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  • 11
    Electronic Resource
    Electronic Resource
    Zur Synthese und Kristallstruktur von LiPdAlF6 und PdZrF6 (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 189-192 
    Details
    ISSN: 0044-2313
    Keywords: Fluoropalladates(II) ; preparation ; single 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 LiPdAlF6 and PdZrF6.For the first time single crystals of the new compounds LiPdAlF6 and PdZrF6 have been obtained. LiPdAlF6 (blue) crystallizes trigonal, space group P31c - D3d2 (No. 163; LiCaAlF6-type [2]), in an ordered structure variant of the Li2[ZrF6]-structure [3], with a=497.21(9) pm, c=914.0(9) pm and Z=2. PdZrF6 (also blue) is isotypic with LiSbF6 [4] and crystallizes trigonal-rhomboedric with a=552,3(1) pm, c=1 447,5(4) pm, space group R 3 - C3i2 (No. 148) and Z=3.
    Notes: Neu dargestellt wurden LiPdAlF6 und PdZrF6, beide in Form von Einkristallen. Blaues LiPdAlF6 kristallisiert trigonal im LiCaAlF6-Typ [2], einer Ordnungsvariante der Li2[ZrF6]-Struktur [3], in der Raumgruppe P31c - D3d2 (Nr. 163) mit a=497,21(9) pm, c=914,0(9) pm und Z=2. PdZrF6 (hellblau) kristallisiert trigonal-rhomboedrisch in der Raumgruppe R 3 - C3i2(Nr. 148) mit a=552,3(1) pm, c=1 447,5(4) pm und Z=3 (isotyp zu LiSbF6 [4]).
    Additional Material: 6 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190131
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  • 12
    Electronic Resource
    Electronic Resource
    Fluoroplatinate(IV) der Lanthaniden LnF[PtF6]. (Ln = Pr, Sm, Gd, Tb, Dy, Ho, Er) (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1431-1440 
    Details
    ISSN: 0044-2313
    Keywords: Fluoroplatinates(IV) ; preparation ; single crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Fluoroplatinates(IV) of the Lanthanides LnF[PtF6] (Ln = Pr, Sm, Gd, Tb, Dy, Ho, Er)For the first time fluorides LnF[PtF6] (Ln = Pr, Sm, Gd, Tb, Dy, Ho, Er), all yellow have been obtained. From single crystal data they crystallize monoclinic, space group P21/n-C2h5 (No. 14), Z = 4, Pr: a = 1 125.77(19) pm, b = 559.04(7) pm, c = 910.27(17) pm, β = 107.29(1)°; Sm: a = 1 114.63(31) pm, b = 552.70(12) pm, c = 898.02(20) pm, β = 107.24(2)°; Gd: a = 1 112.12(15) pm, b = 551.22(7) pm, c = 891.99(11) pm, β = 107.09(1)°; Tb (Powder data): a = 1 108.88(20) pm, b = 552.71(9) pm, c = 889.56(16) pm, β = 107.30(1)°; Dy: a = 1 100.28(23) pm, b = 547.77(8) pm, c = 882.41(13) pm, β = 107.32(1); Ho: a = 1 099.11(16) pm, b = 546.16(7) pm, c = 879.45(15) pm, β = 107.34(1)°; Er: a = 1 095.10(16) pm, b = 544.82(10) pm, c = 874.85(14) pm, β = 107.37(1)°.
    Notes: Erstmals dargestellt wurden Fluoride LnF[PtF6] (Ln = Pr, Sm, Gd, Tb, Dy, Ho, Er), alle gelb. Nach Einkristalluntersuchungen kristallisieren diese monoklin in der Raumgruppe P21/n-C2h5 (Nr. 14), Z = 4, Pr: a = 1 125,77(19) pm, b = 559,04(7) pm, c = 910,27(17) pm, β = 107,29(1)°; Sm: a = 1 114,63(31) pm, b = 552,70(12) pm, c = 898,02(20) pm, β = 107,24(2)°; Gd: a = 1 112,12(15) pm, b = 551,22(7) pm, c = 891,99(11) pm, β = 107,09(1)°; Tb (Pulverdaten): a = 1 108,88(20) pm, b = 552,71(9) pm, c = 889,56(16) pm, β = 107,30(1)°; Dy: 1 100,28(23) pm, b = 547,77(8) pm, c = 882,41(13) pm, β = 107,32(1)°; Ho: a = 1 099,11(16) pm, b = 546,16(7) pm, c = 879,45(15) pm, β = 107,34(1)°; Er: a = 1 095,10(16) pm, b = 544,82(10) pm, c = 874,85(14) pm, β = 107,37(1)°. Im Gegensatz zu älteren Befunden liegt die Raumgruppe P21/n-C2h5 (Nr. 14) mit einem verdoppelten Zellvolumen vor.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190819
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  • 13
    Electronic Resource
    Electronic Resource
    Tetrafluoroaurate(III) der Lanthaniden MF[AuF4]2 (M = Tm, Yb, Lu) (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1661-1668 
    Details
    ISSN: 0044-2313
    Keywords: Rare earth tetrafluoroaurates(III) ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tetrafluoroaurates(III) of Lanthanides MF[AuF4]2 (M = Tm, Yb, Lu).Tetrafluoroaurates(III) MF[AuF4]2 with M = Tm, Yb, Lu, all yellow, have been prepared for the first time. From single crystal data they crystallize orthorhombic, space group Pbcn-D2h14 (No. 60) with M = Tm: a = 1 102.92(8) pm, b = 904.38(8) pm, c = 2 164.46(23) pm; M = Yb: a = 1 100.98(12) pm, b = 902.23(8) pm, c = 2 157.36(23) pm; M = Lu: a = 1 099.28(18) pm, b = 900.70(15) pm, c = 2 151.50(46) pm.
