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  • 1990-1994  (24)
  • 1930-1934
  • 1994  (24)
  • Inorganic Chemistry  (24)
  • 1
    Electronic Resource
    Electronic Resource
    Wanzlick-Carbene in der [4 + 1]-Cycloaddition mit Bis(methylthio)- und Bis(trifluormethyl)-1,2,4,5-tetrazin (1994)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 127 (1994), S. 1803-1806 
    Details
    ISSN: 0009-2940
    Keywords: Singlet carbenes ; [4 + 1] Cycloadditions ; 1,2,4,5-Tetrazines ; SEAr reactions, intramolecular ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Wanzlick Carbenes in the [4 + 1] Cycloaddition Reaction with Bis(methylthio)- and Bis(trifluoromethyl)-1,2,4,5-tetrazineThe 3,6-disubstituted 1,2,4,5-tetrazines 3 and 4 have been submitted to a [4 + 1] cycloaddition reaction with the nucleophilic singlet carbenes (Wanzlick carbenes) 2a-d, which are generated from the precursors 1a-d. With 3 as diazadiene the expected spiro compounds 6a-d are formed. In contrast to this presumed two-step reaction sequence of 3, with the tetrazine 4 the cascade cycloaddition/cycloelimination is surprisingly followed by an intramolecular electrophilic aromatic substitution to yield the chiral tetracyclic compounds of type 8 with high diastereoselectivity. The crystal structure of 8d has been determined by X-ray diffraction methods.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19941270933
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  • 2
    Electronic Resource
    Electronic Resource
    Face-Selective and endo-Selective Cycloadditions with Enantiomerically Pure Cyclopentadienes (1994)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 127 (1994), S. 2505-2509 
    Details
    ISSN: 0009-2940
    Keywords: Cyclopentadienes, bicyclic ; Face selectivity ; endo selectivity ; Chiral discrimination ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A general synthetic route to the enantiopure bicyclic cyclopentadienes (S)-3 and (R)-3 of the hydrindane series, starting from the Hajos-Wiechert ketone 4 or its enantiomer is described. Reasons for the excellent face and endo selectivity of cycloadditions and the resulting consequences for chiral recognition are discussed.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19941271223
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  • 3
    Electronic Resource
    Electronic Resource
    Reaktion von Decaboran mit dem Phosphaalkin PCtBu (1994)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 127 (1994), S. 93-95 
    Details
    ISSN: 0009-2940
    Keywords: Decaborane ; 1-Phosphabutin, 3,3-dimethyl ; Bis(decaboranyl)methane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reaction of Decaborane with the Phosphaalkyne PC tBuThe borane B10H12(SMe2)2 (1) reacts with the phosphaalkyne P°CtBu to form the product [B10H11(SMe2)][C(tBu)-PH](B10H12) (2), in which two B10 units are linked by a HP-CtBu bridge. The B10 unit B is simply bound to the bridge C atom, whereas the B10 unit A is bound to both bridging atoms, P and C, by atom B6 and, moreover, to the P atom by atom B5. The solvate complex 2 · CH2Cl2 crystallizes in the space group P¯.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19941270115
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  • 4
    Electronic Resource
    Electronic Resource
    Zur Thermolyse von Amin - arachno-Nonaboran (1994)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 127 (1994), S. 853-855 
    Details
    ISSN: 0009-2940
    Keywords: Diethylamine - arachno-nonaborane ; Diethylamine - octadecaborane ; conjuncto-Bis[6′5′:5,6]decaborane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: On the Thermolysis of Amine-arachno-NonaboraneTwo molecules of diethylamine-arachno-nonaborane, B9H13-(NHEt2), undergo a condensation at 140°C to give diethylamine-conjuncto-bis[6′,5′:5,6]decaborane, B18H20(NHEt2) (4). The deprotonation of 4 yields the anion [B18H19(NHEt2)]-which can be crystallized with the cation [NEt3(CH2Ph)]+ (space group P1).
