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  • 1
    Electronic Resource
    Electronic Resource
    Das erste gemischt-valente Oxocobaltat(I, II): Rb5Co2O4 [1] (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 540-550 
    Details
    ISSN: 0044-2313
    Keywords: Mixed-valent oxide of cobalt ; structure ; MAPLE, CHARDI, MEFIR-FIT ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A New Mixed-Valent Oxide of Cobalt(I, II): Rb5Co2O4For the first time we obtained a new mixed-valent oxide of mono- and divalent Cobalt. Black-red single-crystals of Rb5Co2O4 were prepared by heating powders of “Rb6CdO4” in closed Co-cylinders at 500° during 48 days.Structure solution and refinement are covered by two measurements with four-circle diffractometers. MoKα: 2 145 Io(hkl), out of 2 818 Io(hkl), R = 9.85%, Rw = 5.93% AgKα: 1 813 Io(hkl) out of 4 007 Io(hkl), R = 9.46%, Rw = 6.51%) and confirm the space-group P1. The lattice constants are a = 696.4(1) pm, b = 922.2(3) pm, c = 958.9(3) pm, α = 117.99(2)°, β = 89.96(2)°, γ h= 108.12(2)°, Z = 2According to its composition Rb10[OCoO]2[OCoO2CoO] the structure is built up by two Co atoms of chemically and crystallographically different nature. We find isolated dumb-bell-like anions [O—Co—O]3- being already known with monovalent Co (e. g. K3CoO2) together with units [OCoO2CoO]4- of two connected triangles CoO3 being well-known from K2BeO2 ≜ K4[Be2O4]. ECoN/mEFIR calculations are made starting with values obtained by a new procedure called “MEFIR-FIT”.
    Notes: Durch 48tägiges Tempern von Rb6CdO4 in verschlossenen Co-Zylindern bei 500°C wurde erstmals ein gemischt-valentes Oxid des ein- und zweiwertigen Cobalts in Form von schwarzroten Einkristallen dargestellt. Die Strukturaufklärung mittels Vierkreisdiffraktometer (zwei Messungen: MoKα: 2 145 von 2 818 Io(hkl), R = 9,85%, Rw = 5,93% AgKα: 1 813 von 4 007 Io(hkl), R = 9,46%, Rw = 6,51%) belegt die Raumgruppe P1. Die Gitterkonstanten nach Pulverdaten sind a = 696,4(1) pm, b = 922,2(3) pm, c = 958,9(3) pm, α = 117,99(2)°, β = 89,96(2)°, γ = 108,12(2)°, Z = 2 (Standardabweichungen in Einheiten der letzten Stelle Klammern).Die chemisch unterschiedlichen Co-Teilchen nehmen auch kristallographisch unterschiedliche Umgebungen an: Während CoI in Form „isolierter“, linearer Hanteln [O—Co—O]3- vorliegt, bildet CoII[Co2O4]4--Einheiten in Form zweier kantenverknüpfter Dreiecke CoO3, analog dem Aufbau des Anions in K4[Be2O4] [2].Zur Berechnung der Startwerte der „Mittleren Fiktiven Ionenradien“ (MEFIR) wird ein neues Verfahren (MEFIR-FIT) angewandt.
