pm; Z = 2; Vm = 334,8 cm3/mol; R = 0,030; Rw = 0,022). Es bestehen jedoch zwei wichtige Unterschiede: In den Kanälen längs [00.1] befinden sich die Kationen NMe4+; sie sind derart fehlgeordnet, daß die Spitzen der Tetraeder in und gegen Richtung [00.1] orientiert sind. IR- und Festkörper-13C-NMR-Spektrum sind im Einklang mit der Erwartung für das Kation NMe4+. Die in plane, terminal-(i,t)-Positionen am Re3-Ring sind nicht mit drei Wassermolekülen besetzt: Es liegt vielmehr die Baugruppe [Re3Cl10(H2O)2]- vor, mit statistischer Verteilung von zwei Koordinationswasser (dRe—o = 224(2)pm) und einem Chlorid-Ion (dRe—cl = 248(1) pm) auf den drei i,t-Positionen.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916040104
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  • 96
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    Synthese und Strukturen von achtgliedrigen Bor- und Germanium-haltigen Siloxanringen und eines Bicycloheptanderivats mit Silicium, Zinn und Sauerstoff als RingbausteinenProfessor Joseph Heubel zum 70. Geburtstag gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 604 (1991), S. 93-103 
    Details
    ISSN: 0044-2313
    Keywords: Boron ; germanium ; eight-membered siloxane rings ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structures of Boron and Germanium containing eight-membered Siloxane Rings and of a Bicycloheptane Derivative with Silicon, Tin, and Oxygen as Building Units of the Ring SystemThe reaction of (t-Bu)2Si(OH)2 with PhBCl2 and GeCl4, respectively, leads in a molar ratio of 1:1 to the formation of 1,3,5,7-tetraoxa-2,6-disila-4,8-diborocine 1 and 1,3,5,7-tetraoxa-2,6-disila-4,8-digermocine 2. μ-O—O′-Di(t-butyl) silandiyl-dihydroxo-di-μ-hydroxo-hexachloro-distannane 3 has been synthesized by treatment of SnCl4 with (t-Bu)2Si(OH)2 in CH2Cl2. The X-ray structure analyses of 1 and 2 exhibit eight-membered rings containing silicon, boron, oxygen and silicon, germanium, oxygen. 1 and 2 crystallize in the triclinic space group P1 with a = 8.727(2), b = 9.523(3), c = 9.816(4) Å; α = 91.81(2), β = 100.76(3), γ = 116.90(1)° and a = 8.297(2), b = 9.325(2), c = 10.900(2) Å; α = 72.36(1), β = 77.48(1), γ = 88.31(1)°. The X-ray structure analysis of 3 exhibits a [3.1.1] bicycloheptane analogue structure. 3 crystallizes in the monoclinic space group P21/c with a = 15.185(3), b = 14.302(3), c = 22.825(5) Å; β = 90.84(3)°.
    Notes: Die Reaktionen von (t-Bu)2Si(OH)2 mit PhBCl2 und GeCl4 führen im molaren Verhältnis 1:1 zur Bildung von 1,3,5,7-Tetraoxa-2,6-disila-4,8-diborocin 1 und 1,3,5,7-Tetraoxa-2,6-disila-4,8-digermocin 2. Durch Umsetzung von SnCl4 mit (t-Bu)2Si(OH)2 in CH2Cl2 wurde μ-O—O′-Di(t-butyl) silandiyl-dihydroxo-di-μ-hydroxo-hexachlorodistannan 3 dargestellt. Die Röntgenstrukturanalysen von 1 und 2 zeigen das Vorliegen achtgliedriger Bor- und Germanium-Silicium-Sauerstoff-Ringe. 1 und 2 kristallisieren in der triklinen Raumgruppe P1 mit a = 8,727(2), b = 9,523(3), c = 9,816(4) Å; α = 91,81(2), β = 100,76(3), γ = 116,90(1)° und a = 8,297(2), b = 9,325(2), c = 10,900(2) Å; α = 72,36(1), β = 77,48(1), γ = 88,31(1)°. Die Röntgenstrukturanalyse von 3 zeigt einen [3.1.1] bicycloheptanartigen Aufbau. 3 kristallisiert in der monoklinen Raumgruppe P21/c mit a = 15,185(3), b = 14,302(3), c = 22,825(5) Å; β = 90,84(3)°.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916040113
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  • 97
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    Phasenübergang von DecamethylmanganocenProfessor Kurt Dehnicke zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 595 (1991), S. 27-34 
    Details
    ISSN: 0044-2313
    Keywords: Decamethylmanganocene ; phase transition ; crystal structure ; DSC thermogram ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phase Transition of DecamethylmanganoceneDecamethylmanganocene (Cp2*Mn) has been investigated X-ray structural analytically at 240, 225, and 125 K, to study a reversible phase transition between 255 and 238 K (DSC thermogram). At 240 K the same space group C2/c is observed as at room temperature [9], whereas after the phase transition at 225 and 125 K the space group Cmca is found. In both phases the Cp* rings are staggered and slightly slipped, but less at 225 and 125 K compared with 240 K.The phase transition is to be traced back to a change of the molecule packing in the crystal lattice: With decreasing temperature the molecules cannot be packed closer in the monoclinic phase (C2/c), because the intermolecular H … H distances already remained under the sum of the van der Waals radii. In the orthorhombic phase (Cmca) (elongation of the a-axis and contraction of the b-axis) the repulsion along the b-axis is avoided.