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19941270512
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  • 5
    Electronic Resource
    Electronic Resource
    Cs4[Sc6C]Cl13 und Cs4[Pr6(C2)]I13  -  zwei Beispiele für das fehlende Bindeglied bei der Verknüpfung der Baueinheiten [M6Z]X12iX6aProfessor Horst Sabrowsky zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1521-1526 
    Details
    ISSN: 0044-2313
    Keywords: Rare Earth Elements ; Halides ; Clusters ; Cesium Scandium Chloride Carbide ; Cesium Praseodymium Iodide Dicarbide ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cs4[Sc6C]Cl13 and Cs4[Pr6(C2)]I13  -  Two Examples for the Missing Link in the Connectivity of [M6Z]X12iX6a Building UnitsCs4[Sc6C]Cl13 (tetragonal, I41/amd, a = 1 540.5(4), c = 1 017.9(7) pm, c/a = 0.661, Z = 4, R = 0.038, Rw = 0.026) and Cs4[Pr6(C2)]I13 (a = 1 804.9(3), c = 1 259.5(3) pm, c/a = 0.698, R = 0.106, Rw = 0.068) are obtained as green-black and blue-black single crystals with brass-like metallic lustre through metallothermic reduction of ScCl3 and PrI3, respectively, with cesium in the presence of carbon in sealed tantalum containers. The, overall, isotypic compounds contain isolated [Sc6C] and [Pr6(C2)] clusters, respectively, that are surrounded by 18 halide (X) ligands (12 Xi and 6 Xa; X = Cl or I). The connection is carried out via the motif [M6Z]X8iX4/21-aX4/2a-1X2/2a-a (M = Sc and Pr; Z = C and C2, respectively) and is thereby the missing link of the motifs of connection for the composition Ax[M6Z]X13. Analogous interconnection of [TiO6] octahedra is found in the anatase-type of structure of TiO2.
    Notes: Cs4[Sc6C]Cl13 (tetragonal, I41/amd; a = 1 540,5(4); c = 1 017,9(7) pm; c/a = 0,661; Z = 4; R = 0,038; Rw = 0,026 und Cs4[Pr6(C2)]I13 (a = 1 804,9(3); c = 1 259,5(3) pm; c/a = 0,698; R = 0,106; Rw = 0,068) werden bei der metallothermischen Reduktion von ScCl3 bzw. PrI3 mit Caesium in Gegenwart von Kohlenstoff in verschweißten Tantalampullen in Form von grünschwarzen bzw. blauschwarzen, messingglänzenden Einkristallen erhalten. Die weitgehend isotypen Kristallstrukturen enthalten isolierte [Sc6C]- bzw. [Pr6(C2)]-Cluster, die von 18 Halogenid-Ionen (X-, 12 Xi und 6 Xa; X = Cl bzw. I) umgeben sind. Die Verknüpfung erfolgt gemäß dem Motiv [M6Z]X8iX4/21-aX4/2a-1X2/2a-a (M = Sc bzw. Pr; Z = C bzw. C2) und stellt damit ein noch unbekanntes Verknüpfungsmuster für Verbindungen der Zusammensetzung Ax[M6Z]X13 dar, das jenem der [TiO6]-Oktaeder in der Anatas-Struktur von TiO2 entspricht.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200905
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  • 6
    Electronic Resource
    Electronic Resource
    Cs3[Tb10(C2)2]Cl21, ein neuer Formel- und Strukturtyp mit isolierten, dimeren Clustern (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1527-1531 
    Details
    ISSN: 0044-2313
    Keywords: Terbium Cluster ; [Tb10(C2)2] ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cs3[Tb10(C2)2]Cl21, A New Formula and Structure Type with Isolated Dimeric ClustersCs3[Tb10(C2)2]Cl21 is obtained via the metallothermic reduction of TbCl3 with caesium in the presence of graphite as black single crystals. The crystal structure (monoclinic, C2/c, Z = 4; a = 2318.72(13); b = 1245.8(9); c = 1502.0(13) pm; β = 98.13(6)°; R = 0.089; Rw = 0.049) contains dimeric clusters that are built from two octahedra connected via one common edge and filled with C2 units. These isolated [Tb10(C2)2] clusters are surrounded by 26 chloride ligands which are then connected via i - a and a - a bridges in a way that voids for Cs+ of coordination number 10 are formed.