    Additional Material: 12 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190320
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  • 2
    Electronic Resource
    Electronic Resource
    Zur Existenz polynärer Oxide der Alkalimetalle mit einwertigen Cobalt bzw. Nickel [1, 2] (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 923-933 
    Details
    ISSN: 0044-2313
    Keywords: Oxides of monovalent Co and Ni ; structure ; MAPLE ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Existence of Polynary Oxides of the Alkali Metals with Monovalent Cobalt and NickelFor the first time we obtained RbNa2NiO2, KNa2NiO2, Na3CoO2 and K3CoO2 [RbNa2NiO2: Na2NiO2 + Rb2O, Rb:Ni = 1.8:1, 600°C, 28 d, Ni-tube; KNa2NiO2: Na2NiO2 + K2O, K:Ni = 1.8:1, 600°C, 20 d, Ni-tube; Na3CoO2: Na2O + CoO: Na:Co = 8.8:1, 500°C, 20 d, Co-tube; K3CoO2: K2O + CoO: K:Co = 4.4:1, 550°C, 20 d, Co-tube]. According to X-ray structure analysis of single crystals monovalent Co and Ni is present [always four-circle-diffractometer data, MoKα-radiation; RbNa2NiO2: AED 2, all 163 Io(hkl), R = 3.4%, Rw = 1.9%, I4/mmm, a = 461.7(1), c = 973.6(3) pm, Z = 2; KNa2NiO2: AED 2, all 341 Io(hkl), R = 5.6%, Rw = 3.5%, Cmma, a = 1 048.5(3), b = 626.8(1), c = 621.9(1) pm, Z = 4; Na3CoO2: PW 1 100, 517 of 568 Io(hkl), R = 2.9%, Rw = 1.8%, P42/mnm, a = 940.0, c = 464.5 pm, Z = 4; K3CoO2: PW 1 100, all 940 Io(hkl), R = 5.0%, Rw = 3.9%, Pnma, a = 1 190.0, b = 730.4, c = 604.1 pm, Z = 4]. All samples are red, the single crystals transparent. Two O2- coordinate Ni1+ and Co1+, respectively, like a dumb-bell. Mean Fictive Ionic Radii, MEFIR, and Effective Coordination Numbers, ECoN, and Madelung part of lattice energy, MAPLE, are given.
    Notes: Erstmals wurden RbNa2NiO2, KNa2NiO2, Na3CoO2 und K3CoO2 dargestellt [RbNa2NiO2: Na2NiO2 + Rb2O, Rb:Ni = 1,8:1, 600°C, 20 d, Nickelbombe; KNa2NiO2: Na2NiO2 + K2O, K:Ni = 1,8:1, 600°C, 20 d, Nickelbombe; Na3CoO2: Na2O + CoO, Na:Co = 8,8:1, 500°C, 20 d, Cobaltbombe; K3CoO2: K2O + CoO, K:Co = 4,4:1, 550°C, 20 d, Cobaltbombe]. Nach Einkristalldaten weisen Cobalt wie Nickel die Oxydationsstufe + 1 auf [jeweils Vierkreisdiffraktometer mit MoKα-Strahlung; RbNa2NiO2: AED 2, alle 163 Io(hkl), R = 3,4%, Rw = 1,9%, I4/mmm, a = 461,7(1), c = 973,6(3) pm, Z = 2; KNa2NiO2: AED 2, alle 341 Io(hkl), R = 5,6%, Rw = 3,5%, Cmma, a = 1 048,5(3), b = 626,8(1), c = 621,9(1) pm, Z = 4; Na3CoO2: PW 1 100, 517 aus 568 Io(hkl), R = 2,9%, Rw = 1,8%, P42/mnm, a = 940,0, c = 464,5 pm, Z = 4; K3CoO2: PW 1 100, alle 940 Io(hkl), R = 5,0%, Rw = 3,9%, Pnma, a = 1 190,0, b = 730,4, c = 604,1 pm, Z = 4].Alle Präparate sind rot, die Einkristalle transparent. Ni1+ bzw. Co1+ ist jeweils in Form einer Hantel von 2 O2- koordiniert. Mittlere Fiktive Ionenradien (MEFIR) und Effektive Koordinationszahlen (ECoN), sowie der Madelunganteil der Gitterenergie (MAPLE), werden angegeben.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190520
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  • 3
    Electronic Resource
    Electronic Resource
    Über Oxide mit dem “Butterfly-Motiv”: Rb6[Fe2O5] und K6[Fe2O5] (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 618 (1992), S. 63-73 
    Details
    ISSN: 0044-2313
    Keywords: New oxides of divalent iron ; structure ; MAPLE ; CHARDI ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Oxides with the “Butterfly-Motive”: Rb6[Fe2O5] and K6[Fe2O5]Rb6[Fe2O5] and K6[Fe2O5] were obtained for the first time by annealing intimate mixtures of “Rb6CdO4” with CdO (molar ratio 1 : 1.1) and KO0.48 with CdO (molar ratio 5.9 : 1) respectively in closed Fe-cylinders. Determination and refinement of the crystalstructure confirms the space group C2/m (four-circle-diffractometer data). Rb6[Fe2O5]: Ag Kα, 720 out of 1220 Io(hkl), R = 9.68%, Rw = 6.09%; a = 718.9pm, b = 1183.1 pm, c = 695.4pm, β = 95.05°, Z = 2; K6[Fe2O5]: MoKα, 1214 Out of 12141o(hkl), R = 3.20070, Rw = 2.48%, a = 691.21 pm, b = 1142.78pm, c = 665.50pm, β = 93.82°, Z = 2. The binuclear unit [O2FeOFeO2]6- already known to be planar with oxoferrates(II) now was observed to be angular here and closely related to Na6[Be2O5].