    Notes: Decamethylmanganocen (Cp2*Mn) wurde bei 240, 225 und 125 K röntgenstrukturanalytisch untersucht, um einen zwischen 240 und 225 K stattfindenden reversiblen Phasenübergang (DSC-Thermogramm) zu untersuchen. Bei 240 K wird dieselbe Raumgruppe C2/c beobachtet wie bei Raumtemperatur [9], während nach dem Phasenübergang bei 225 und 125 K die Raumgruppe Cmca gefunden wird. In beiden Phasen sind die Cp*-Ringe gestaffelt und leicht gegeneinander verschoben angeordnet, jedoch bei 225 und 125 K weniger als bei 240 K. Der Phasenübergang ist auf eine Packungsänderung der Moleküle im Kristallgitter zurückzuführen: Mit abnehmender Temperatur können die Moleküle in der monoklinen Phase (C2/c) sich nicht mehr dichter packen, da die intermolekularen H … H-Abstände bereits die Summe der van der Waals-Radien unterschritten haben. In der orthorhombischen Phase (Cmca) (Verlängerung der a-Achse und Kontraktion der b-Achse) wird die Repulsion entlang der b-Achse vermieden.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915950105
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    Ein metallsubstituiertes Cyclotriphosphan [(η5-C5Me5)(Co)2Fe—P]3 als terminaler η2-Ligand in Chrom-und Molybdäntetracarbonyl-Komplexen (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 605 (1991), S. 87-99 
    Details
    ISSN: 0044-2313
    Keywords: Chromium, molybdenum complexes ; metal-substituted cyclotriphane ligand ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Metal-Substituted Cyclotriphosphane [(η5-C5Me5)(CO)2Fe—P]3 as Terminal η2-Ligand in Chromium and Molybdenum Tetracarbonyl ComplexesThe transition metal-substituted cyclotriphosphane [(η5-C5Me5)(CO)2Fe - P]3 reacts with (norbornadiene)M(CO)4 (M = Cr, Mo) to give monomeric complexes of the composition η2-[(η5-C5Me5)(CO)2Fe—P]3M(CO)4. The molecular structure of 2 is elucidated by X-ray analysis. The skeleton of the molecule consists of a P3 triangle with one trans and two cis-located Fe(CO)2(C5Me5) substituents. Both cis-configurated phosphorus atoms of the triangle are coordinated to a Cr(CO)4 fragment. The bond distance between the two cis orientated phosphorus atoms [2.191(5) and 2.183(6) Å] is slightly shorter with respect to the other P—P bonds [2.206(5), 2.217(5) and 2.214(5), 2.211(5) Å, respectively]. The cyclotriphosphane unit and the triangle defined by two phosphorus atoms and the metal atom enclose a dihedral angle of 44.8° and 43.4°, respectively. The Cr(CO)4 group is severely distorted by interactions with the cis-oriented (η5-C5Me5)(CO)2Fe substituent at P(3).