    Notes: Neu dargestellt wurden gelbe Tetrafluoroaurate(III) der Lanthaniden MF[AuF4]2 mit M = Tm, Yb, Lu. Nach Einkristalluntersuchungen kristallisieren diese orthorhombisch in der Raumgruppe Pbcn-D2h14 (Nr. 60) mit Z = 12. Im Einzelnen wurden folgende Werte gefunden: Für M = Tm: a = 1 102,92(8) pm, b = 904,38(8) pm, c = 2 164,46(23) pm; M = Yb: a = 1 100,98(12) pm, b = 902,23(8) pm, c = 2 157,36(23) pm; M = Lu: a = 1 099,28(18) pm, b = 900,70(15) pm, c = 2 151,50(46) pm.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936191004
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  • 14
    Electronic Resource
    Electronic Resource
    Neue Fluoropalladate(II) M2[PdF4] (M = Na, K) sowie K2RbPdF5Professor Hanskarl Müller-Buschbaum zum 60. Geburtstag (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 9-18 
    Details
    ISSN: 0044-2313
    Keywords: Alkali fluoro palladate(II) ; preparation ; single crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Fluoropalladates(II) M2[PdF4] (M = Na, K) and K2RbPdF5For the first time bright yellow single crystals M2[PdF4] (M = Na, K) have been obtained and their structure determined. K2[PdF4] crystallizes monoclinic, space group C2/m-C2h3 (No. 12) with a = 975.2(3) pm, b = 597.6(1) pm, c = 420.2(1) pm, β = 92.17(2)° and Z = 2. Structure related Na2[PdF4] crystallizes monoclinic too, but in space group P21/c-C2h5 (No. 14) with a = 340.88(7) pm, b = 561.1(1) pm, c = 999.2(2) pm, β = 93.97(2)° and Z = 2. K2RbPdF5, yellow, crystallizes tetragonal with a = 724.9(1) pm, c = 627.9(1) pm, Z = 2 and is isotypic with Rb2CsPdF5 (space group P4/mbm-D4h5, No. 127), an ordered structure variant of the Rb3PdF5-type [1].
    Notes: Erstmals konnten leuchtend gelbe Einkristalle M2[PdF4] (M = Na, K) dargestellt und ihre Struktur bestimmt werden. K2[PdF4] kristallisiert monoklin, R.G. C2/m-C32h (Nr. 12) mit a = 975,2(3) pm, b = 597,6(1) pm, c = 420,2(1) pm, β = 92,17(2)° und Z = 2. Strukturverwandtes Na2[PdF4] kristallisiert ebenfalls monoklin, jedoch in der R.G. P21/c-C2h5 (Nr. 14) mit a = 340,88(7) pm, b = 561,1(1) pm, c = 999,2(2) pm, β = 93,97(2)°und Z = 2. K2RbPdF5, gelb, kristallisiert tetragonal mit a = 724,9(1) pm, c = 627,9(1) pm, Z = 2 und ist isotyp zu Rb2CsPdF5 (R.G. P4/mbm-D4h5, Nr. 127), einer geordneten Strukturvarianten des Rb3PdF5-Typs [1].