    Notes: Rb6[Fe2O5] und K6[Fe2O5] wurden erstmals durch Tempern inniger Gemenge von “Rb6CdO4” mit CdO (im Verhältnis 1 : 1,1) bzw. KO0,48 mit CdO (im Verhältnis 5,9 : 1) in verschlossenen Fe-Zylindern in Form von roten Einkristallen erhalten. Die Strukturaufklärung (Vierkreisdiffraktometerdaten, Rb6[Fe2O5]: Ag Kα, 720 von 1 220 Io(hkl), R = 9,68%, Rw = 6,09%; K6[Fe2O5]: Mo Kα, 1 214 von 1 214 Io(hkl), R = 3,20%, Rw = 2,48%) belegt die Raumgruppe C2/m. Rb6[Fe2O5]: a = 718,9 pm, b = 1183,1 pm, c = 695,4 pm, β = 95,05°, Z = 2. K6[Fe2O5]: a = 691,21 pm, b = 1 142,78 pm, c = 665,50 pm, β = 93,82°, Z = 2. Zum ersten Male wird bei derartigen Ferraten eine deutlich gewinkelte Baueinheit [Fe2O5]6- beobachtet, wie sie analog bei Na6[Be2O5] vorliegt.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926180112
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  • 4
    Electronic Resource
    Electronic Resource
    Über ein neues Oxoferrat mit „Butterfly-Motiv“: K2Na4[Fe2O5] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 581-585 
    Details
    ISSN: 0044-2313
    Keywords: New oxide of divalent iron ; structure ; MAPLE ; CHARDI ; VADI ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A New Oxoferrate with “Butterfly-Motiv”: K2Na4[Fe2O5]Dark red-brown single-crystals of K2Na4[Fe2O5] were obtained for the first time by heating “K3Na3CdO4” at 500°C in closed Fe-cylinders. Determination and refinement of the crystal structure confirms the space group P42/mnm (No. 136). Four-circle diffractometer data: MoKα, 373 out of 373 Io(hkl); R = 5.3%; Rw = 4.6%; a = 645.94(5), c = 1 039.2(1) pm.In contrast to the already known oxoferrates(II) with the “Butterfly-Motiv”, Rb6[Fe2O5] and K6[Fe2O5] [1], we now found an isotypic structure for K2Na4[Fe2O5] with the oxocobaltates of Rb2Na4[Co2O5] and K2Na4[Co2O5] [2].