    Notes: Cs3[Tb10(C2)2]Cl21 entsteht bei der metallothermischen Reduktion von TbCl3 mit Caesium in Gegenwart von Graphit in Form schwarzer Einkristalle. Die Kristallstruktur (monoklin, C2/c, z = 4; a = 2318,72(13); b = 1245,8(9); c = 1502,0(13) pm; β = 98,13(6)°; R = 0,089; Rw = 0,049) enthält dimere Cluster, die aus zwei über eine gemeinsame Kante verknüpften und durch zwei C2-Hanteln aufgefüllten Oktaedern gebildet werden. Die isolierten [Tb10(C2)2]-Cluster sind von insgesamt 26 Cl- umgeben und durch i - a- bzw. a - a-Brücken so miteinander verknüpft, daß für die Cs+ Lücken der Koordinationszahl 10 verbleiben.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200906
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  • 7
    Electronic Resource
    Electronic Resource
    Cs[Er10(C2)2]I18 und [Er10(C2)2]Br18: zwei neue Beispiele für „reduzierte“ Halogenide der Lanthanide mit isolierten [M10(C2)2]-Clustern (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1532-1536 
    Details
    ISSN: 0044-2313
    Keywords: Erbium Clusters, [Er10(C2)2] ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cs[Er10(C2)2]I18 and [Er10(C2)2]Br18: Two New Examples for Reduced Halides of the Lanthanides with Isolated [M10(C2)2] ClustersCs[Er10(C2)2]I18 is obtained from the reaction of ErI3 with caesium and carbon in sealed tantalum containers at 700°C and [Er10(C2)2]Br18 through the metallothermic reduction of ErBr3 with rubidium in the presence of carbon at 750°C in sealed niobium containers. The crystal structures {Cs[Er10(C2)2]I18: triclinic, P1; a = 1 105.2(8) pm, b = 1 112.0(7) pm; c = 1 122.9(8) pm; α = 66.91(3)°, β = 87.14(3)°; γ = 60.80(3)°; Z = 1; R = 0.049, Rw = 0.043; [Er10(C2)2]Br18: monoclinic, P21/n, a = 971.8(6) pm, b = 1 623.4(9) pm, c = 1 163.8(6) pm, β = 104.00(6)°; Z = 2; R = 0.077, Rw = 0.057} contain isolated dimeric [Er10(C2)2] clusters. Due to the inclusion of C2 units, the octahedra are elongated in the direction of the pseudo C4 axis. The connecting edges of the two octahedra are exceptionally short (316.7 pm and 314.8 pm respectively). The dimeric units are connected via Xi-a and Xa-i (X = Br, I) bridges according to [Er10(C2)2X10iX8/2i-a]X8/2a-i. Cs+ is surrounded by a cuboctahedron of iodide ions in Cs[Er10(C2)2]I18.
    Notes: Cs[Er10(C2)2]I18 entsteht bei der Umsetzung von Erl3 mit Caesium und Kohlenstoff in verschweißten Tantalampullen bei 700°C, [Er10(C2)2]Br18 bei der metallothermischen Reduktion von ErBr3 mit Rubidium in Gegenwart von Kohlenstoff bei 750°C in verschweißten Niobampullen. Die Kristallstrukturen {Cs[Er10(C2)2]I18: triklin, P1; a = 1 105,2(8) pm; b = 1 112,0(7) pm; c = 1 122,9(7) pm; α = 66,91(3)°; β = 87,14(3)°; γ = 60,80(3)°; Z = 1; R = 0,049, Rw = 0,043; [Er10(C2)2]Br18: monoklin, P21/n; a = 971,8(6); b = 1 623,4(9); c = 1 163,8(6); β = 104,00(6)°; Z = 2; R = 0,077, Rw = 0,057} beinhalten isolierte dimere [Er10(C2)2]-Cluster. Wegen des Einbaus der C2-Hantel sind die Oktaeder entlang ihrer pseudovierzähligen Achse gestreckt. Die verknüpfenden Oktaederkanten weisen einen besonders kurzen Metall-Metall-Abstand auf (316,7 bzw. 314,8 pm). Die dimeren Einheiten sind über Xi-a bzw. Xa-i-Brücken (X = Br, I) miteinander verknüpft, gemäß [Er10(C2)2X10iX8/2i-a]X8/2a-i. Cs+ ist in Cs[Er10(C2)2]I18 kuboktaederisch von Iodidionen umgeben.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200907
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  • 8
    Electronic Resource
    Electronic Resource
    Zur Kenntnis der Struktur von Sr3(BN2)2 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 262-265 
    Details
    ISSN: 0044-2313
