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  • Inorganic Chemistry  (11)
  • Wiley-Blackwell  (11)
  • American Association for the Advancement of Science (AAAS)
  • American Geophysical Union
  • PANGAEA
  • 1990-1994  (11)
  • 1993  (11)
Collection
Publisher
  • Wiley-Blackwell  (11)
  • American Association for the Advancement of Science (AAAS)
  • American Geophysical Union
  • PANGAEA
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  • 1990-1994  (11)
Year
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 587-592 
    ISSN: 0044-2313
    Keywords: Lanthanoid-nickel phosphides ; 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 La2Ni12P5 und isotypen ternären Lanthanoid-Nickel-PhosphidenDas neue ternäre Phosphid La2Ni12P5 wurde durch Aufschmelzen reiner Komponenten in einem Lichtbogenofen synthetisiert und seine Kristallstruktur durch Einkristalldaten belegt. La2Ni12P5 ist ein erster Vertreter eines neuen Strukturtyps: Raumgruppe P21/m, a = 10,911(3), b = 3,696(2), c = 13,174(4) Å, β = 108,02(2)°, V = 505,2(6) Å3, Z = 2. Die Lageparameter wurden “anisotrop” aus 1 284 Io(hkl) zu RF = 0,0278, RW = 0,0287 (I 〉 3s̰I; 116 Parameter) verfeinert. Charakteristisch für den Aufbau ist die trigonal-prismatische Koordination der Phosphoratome. Die isotypen Phosphide Ln2Ni12P5 (Ln = Ce, Pr, Nd und Eu) wurden ebenfalls dargestellt und durch Pulverdaten charakterisiert.
    Notes: The new ternary phosphide La2Ni12P5 has been prepared by direct arc melting of the components as pure metals and red phosphorus. The crystal structure has been determined using X-ray single crystal diffraction data. The compound exhibits a new type of crystal structure, P21/m with lattice parameters a = 10.911(3), b = 3.696(2), c = 13.174(4) Å, β = 108.02(2)°, V = 505,2(6) Å3, Z = 2. Atomic parameters least squares refinement of 116 independent variables (anisotropic approximation for thermal vibrations) employed 1 284 independent Io(hkl); RF = 0.0278 and RW = 0.0287. The crystal structure is characterized by trigonal prismatic arrangement of phosphorus atoms stacking variant of infinite (with phosphorus centered) columns built by metal trigonal prisms ‖ [010]. Two or three such columns are connected through common edges (lanthanum atoms). The compounds RE2Ni12P5 (where RE = Ce, Pr, Nd and Eu) display the same with La2Ni12P5 crystal structure. Lattice parameters of these compounds have been refined using powder diffraction data.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 889-892 
    ISSN: 0044-2313
    Keywords: Calcium ; lanthanum ; aluminium ; gallium ; oxide ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Crystal Structure of CaLaAl3O7 and CaLaGa3-xAlxO7 (x = 0.66)Single crystals of (I): CaLaAl3O7 and (II): CaLaGa2.34Al0.66O7 were grown from molten oxide mixtures and investigated by single crystal X-ray technique. Both compounds crystallize with tetragonal symmetry, space group D2d3—P421m, (I): a = 7.8075; c = 5.1564 Å, (II): a = 7.9130, c = 5.2360 Å, Z = 2 and are isostructural with the Melilites. The crystal structure is discussed.