    Notes: Dunkel-rotbraune Einkristalle von K2Na4[Fe2O5] wurden erstmals durch Reaktion mit der Gefäßwand beim Tempern von „K3Na3CdO4“ in verschlossenen Fe-Zylindern bei 500°C erhalten. Die Strukturaufklärung (Vierkreisdiffraktometerdaten: MoKα; 373 von 373 Io(hkl); R = 5,3%; Rw = 4,6%; a = 645,94(5), c = 1 039,2(1) pm) belegt die Raumgruppe P42/mnm (Nr. 136).Im Gegensatz zu den bisher bekannten Oxoferraten(II) mit „Butterfly-Motiv“ Rb6[Fe2O5] und K6[Fe2O5] [1] wird hier eine zu den Oxocobaltaten Rb2Na4[Co2O5] und K2Na4[Co2O5] [2] isotype Struktur gefunden.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200402
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  • 5
    Electronic Resource
    Electronic Resource
    Das erste Oxocobaltat des Typs A2CoIIO2: K2CoO2 = K4[OCoO2CoO] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 586-591 
    Details
    ISSN: 0044-2313
    Keywords: Oxide of divalent cobalt ; structure ; MAPLE ; CHARDI ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The First Oxocobaltate of the Type A2CoIIO2: K2CoO2 = K4[OCoO2CoO]By “reaction with the cylinder surface” of intimate mixtures of K2O and CdO (molar ratio 1:1) in closed Co-Cylinders at 450°C during 73 d dark-red single-crystals of K2CoO2 were obtained.Structure solution and refinement (four-circle diffractometer-data, MoKα, 1 567 independent Io(hkl), none was omitted, R = 3.25%, Rw = 2.67%) result in a monoclinic unit cell containing anions [Co2O4]4- of two connected triangles similar to those of Rb10[CoIO2]2[Co2IIO4]. MAPLE-values and Charge-distributions are given and discussed.
    Notes: Durch „Reaktion mit der Gefäßwand“ von äquimolaren Gemengen aus K2O und CdO in verschlossenen Co-Bomben entstanden während 73 d bei 450°C dunkelrote Einkristalle von K2CoO2.Nach der Strukturaufklärung mittels Vierkreisdiffraktometer (MoKα, alle 1 567 Io(hkl) zur Verfeinerung, R = 3,25%, Rw = 2,67%) liegt eine monokline Elementarzelle vor. Strukturbestimmendes Merkmal sind planare, dimere [Co2O4]4--Einheiten, wie sie analog bei Rb10[CoIO2]2[Co2IIO4] [2] vorliegen. Der Madelunganteil der Gitterenergie, MAPLE, und die Verteilung der Ladungen werden berechnet und diskutiert. Die Gitterkonstanten nach Pulverdaten (Guinier-Simon) betragen: \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{l} a = 651,5(1)\,{\rm pm,}\,b = 952,98(7)\,{\rm pm,}\,c = 695,7(1)\,{\rm pm,}\\ \beta \, = \,117,29(1)^{\circ},\,z = 4.\\ \end{array} $$\end{document}(Standardabweichungen in Einheiten der letzten Stelle in Klammern).
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200403
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  • 6
    Electronic Resource
    Electronic Resource
    Zur kenntnis ‚Kationen-reicher‘ Tantalate und Niobate Über Na5TaO5 und Na5NbO5 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 614 (1992), S. 38-46 
    Details
    ISSN: 0044-2313
    Keywords: Na5TaO5 ; Na5NbO5 ; single crystals ; structure ; MAPLE ; bond length bond strength ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Tantalates and Niobates ‘rich in Cations’. On Na5TaO5 and Na5NbO5Colourless, transparent single crystals of Na5TaO5 [annealed mixtures of Na2O, Li2O, and Ta2O5, Na : Li : Ta = 6.6 : 1.1 : 1, Ni-cylinder, 1000°C, 75 d] as well as Na5NbO5 [annealed mixtures of Na2O, Li2O, and Nb2O5, Na : Li : Nb = 6.6 : 1.1 : 1, Ni-cylinder, 1000°C, 75 d] have been prepared. Single crystal data show that both isotypic oxides represent a deformed variant of the NaCl-type of structure [Na5TaO5: 1154 from 1250 I0 (hkl), four-cycle diffractometer Philips PW 1100, ω2-θ scan, Ag—Kα, R = 4.88%, space group c2/c with a = 629.3(1) pm, b = 1025.4(2) pm, c = 1004.6(2) pm, b̃ 106.80(2)°, z = 4 and Na5NbO5: 998 from 1247 I0(hkl), four-cycle diffractometer Philips PW 1100, ω-2θ scan, Ag—Kα, R = 8.58% and Rw = 7.67%, space group C2/2 with a = 629.1(1) pm, b = 1024.4(2) pm, c = 1004.2(2) pm, b̃ = 106.80(2)°, Z = 4].The Madelung Part of Lattice Energy, MAPLE, and Effective Coordination Numbers, ECoN, the latter derived from Mean Effective Fictive Ionic Radii, MEFIR, as well as Charge Distribution, CHARDI, are calculated.