    Keywords: Ca3(BN2)2 ; Sr3(BN2)2 ; NaSr4(BN2)3 ; preparation ; structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Structure of Sr3(BN2)2The structure of Sr3(BN2)2 was determined on single-crystal X-ray data collected with a four-circle diffractometer. Sr3(BN2)2 crystallizes in the cubic space group Im3m (no. 229) with a = 764.56(3) pm and Z = 3. The structure contains linear BN3-2 ions with a B—N bond length of 135.8(6) pm. The straight forward synthesis employing metal nitrides plus boron nitride yielded crystalline powders of M3(BN2)2 (M = Ca, Sr) at 1100°C (5 days). Cubic indexing of guinier patterns gave a = 765.8(1) pm for M = Sr and a = 734.7(2) pm for M = Ca. The structure refinement on a single crystal of Sr3(BN2)2 revealed that one strontium site (2a; 0, 0, 0) is occupied by only about 50%. It has been tried to fully occupy this site with an alkali metal (A) to obtain ASr4(BN2)3 (Z = 2). Reactions with A = Na yielded crystalline powders. Cubic indexing of the guinier pattern analogous to that of Sr3(BN2)2 gave a = 754.2(1) pm.
    Notes: Die Struktur von Sr3(BN2)2 wurde anhand von Einkristall-Röntgendaten, die durch Messung an einem Vierkreisdiffraktometer erhalten wurden, bestimmt. Sr3(BN2)2 kristallisiert in der kubischen Raumgruppe Im3m (Nr. 229) mit a = 764,56(3) pm und Z = 3. Die Struktur enthält lineare BN3-2-Ionen mit einer Bindungslänge B—N von 135,8(6) pm. Die gezielte Darstellung aus den Metallnitriden und Bornitrid zu M3(BN2)2 (M = Ca, Sr) bei 1100°C (5 Tage) ergab kristalline Pulver. Kubische Indizierung der Guinierdiagramme gab a = 765,8(1) pm für M = Sr und 734,7(2) pm für M = Ca. Die Strukturverfeinerung an einem Einkristall von Sr3(BN2)2 zeigte, daß eine Strontiumlage (2a; 0,0,0) nur zu etwa 50% besetzt ist. Es wurde versucht, diese Lage mit einem Alkalimetall (A) entsprechend ASr4(BN2)3 (Z = 2) vollständig zu besetzen. Reaktionen mit A = Na ergaben kristalline Pulver, deren Guinierdiagramme analog zu Sr3(BN2)2 kubisch mit a = 754,2(1) pm indiziert werden konnten.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200210
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  • 9
    Electronic Resource
    Electronic Resource
    Synthesis, crystal structure, magnetism, and absorption spectra of A2UX5 Type Halides (A = K, Rb; X = Cl, Br, I)Dedicated to Professor Hugo F. Franzen on his 60th Birthday (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1339-1345 
    Details
    ISSN: 0044-2313
    Keywords: Alkali uranium halides, A2UX5 (A = K, Rb; X = Cl, Br, I) ; preparation ; crystal structure ; magnetic susceptibility ; UV-Vis spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese, Kristallstruktur, Magnetismus und Absorptionsspektren von Halogeniden des Typs A2UX5 (A = K, Rb; X = Cl, Br, I)Die ternären Uran(III)-halogenide A2UX5 (A = K, Rb; X = Cl, Br, I) wurden aus den binären Komponenten AX und UX3 in verschweißten Tantalampullen gewonnen. Nach Guinier-Aufnahmen (Raumtemperatur) kristallisieren sie sämtlich im K2PrCl5/Y2HfS5-Typ. Einkristall-Strukturverfeinerungen wurden für K2UI5 und Rb2UCl5 unternommen. Magnetische Suszeptibilitätsmessungen erfolgten mit einem SQUID-Magnetometer von Raumtemperatur bis zur Temperatur des flüssigen Heliums: Eindimensionale (innerhalb einer Kette) und dreidimensionale antiferromagnetische Ordnung wird bei tiefen Temperaturen, abhängig vom Abstand U3+—U3+, beobachtet. Absorptionsspektren wurden zwischen 4000 und 28000 cm-1 aufgenommen. Sie zeigen die für U3+ charakteristischen Übergänge und, abhängig vom Halogenid, sehr starke f - d Übergänge oberhalb 14000 bzw. 15000 cm-1.