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19915970103
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  • 15
    Electronic Resource
    Electronic Resource
    (PPh4)[(ReO2S2)CuI] und (NEt4)2[(ReOS3)Cu3Cl4]: Fixierung der bisher nicht isolierten Ionen [ReO2S2]- und [ReOS3]- durch Ausnutzung der Stabilität der CuS2(Re)- und Cu3S3(Re)-Fragmente (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 614 (1992), S. 115-120 
    Details
    ISSN: 0044-2313
    Keywords: Oxothioperrhenate ions, ReO2S2-, ReOS3- ; preparation ; crystal structure ; IR, UV/Vis spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: (PPh4)[(ReO2S2)CuI] and (NEt4)2[ReOS3)Cu3Cl4]: Fixation of the up to now not Isolated Ions [ReO2S2]- and [ReOS3]- Utilizing the Stability of the CuS2(Re) and Cu3S3(Re) Fragments(PPh4)[(ReO2S2)CuI] (1) and (NEt4)2[ReOS3)Cu3Cl4] (2) containing the up to now not isolated oxothioperrhenate ions [ReO2S2]- and [ReOS3]- as ligands, have been prepared by the reaction of (NEt4)[ReS4] with PPh3 and CuI in acetone in the presence of (PPh4)I ((1)) or with CuCl in CH2Cl2 in the presence of (NEt4)Cl ((2)), respectively. 1 and 2 have been characterized by X-ray structure analysis, elemental analysis and spectroscopic studies (IR, UV/Vis). The electronic spectra show bands which can approximately be assigned to interesting low-energy charge-transfer-transitions of the type d(Cu) → d(Re).For crystal data see Inhaltsübersicht.
    Notes: (PPh4)[(ReO2S2)CuI] (1) und (NEt4)2[(ReOS3)Cu3Cl4] (2), die die bisher nicht isolierten Oxothioperrhenat-Ionen [ReO2S2]- und [ReOS3]- als Liganden enthalten, wurden durch Reaktion von (NEt4)[ReS4] mit PPh3 und CuI in Aceton in Gegenwart von (PPh4)I ((1) bzw. entsprechend mit CuCl in CH2Cl2 in Gegenwart von (NEt4)Cl ((2) erhalten. 1 und 2 wurden durch Einkristall-Röntgenstrukturanalyse, Elementaranalyse, sowie spektroskopische Untersuchungen (IR, UV/Vis) charakterisiert. In den Elektronenspektren findet man Banden, die interessanten niederenergetischen Charge-Transfer-Übergängen des Typs d(Cu) → d(Re) näherungsweise zugeordnet werden können.Kristalldaten: 1P21/n, a = 1162,2(4), b = 1395,7(6), c = 1612,3(9)pm, β = 96,53(4)° V = 2598(2) · 106pm3, R = 0,049 für 4623 unabhängige Reflexe (F0≥4,0σ(F0)).2C2/c, a = 2059,0(5), b = 1352,9(3), c = 2217,1(5)pm, β = 90,26(22)° V = 6176(2) · 106pm3, R = 0,080 für 3162 unabhängige Reflexe (F0≥4,0σ(F0)).
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926140820
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  • 16
    Electronic Resource
    Electronic Resource
    Darstellung und Charakterisierung von Reagenzien mit der MesityldimethylsilylgruppeProfessor Rudolf Taube zum 60. Geburtstag gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 603 (1991), S. 15-20 
    Details
    ISSN: 0044-2313
    Keywords: Mesityldimethylsilyl compounds ; preparation ; reactivity ; 1H, 13C n.m.r. data ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Characterization of Reagents with the Mesityldimethylsilyl GroupThe syntheses of MesMe2SiCl, MesMe2SiBr, MesMe2SiC5H5, MesMe2SiC2Ph, MesMe2SiPh, MesMe2SiNEt2, MesMe2SiN2C3H3, MesMe2SiNC8H6, (MesMe2Si)2NH, (MesMe2Si)2, and the preparation of solutions of the silyllithium and silylpotassium compound are reported. The compounds are characterized by 1H NMR spectroscopy, 13C NMR spectroscopy, and elemental analysis.
    Notes: Die Synthesen der Verbindungen MesMe2SiCl, MesMe2SiBr, MesMe2SiC5H5, MesMe2SiC2Ph, MesMe2SiPh, MesMe2SiNEt2, MesMe2SiN2C3H3, MesMe2SiNC8H6, (MesMe2Si)2NH, (MesMe2Si)2 und die Herstellung von Lösungen der Silyllithium- und Silylkaliumverbindung werden beschrieben. Die Verbindungen werden durch 1H-NMR-Spektroskopie, 13C-NMR-Spektroskopie und Elementaranalyse charakterisiert.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19916030103
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  • 17
    Electronic Resource
    Electronic Resource
    Zur Kristallstruktur von KGaO2 und NaGaO2(II) [1]Herrn Professor Wolfgang Beck zum 60. Geburtstage am 5. Mai 1992 gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 611 (1992), S. 73-80 
    Details
    ISSN: 0044-2313
    Keywords: Potassium, sodium gallate ; preparation ; crystal structure ; MAPLE calculation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of KGaO2 and NaGaO2(II)By annealing intimate mixtures of K2O, Na2O and β-Ga2O3 (K : Na : Ga = 2.2 : 1.1 : 1) we obtained single crystals of K2Na4[(GaO3)2] and KGaO2 (Ag-cylinder; 600°C, 26 d). Structure refinement for KGaO2 (four-circle diffractometer data, Mo-Kα, 1 390 or 1 390 Io(hkl); R = 5.55%, Rw = 3.05%) confirms the space group Pbca; a = 552.1 pm, b = 1 107.5 pm, c = 1 580.7 pm, Z = 16.According to K[GaO4/2] we have a stuffed cristobalite-related structure.Single crystals of NaGaO2(II) were grown by annealing intimate mixtures of Na2O2 and GaAs (Na2O2 : GaAs 4.1 : 1) in Ag-cylinders that were not completely closed (570°C, 6 weeks). Structure refinement for NaGaO2(II) (four-circle diffractometer data, Mo-Kα, 588 of 616 Io(hkl); R = 4.54%, Rw = 4.06%) confirms the spacegroup Pna21; a = 549.8(1) pm, b = 720.6(1) pm, c = 529.8(1) pm, Z = 4. In NaGaO2(II) we have a wurtzite-related structure.