    Notes: Erstmals wurden farblose, transparente Einkristalle von Na5TaO5 [aus innigen Gemengen von Na2O, Li2O5 und Ta2O5, Einwaage vor dem Verreiben: Na : Li : Ta = 6,6 : 1,1 : 1, Ni-Zylinder, 1000°C, 75 d] sowie erneut solche von Na5NbO5 [aus Gemengen von Na2O, Li2O und Nb2O5, Na : Li : Nb = 6,6 : 1,1 : 1, Ni-Zylinder, 1000°C, 75 d] dargestellt. Nach Einkristalluntersuchungen liegt bei den beiden isotypen Oxiden eine Ordnungsvariante des NaCl-Typs [Na5TaO5: 1154 von 1250 I0(hkl), Vierkreisdiffraktometer Philips PW 1100, ω-2θ scan, Ag—Kα, R = 4,88%, Raumgruppe C2/c mit a = 629,3(1) pm, b = 1025,4(2) pm, c = 1004,6(2) pm, b̃ = 106,80(2)° (Guinier-Simon-Daten), Z = 4 bzw. Na5NbO5: 998 von 1247 I0(hkl), Vierkreisdiffraktometer Philips PW 1100, ω-2θ scan, Ag—Kaα, R = 8,58% und Rw = 7,67%, Raumgruppe C2/c mit a = 629,1(1) pm, b = 1024,4(2) pm, c = 1004,2(2) pm, b̃ = 106,80(2)° (Guinier-Simon-Pulverdaten), Z = 4] vor.Der Madelunganteil der Gitterenergie, MAPLE, und Effektive Koordinationszahlen, ECoN, diese über Mittlere Fiktive Ionenradien, MEFIR, sowie die Ladungsverteilung ‚CHARDI‘ wurden berechnet.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926140809
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  • 7
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    Electronic Resource
    Das erste Oxoferrat(I): Zur Konstitution von K3[FeO2] und K3[NiO2] (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 969-975 
    Details
    ISSN: 0044-2313
    Keywords: Oxide of monovalent Fe and Ni ; preparation ; structure ; MAPLE comparisons ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The First Oxoferrate(I): On the Constitution of K3[FeO2] and K3[NiO2]Garnet-red single crystals of K3[FeO2] were obtained for the first time by heating intimate mixtures of K6[CdO4] and CdO (molar ratio 1:1.16) in closed Fe-cylinders at 450°C during 40 d.The same way of preparation via “reaction with the cylinder surface” was applied to prepare similarly coloured single crystals of K3[NiO2] (K6CdO4 in closed Ni-cylinders at 500°C during 49 d).The structure determination by four circle diffractometer data (MoKα, K3[FeO2]: 731 out of 731 Io(hkl), R = 5.76%, Rw = 5.33%, K3[NiO2]: 755 out of 755 Io(hkl), R = 8.70%, Rw = 4.25%) confirms the space groups P 41212 and P 43212, respectively.K3[FeO2]: a = 604.2(2) pm, c = 1 402.7(3) pm, Z = 4K3[NiO2]: a = 603.6(1) pm, c = 1 405.2(2) pm, Z = 4.(powder data, standard deviations in parentheses)Essential feature of the structure are the dumb-bell-like anions [O—M—O]3- (M = Fe, Ni). Their arrangement corresponds to a stuffed derivative of the KrF2-type. Magnetic properties of K3[FeO2] were determined and cover the monovalence of Fe. MAPLE-calculations reveal the strong coincidence of monovalent VIIIb-cations.