    Notes: The ternary uranium(III) halides A2UX5 (A = K, Rb; X = Cl, Br, I) have been prepared from the binary components AX and UX3 in sealed tantalum containers. According to their Guinier X-ray powder patterns, they all crystallize with the K2PrCl5/Y2HfS5 type of structure. Lattice constants for ambient temperature are reported. Single-crystal structure refinemens were undertaken for K2UI5 and Rb2UCl5. Magnetic susceptibility data were recorded with a SQUID magnetometer from liquid helium to room temperature. One-dimensional (intrachain) and three-dimensional antiferromagnetic ordering occur at low temperatures dependent upon the U3+—U3+ distance. Absorption spectra were recorded between 4 000 and 28 000 cm-1. They show f - f transitions typical for U3+ and, depending on the halide, very strong f - d transitions above 14 000 to 15 000 cm-1, respectively.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200802
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  • 10
    Electronic Resource
    Electronic Resource
    Zwei neue Silicat-Chloride mit zweiwertigem Europium: LiEu3[SiO4]Cl3 und Li7Eu8[SiO4]4Cl7Professor Philipp Gütlich zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1351-1356 
    Details
    ISSN: 0044-2313
    Keywords: Silicate-chloride ; crystal structure ; europium ; lithium ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Two New Silicate-Chlorides with Divalent Europium: LiEu3[SiO4]Cl3 and Li7Eu8[SiO4]4Cl7LiEu3[SiO4]Cl3 was prepared by reaction of LiCl with Eu2SiO4 and Li7Eu8[SiO4]4Cl7 from Li with Eu2O3, SiO2 and LiCl. The crystal structures of LiEu3[SiO4]Cl3 (Pmna, a = 946.95(13); b = 699.52(8); c = 1 368.0(2) pm; Z = 4; R1 = 0.0325, R2w = 0.0642) and Li7Eu8[SiO4]4Cl7 (P21/c; a = 851.85(5); b = 948.62(7); c = 1 679.0(2) pm; β = 96.221(8)°; Z = 2; R1 = 0.0352, R2w = 0.0744) were determined from four-circle diffractometer data. LiEu3[SiO4]Cl3 contains [Li(SiO4)2] units and LiCl6 octahedra while in Li7Eu8[SiO4]4Cl7 larger „lithosilicate“ groups are found. In both structures, the Eu2+ ions are coordinated mostly eightfold by O2- and Cl- ligands.
    Notes: LiEu3[SiO4]Cl3 wurde durch Umsetzung von LiCl mit Eu2SiO4 dargestellt, Li7Eu8[SiO4]4Cl7 durch Umsetzung von Li mit Eu2O3, SiO2 und LiCl. Die Kristallstrukturen von LiEu3[SiO4]Cl3 (Pmna, a = 946,95(13); b = 699,52(8); c = 1 368,0(2) pm; Z = 4; R1 = 0,0325, R2w = 0,0642) und Li7Eu8[SiO4]4Cl7 (P21/c; a = 851,85(5); b = 948,62(7); c = 1 679,0(2) pm; β = 96,221(8)°; Z = 2; R1 = 0,0352, R2w = 0,0744) wurden aus Einkristall-Vierkreisdiffraktometer-Daten bestimmt. LiEu3[SiO4]Cl3 enthält [Li(SiO4)2]-Einheiten neben LiCl6-Oktaedern, während in Li7Eu8[SiO4]4Cl7 größere „Lithosilicat“-Baugruppen vorliegen. Die Eu2+-Ionen sind in beiden Strukturen meist achtfach von O2-- und Cl--Liganden koordiniert.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200804
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