    Notes: Einkristalle von (I): CaLaAl3O7 und (II): CaLaGa2,34Al0,66O7 wurden aus Schmelzen der Oxidgemenge dargestellt und mit röntgenographischen Methoden untersucht. Beide Oxide kristallisieren tetragonal in der Raumgruppe D2d3—P421m mit (I): a = 7,8075; c = 5,1564 Å, (II): a = 7,9130, c = 5,2360 Å, Z = 2 und sind isotyp mit den Meliliten. Die Kristallstruktur wird diskutiert.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 499-502 
    ISSN: 0009-2940
    Keywords: Iodocarbene, addition to alkenes ; endo1-Selectivity ; Cyclooctadiene ; Cyclooctatetraene ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: New Observations Concerning the Stereoselectivity of Monoiodocarbene AdditionsContrary to our earlier claim, CHI gives endo/exo isomer mixtures with cyclooctene. However, only endo1-iodo compounds 7, 8, 10-12 are obtained from COD and COT. Tricyclic compound 7 rearranges partially to bicyclic 9, X-ray structure determinations of 7 and 9 were performed.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 2379-2382 
    ISSN: 0009-2940
    Keywords: Steric overcrowding ; Trisphosphane, linear, bismethylene-bridged ; Molybdenum, complexes with bis- and trisphosphanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Bis[(di-tert-butylphosphanyl)methyl]methylphosphane[1]The synthesis of [(di-tert-butylphosphanyl)methyl]dimethyl-phosphane (3) and of the title compound 5 is described. 5 reacts with sulfur to form the trisulfide 6. Both 3 and 5 behave as bidentate ligands in forming the molybdenum complexes 8 and 10, which are characterized by single crystal X-ray structure determinations. 10 reacts with sulfur to yield the sulfide 11, which decomposes in solution within 6 h.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 2759-2763 
    ISSN: 0009-2940
    Keywords: Dichloroketene ; Stereoselective ketone reduction ; Mitsunobu reaction ; Cyclobutyl bromides ; Cross-coupling reaction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Stereoselective Synthesis of 3-Substituted Cyclobutanols and Products Derived Therefrom3-Substituted cyclobutanones 2 are prepared by alkene/dichloroketene cycloadditions and subsequent dehalogenation. Reduction with LiAlH(OtBu)3 furnishes cis-cyclobutanols 3 in 95-100% selectivity. Mitsunobu inversion turned out to be the only practical method to get trans isomers 4 in high selectivity. A stereoselective cyclobutanol→bromocyclobutane conversion could be achieved only by a modified Mitsunobu reaction. Cross coupling between zinc derivatives of bromocyclobutanes 9 and aromatic bromides is not stereoselective.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 2765-2766 
    ISSN: 0009-2940
    Keywords: O-/C-Alkylation ; Phase transfer catalysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Applications of Phase Transfer Catalysis, 61[1]. - Directing Effects on O- vs. C-Alkylations by Phase Transfer CatalystsStrong catalyst effects on the O- vs. C-alkylation ratio of 1,1-dimethylindan-2-one (4) by dimethyl sulfate are found. They differ in the two consecutive alkylation steps and range between 〈1 and ≈60. No such catalyst influence exists in the methylation of 2-methylindane-1,3-dione (1).
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 641-651 
    ISSN: 0044-2313
    Keywords: 1,3-Di-tert-butyl-2,2-dimethyl-4-azido-4-R- 1,3,2,4-diazasilagermaetidines (R = organic group, amine or azide); reactions with germylenes ; trapping of germa-imines ; insertion of Ge=N into C-H bonds ; NMR ; x-ray structure analyses ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of a Cyclic Bis(amino)germylene with Germaniumazides: Trapping-Reactions of Unstable Germa-Imines.The cyclic bis(amino)germylene 1 reacts with different germaniumazides of the type Me2Si(NtBu)2Ge(R)N3 (R = Me (2), tBu (3), N(SiMe3)2 (4), R = N3 (5)). With the exception of 4 all azides lose dinitrogen when treated with 1 and the GeII center coordinates the α-nitrogen of the azide group. It seems to be reasonable to assume a transient germaimine (nitride) which is trapped by further reaction with the azide molecules 2 and 5 or by reaction with the solvent pyridine (3). In the case of 2 the germatetrazole [Me2Si(NtBu)2]GeN4[Ge(NtBu)2SiMe2]2 (6) is formed, the tetrazole nitrogens being exclusively substituted by germanium atoms (point symmetry of the molecule Cs(m)). When 1 is treated with 5 a tris(germa)amine [Me2Si(NtBu)2Ge(N3)]3N (8) is formed, which has an azide group attached to each Ge-atom. X-ray analysis reveals that the nine nitrogen atoms of the azide groups are coplanar with the trigonal planar Ge3N moiety (crystallographic symmetry: 3/m). The reaction of 1 with 3 is very surprising: the pyridine in the product Me2Si(NtBu)2Ge(C5H4N)—N(H)Ge(tBu)(NtBu)2SiMe2 (7) is bonded via an α-carbon atom while the remaining hydrogen has added to the nitride-nitrogen. 6 crystallizes in the monoclinic system space group C2/m, a = 24.306(9), b = 10.933(6), c = 19.420(9) Å, β = 91.81(2)° and Z = 4. 7 crystallizes in the hexagonal system space group P63/m with a = b = 16.73(1), c = 11.006(8) Å, γ = 120° and Z = 2, and 8 crystallizes in the monoclinic system space group P21/n, a = 11.341(6), b = 26.086(9), c = 13.244(7) Å, β = 98. I2(2)° mit Z = 4.