    Notes: K3[FeO2] wurde erstmals in Form granatroter Einkristalle durch 40tägiges Tempern von K6CdO4 und CdO (molares Verhältnis vor dem Verreiben 1:1,16) in verschlossenen Fe-Zylindern bei 450°C dargestellt. Ebenfalls durch „Reaktion mit der Gefäßwand“ wurden isotype, gleichfarbene Einkristalle von K3[NiO2] durch Tempern von K6CdO4 (500°C, 49 d) in verschlossenen Ni-Zylindern erhalten. Die Strukturaufklärung mittels Vierkreisdiffraktometer (K3[FeO2]: MoKα, 731 von 731 Io(hkl), R = 5,76%, Rw = 5,33%, K3[NiO2]: MoKα, 755 von 755 Io(hkl), R = 8,70%, Rw = 4,25%.) verweist auf die beiden zueinander enantiomorphen Raumgruppe P 41212 bzw. P 43212.Die Gitterkonstanten nach Pulverdaten (Guinier-Simon) betragen für K3[FeO2]: a = 604,2(2) pm, c = 1 402,7(3) pm, Z = 4 für K3[NiO2]: a = 603,6(1) pm, c = 1 405,2(2) pm, Z = 4.(Standardabweichungen jew. in Einheiten der letzten Stelle in Klammern.)Die Struktur läßt sich als „aufgefüllte“ KrF2-Variante [2] beschreiben, bei der hantelförmige Anionen [FeO2]3- bzw. [NiO2]3- vorliegen.Die unerwartete Einwertigkeit von Eisen wird zusätzlich durch magnetische Messungen gestützt.Der Madelunganteil der Gitterenergie, MAPLE, wird für die ternären Oxide berechnet und daraus ein Schätzwert für die binären Oxide Fe2O und Ni2O angegeben.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190602
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  • 8
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    K10[Co4O9], ein neues Oxocobaltat(II) mit oligomerem Anion (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1807-1817 
    Details
    ISSN: 0044-2313
    Keywords: New oligooxocobaltate(II) ; structure ; MAPLE ; CHARDI ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: K10[Co4O9], a New Oligooxocobaltate(II)For the first time dark-red single crystals of K10[Co4O9] were obtained by heating mixtures of KO0.48 and CdO (molar ratio 2.7:1) in closed Co-cylinders at 450°C during 73 d.Structure solution and refinement (four-circle diffractometer data, Mo Kα, 2 996 out of 2 996 Io(hkl), R = 5.20%, Rw = 3.03%) confirm the space-group P1 and show structural relationship with Na10[Co4O9] [2]. The lattice constants are a = 667.84(5) pm, b = 917.91(9) pm, c = 908.49(7) pm, α = 119.400(7)°, β = 90.851(7)°, γ = 110.260(6)°, Z = 1. (powder data (Guinier-Simon), standard deviations in parentheses)MAPLE calculations are made and a comparative survey of MAPLE values of oxocobaltates(II) is given.
    Notes: Erstmals wurde K10[Co4O9] in Form dunkelroter Einkristalle durch „Reaktion mit der Gefäßwand“ beim Tempern inniger Gemenge von KO0,48 mit CdO (molares Verhältnis 2,7:1, 73 d, 450°C) in verschlossenen Co-Bomben dargestellt.Die Strukturaufklärung mittels Vierkreisdiffraktometer (Mo Kα, 2 996 von 2 996 Io(hkl), R = 5,20%, Rw = 3,03%) bestätigt die strukturelle Analogie zu Na10[Co4O9] [2].K10[Co4O9] kristallisiert triklin (Raumgruppe P1) mit a = 667,84(5) pm, b = 917,91(9) pm, c = 908,49(7) pm, α = 119,400(7)°, β = 90,851(7)°, γ = 110,260(6)°, Z = 1. (Guinier-Simon-Daten, Standardabweichungen in Klammern)Der Madelunganteil der Gitterenergie, MAPLE, wird berechnet und mit Werten bereits bekannter Oxocobaltate(II) verglichen.
    Additional Material: 9 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936191102
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  • 9
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    Electronic Resource
    Das erste quaternäre Oxocobaltat(I): CsK2[CoO2] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 187-191 
    Details
    ISSN: 0044-2313
    Keywords: Oxide of monovalent cobalt ; structure ; magnetism ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The First Quaternary Oxide of Monovalent Cobalt: CsK2[CoO2]Dark-red single crystals of CsK2[CoO2] were obtained via „reaction with the cyliner surface“ by heating powders of Cs2K2Cd3O5 in closed Co-cylinders at 500°C during 48 d.Structure solution and refinement (four-circle diffractometer data, MoKα, 147 independent Io(hkl), none was omitted, R = 3.42%, Rw = 2.24%) show close relationship with RbNa2[NiO2] [2].The lattice-constants are: \documentclass{article}\pagestyle{empty}\begin{document}$$ a{\rm = 529.506(5) pm, }c{\rm = 986.18(1) pm, }Z{\rm = 2}{\rm .} $$\end{document} (powder data, standard deviations in parentheses) MAPLE calculations, investigations of magnetism and EPR measurement add to the monovalence of Co.