    Notes: Beim Tempern inniger Gemenge von K2O, Na2O und β-Ga2O3 (vor Verreiben: K : Na : Ga = 2,2 : 1,1 : 1) erhielten wir neben Einkristallen von K2Na4[(GaO3)2] auch solche von KGaO2 (Ag-Zylinder, 600°C, 26 d). Die Strukturverfeinerung (Vierkreisdiffraktometerdaten, Mo-Kα, 1 390 von 1 390 Io(hkl); R = 5,55%, Rw = 3,05%) belegt die Raumgruppe Pbca; a = 552,1 pm, b = 1 107,5 pm, c = 1 580,7 pm, Z = 16.Es liegt eine aufgefüllte Cristobalit-Variante gemäß K[GaO4/2] vor.Einkristalle von NaGaO2(II) erhielten wir durch Tempern inniger Gemenge von Na2O2 und GaAs (vor Verreiben: Na2O2: GaAs 4,1 : 1) in nicht ganz verschlossenen Ag-Zylindern (570°C, 6 Wochen). Die Strukturverfeinerung (Vierkreisdiffraktometerdaten, Mo-Kα, 588 von 616 Io(hkl); R = 4,54%, Rw = 4,06%) belegt die Raumgruppe Pna21; a = 549,8(1) pm, b = 720,6(1) pm, c = 529,8(1) pm, Z = 4 (Guinier-de Wolff-Daten). NaGaO2(II) ist eine Ordnungsvariante des Wurtzit-Typs.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926110512
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  • 18
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    Electronic Resource
    Zur Kenntnis des Natrium-tetrahydroxoaluminat-chlorids Na2[Al(OH)4]Cl (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 771-776 
    Details
    ISSN: 0044-2313
    Keywords: Tetrahydroxoaluminate chloride, Na2[Al(OH)4]Cl ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Sodium Tetrahydroxoaluminate Chloride Na2[Al(OH)4]ClThe hitherto unknown compound Na2[Al(OH)4]Cl was prepared by crystallisation from a NaCl containing sodium aluminate solution. According to the X-ray single crystal investigation (tetragonal, space group P4/nmm, a = 7.541 Å, c = 5.059 Å, Z = 2) the compound represents the first example of a crystalline hydroxoaluminate with monomeric [Al(OH)4]- anions. Cl- shows a quadratic anti prismatic coordination to 4 Na+ and over hydrogen bonds to 4 O2- while Na+ is octahedrally coordinated by 4 O2- and 2 Cl- (axial). The results of the crystal structure analysis are confirmed by 27Al and 23Na MAS NMR investigations. Na2[Al(OH)4]Cl decomposes at about 200°C without intermediates under formation of β-NaAlO2 and NaCl.
    Notes: Die bisher unbekannte Verbindung Na2[Al(OH)4]Cl wurde durch Kristallisation aus mit NaCl versetzter Natriumaluminatlösung erhalten. Entsprechend der Röntgenstrukturanalyse an einem Einkristall (tetragonal, Raumgruppe P4/nmm, a = 7,541 Å, c = 5,059 Å, Z = 2) liegt mit dieser Verbindung erstmals ein Beispiel für ein kristallines Hydroxoaluminat mit monomeren [Al(OH)4]--Anionen vor. Cl- ist quadratisch antiprismatisch mit 4 Na+ sowie über Wasserstoffbrückenbindungen mit 4 O2- koordiniert, während Na+ oktaedrisch von 4 O2- und 2 Cl- (axial) umgeben ist. Die Ergebnisse der Kristallstrukturanalyse werden durch 27Al- und 23Na-MAS-NMR-Messungen bestätigt. Na2[Al(OH)4]Cl zersetzt sich ohne Zwischenprodukte bei 200°C zu β-NaAlO2 und NaCl.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200432
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