    Notes: Das cyclische Bis(amino)germylen 1 wurde mit verschiedenen Germaniumaziden Me2Si(NtBu)2GeR(N3) (R = Me (2), tBu (3), N(SiMe3)2 (4), N3 (5)) umgesetzt. Außer 4 reagieren alle Azide mit dem Germylen 1 unter Distickstoffentwicklung und gleichzeitigem Angriff des GeII-Zentrums auf den α-Stickstoff einer Azidgruppe. Das sich offenbar zwischenzeitlich bildende Germaimin (bzw. Germanitrid) wird durch weitere Reaktion mit der Azidkomponente (2 und 5) bzw. mit dem Lösungsmittel Pyridin abgefangen. Im Falle der Reaktion mit 2 bildet sich ein Germatetrazol [Me2Si(NtBu)2]GeN4[Ge(Me)(NtBu)2SiMe2]2 (6), dessen Stickstoffatome ausschließlich durch Germaniumatome substituiert sind (Punktsymmetrie Cs(m)). Bei der Reaktion mit 5 entsteht ein Tris(germa)amin [Me2Si(NtBu)2Ge(N3)]3N (7), das an jedem Germaniumatom noch jeweils eine Azidgruppe gebunden hat. Nach Röntgenstrukturanalyse befinden sich neben der trigonal planaren Ge3N-Einheit noch die 9 Stickstoffatome der Azidgruppen in der Molekülebene (kristallographische 3/m Symmetrie). Besonders überraschend ist die Reaktion von 1 mit 3 in Pyridin: im Produkt Me2Si(NtBu)2Ge(C5H4N)N(H)Ge(tBu)(NtBu)2SiMe2 (8) ist der Pyridinrest über das α-Kohlenstoffatom an das Germanium gebunden, während das verbleibende Wasserstoffatom sich an den Nitrid-Stickstoff addiert hat. 6 kristallisiert monoklin in C2/m mit a = 24,306(9), b = 10,933(6), c = 19,420(9) Å, β = 91,81(2)° mit Z = 4, 7 kristallisiert hexagonal in P63/m mit a = b = 16,73(1), c = 11,006(6) Å, γ = 120° mit Z = 2, und 8 kristallisiert monoklin in P21/n mit a = 11,341(6), b = 26,086(9), c = 13,244(7) Å, β = 98,12(2)° mit Z = 4.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1909-1919 
    ISSN: 0044-2313
    Keywords: Sodium iron fluoride ; weberite structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Struktur von Na2Fe2F7 und Strukturbeziehungen in der Weberitfamilie Na2MIIMIIIF7Die gemischtvalente Verbindung Na2Fe2F7 kristallisiert im monoklinen Weberit-Typ von Na2CuFeF7-II (M-II), Raumgruppe C2/c, Z = 16, a = 12,676, b = 7,422, c = 24,710 Å, β = 99,97°. Die Verfeinerung mit F2-Daten ergab wR(F2) = 0,117 für alle 2 645 Reflexe, R = 0,057 für 1 258 Reflexe mit Fo 〉 4σ(F). Auf der Grundlage dieser und anderer neuer Einkristalluntersuchungen werden die Strukturen der Weberite Na2MIIMIIIF7 in vier Haupttypen eingeteilt: O-I ist der „klassische“ orthorhombische Weberit (RG Imma), wie er im Mineral Na2MgAlF7 auftritt, und von dem sich zwei niedriger symmetrische Varianten, O-II (Na2CuCrF7-Typ) und O-III (Na2NiInF7), ableiten. Der zweite M-I und dritte M-II Typ sind monoklin (z. B. Na2CuFeF7-I and -II), der vierte Typ T ist trigonal (Na2MnFeF7). Die strukturellen Verwandtschaften innerhalb der Weberitfamilie werden diskutiert und die Zusammenhänge aufgezeigt, die es erlauben, diese Weberite ebenso wie die Pyrochlore als Subtraktionsabkömmlinge des Fluorittyps zu betrachten.
    Notes: The mixed valence compound Na2Fe2F7 crystallizes in the monoclinic weberite structure of the Na2CuFeF7-II type (M-II), space group C2/c, Z = 16, a = 12.676, b = 7.422, c = 24.710 Å, β = 99.97°. Refinement on F2 led to wR(F2) = 0.117 for all 2 645 reflections, R = 0.057 for 1 258 refl. with Fo 〉 4σ(F). On the basis of this and other recent single crystal investigations the structures of weberites Na2MIIMIIIF7 are classified in four main structure types: O-I is the ‘classical’ orthorhombic weberite type (S.G. Imma) encountered e.g. in the mineral Na2MgAlF7, from which two lower symmetric variants O-II (Na2CuCrF7 type) and O-III (Na2NiInF7) are deriving. The second M-I and third M-II basic type are monoclinic (e. g. Na2CuFeF7-I and -II), the fourth type T is trigonal (Na2MnFeF7). The structural relations within the weberite family are discussed and the connections established, which allow to regard these weberites as well as the pyrochlores as subtraction derivatives of the fluorite type.