    Notes: Bei der Umsetzung des übergangsmetallsubstituierten Cyclotriphosphans [(η5-C5Me5)(CO)2Fe-P]3 (1) mit (Norbornadien)M(CO)4 (M = Cr, Mo) werden monomere Komplexe der Zusammensetzung η2-[(η2-C5Me5)Fe-P]3M(CO)4 (2: M = Cr; 3: M = Mo) erhalten. Die Struktur von 2 wurde durch Röntgenbeugungsanalyse bestimmt. Das Grundgerüst des Moleküls besteht aus einem Dreieck aus Phosphoratomen mit zwei cis- und einem trans-ständigen Fe(CO)2(C5Me5)-Substituenten. Die beiden cis-konfigurierten P-Atome des Dreiringes sind an ein Cr(CO)4-Fragment koordiniert. Dabei ist ihr Abstand [2, 191 (5) und 2,183(6) Å] gegenüber den beiden anderen P-P-Bindungen [2,206(5) und 2,217(5) bzw. 2,214(5) Å] geringfügig verkürzt. Die P3-Einheit und das P2Cr-Dreieck schließen einen Diederwinkel von 44,8° bzw. 43,4° ein. Aufgrund sterischer Wechselwirkungen mit dem cis-orientierten (η5-C5Me5)(CO)2FE-Substituenten an P(3) ist das Cr(CO)4-Fragment stark verzerrt.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916050110
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    Structural investigations of two 2-amino-5-nitropyridinium Salts: C5H6N3O2+NO3- and (C5H6N3O2+)2CuCl42- (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 606 (1991), S. 59-71 
    Details
    ISSN: 0044-2313
    Keywords: 2-Amino-5-nitropyridinium salts ; preparation ; crystal structure ; polar nonpolar packing ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kristallstruktur-Untersuchungen an zwei 2-Amino-5-nitropyridinium-Salzen: C5H6N3O2+NO3- und (C5H6N3O2+)2CuCl42-Am Beispiel der Darstellung und Kristallstrukturuntersuchung des 2-Amino-5-nitropyridinnitrats und des 2-Amino-5-nitropyridin-tetrachlorocuprats wird gezeigt, daß sich diese polaren Kristalle aus 2-Amino-5-nitropyridin-Kationen und anorganischen Anionen züchten lassen. Der Einfluß der Größe und der Ladung des Anions auf die Ausbildung der zentrosymmetrischen Packung wird diskutiert. In den Tetrachlorocupraten liegen tetraedrisch verzerrte CuCl42--Anionen mit D2d-Symmetrie vor. Die Kristallstruktur von C5H6N3O2+NO3-(P21/n; a = 13,672(3), b = 7,762(1), c = 7,577(1) Å, β = 101,45(5)°, Z = 4, dx = 1,703) wurde mit Hilfe von 1 386 Röntgenreflexen bis zum R-Wert von 0,044 bestimmt. Die Kristallstruktur von (C5H6N3O2+)2CuCl42- (P21/c; a = 7,701(3), b = 31,99(5), c = 7,107(3) Å, β = 92,65(5)°, Z = 4, dx = 1,844) wurde mit Hilfe von 3 367 Röntgenreflexen bis zu einem R-Wert von 0,039 bestimmt.
    Notes: Through chemical preparations and crystal structures of the 2-amino-5-nitropyridinium nitrate and the bis(2-amino-5-nitropyridinium)tetrachlorocuprate, an attempt at polar crystal engineering using the 2-amino-5-nitropyridinium cation and inorganic counter anions is illustrated. The role of the ratio of anion charge to dimension in the building of centric packings is illustrated and discussed. In the tetrachlorocuprate salt, distorted CuCl42- tetrahedral anions of D2d symmetry are present. C5H6N3O2+NO3- is monoclinic, P21/n, with a = 13.672(3), b = 7.762(1), c = 7.577(1) Å, β = 101.45(5)°, Z = 4, dx = 1.703. The crystal structure has been solved using 1 386 independent reflections with a final R value of 0.044. (C5H6N3O2+)2CuCl42- is monoclinic, P21/c, with a = 7.701(3), b = 31.99(5), c = 7.107(3) Å, β = 92.65(5)°, Z = 4, dx = 1.844. The crystal structure has been solved using 3 367 independent reflections with a reliability factor of 0.039.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916060106
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