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1927-1930 
    ISSN: 0044-2313
    Keywords: Metallocene dihalides ; titanocene dibromide ; X-ray analysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Molekular- und Kristallstruktur von Bis(η5-cyclopentadienyl)titan(IV)-dibromidDie Molecular- und Kristallstruktur von Bis(η5-cyclopentadienyl)titan(IV)-dibromid wurde durch Röntgenstrukturanalyse bestimmt. Kristalldaten: Triklin, Raumgruppe P1, a = 7,872(5), b = 11,807(5), c = 12,310(3) Å, α = 107,62(3), β = 100,83(4), γ = 90,69(4)°, V = 1 068(14) Å3, T = 293, Z = 4 (mit zwei kristallographisch unabhängigen Molekülen in der Elementarzelle und ähnlicher Konformation). Abschließende R-Werte: R = 0,068 und Rw = 0,073. Die Strukturergebnisse werden mit denen analoger Verbindungen verglichen.
    Notes: The crystal and molecular structure of Bis(η5-cyclopentadienyl)titanium(IV) dibromide, Ti(η5-C5H5)2Br2, has been investigated by an X-ray structure determination. Crystal data: triclinic, a = 7.872(5), b = 11.807(5), c = 12.310(3) Å, α = 107.62(3), β = 100.83(4), γ = 90.69(4)°, V = 1 068(14) Å3, T = 293, space group P1, Z = 4 (there are two crystallographically independent molecules in the asymmetric unit cell and their conformations are similar). Final R and Rw values are 0.068 and 0.073, respectively. The structural results are compared to those for similar type molecules.
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  • 10
    ISSN: 0044-2313
    Keywords: Molybdenum / tungsten complexes ; pyridinium molybdenum / tungsten tetrabromine complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kristallstruktur von trans-pyH[MoBr4py2] und die Reaktivität von trans-pyH[MBr4py2] (M = Mo, W; py = Pyridin) gegenüber Stickstoff-Liganden und zur Oxidation mit Brom.Die Kristallstruktur von trans-pyH[MoBr4py2] wurde bestimmt: orthorhombisch, Pnma (No. 62), a = 16,197(3), b = 13,995(3), c = 8,615(1) Å, Z = 4, Dgemess. = 2,20(3), Dröntg. = 2,23 g/cm3, V = 1953(1) Å3. R1, Rw = 0,057 and 0,053. Trans-[MoBr4py2]-, mit der gestaffelten Konformation der Pyridin-Liganden in der Spiegelebene. Mo—Br- und Mo—N(Pyridin)-Abstände sind 2,593(1), 2,573(1), 2,227(8) und 2,213(7) Å. Die Kationen befinden sich in den Symmetriezentren.Das Kation in trans-pyH[MBr4py2] ist ersetzbar; trans-NH4[MBr4py2] · H2O, Cs[MBr4py2], LH[MBr4py2] (M = Mo, W; L = 4-Methylpyridin, 4-pic; 2,2′-Bipyridyl, bipy) wurden dargestellt. Die Molybdän- und Wolfram-Verbindungen analoger Zusammensetzung sind isostrukturell. Alle Stoffe reagieren mit Pyridin und 4-Methyl-pyridin zu trans-MBr3L3 und im Fall des Molybdäns auch zu trans-MoBr3py2(4-pic). Brom oxidiert trans-MI[MBr4py2] zu trans-MBr4py2.
    Notes: The crystal structure of trans-pyH[MoBr4py2] has been determined: orthorhombic, Pnma (No. 62), a = 16.197(3), b = 13.995(3), c = 8.615(1) Å, Z = 4, Dc = 2.23, Do = 2.20(3) g/cm3, V = 1 953(1) Å3. R1, Rw = 0.057 and 0.053. Trans-[MoBr4py2]- anions with staggered conformation of pyridine rings are located on the mirror planes. Mo—Br, Mo—N(pyridine) distances are 2.593(1), 2.573(1), 2.227(8) and 2.213(7) Å. Cations are located on the symmetry centers.The cation in trans-pyH[MBr4py2] can be replaced. Trans-NH4[MBr4py2] · H2O, Cs[MBr4py2], LH[MBr4py2] (M = Mo, W; L = 4-methylpyridine, 4-pic; 2,2′-bipyridyl, bipy) were prepared. The compounds of molybdenum and tungsten with the same chemical composition are isostructural. All compounds react with pyridine and 4-methylpyridine. The products are trans-MBr3L3, and in the case of molybdenum, also trans-MoBr3py2(4-pic). Bromine oxidizes trans-MI[MBr4py2] to trans-MBr4py2.
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