    Notes: Tiefdunkelrote Einkristalle von CsK2[CoO2] entstanden durch „Reaktion mit der Gefäßwand“ von vorgetempertem Cs2K2Cd3O5 in verschlossenen Co-Bomben bei 500°C während 48 d.Die Strukturaufklärung mittels Vierkreisdiffraktometer (MoKα, alle 147 symmetrieunabhängigen Io(hkl) zur Verfeinerung, R = 3,42%, Rw = 2,24%) belegt die strukturelle Analogie zu RbNa2[NiO2] [2], dem ersten quaternären Oxoniccolat(I) der Alkalimetalle.Die Gitterkonstanten nach Pulverdaten (Guinier-Simon) betragen: \documentclass{article}\pagestyle{empty}\begin{document}$$ a{\rm = 529,506(5) pm,}c{\rm = 986,18(1) pm,}Z{\rm = 2}{\rm .} $$\end{document} (Standardabweichungen in Einheiten der letzten Stelle in Klammern)MAPLE-Berechnungen, magnetische Untersuchungen und EPR-Messungen belegen erstmals die Anwesenheit formal einwertigen Cobalts in einem Oxid.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200202
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    Über „Orthoindate“ der Alkalimetalle: Zur Kenntnis von K5[InO4] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 210-224 
    Details
    ISSN: 0044-2313
    Keywords: „Orthoindat“ K5[InO4] ; structure ; MAPLE ; VADI ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A New „Orthoindate“ of an Alkali Metal: K5[InO4]Hitherto unknown K5[InO4] was prepared by heating intimate mixtures of K2O, In2O3 and elementar In (molar ratio 10.0 : 1.0 : 4.0) in closed Ni-cylinders (30 days, 500°C) in form of pale red, nearly colourless, transparent, single crystals. Same crystals were obtained by heating mixtures of K2O, CdO and elementar In (molar ratio 3.1 : 1.0 : 1.0) in closed Ag-cylinders (30 days, 450°C), too. In this case we also found yellow-brown crystals of K14[In4O13] [1]. Structure determination by four circle diffractometer data (MoKα, 15279 out 17454 Io(hkl), R = 5.60%, Rw = 5.25%). Space group P1 with a = 1827.9 pm; b = 1694.4 pm; c = 1329.4 pm; α = 113.3°; β = 111.4°; γ = 105.2°; Z = 16. Characteristic feature of the structure are isolated [InO4]5--tetraeder. The Madelung Part of Lattice Energy, MAPLE, the Mean Fictive Ionic Radii, MEFIR, Effective Coordination Numbers, ECoN, and Charge Distribution, VADI, are calculated.
    Notes: Beim Tempern inniger Gemenge von K2O, In2O3 und elementarem In (10,0 : 1,0 : 4,0) in verschlossenen Ni-Zylindern (30 Tage, 500°C) erhielten wir erstmals K5[InO4] als blaßrote, fast farblose, transparente Einkristalle. Gleichartige Kristalle erhielten wir auch beim Tempern von K2O, CdO und elementarem In (3,1 : 1,0 : 1,0) in verschlossenen Ag-Zylindern (30 Tage, 450°C). Neben den blaßroten Kristallen von K5[InO4] lagen in dieser Probe auch bernsteinfarbene Kristalle von ebenfalls vorher unbekanntem K14[In4O13] [1] vor. Die Strukaufklärung (Vierkreisdiffraktometerdaten, MoKα, 15279 von 17454 Io(hkl), R = 5,60%, Rw = 5,25%) erfolgte in der Raumgruppe P1 mit den Gitterkonstanten: a = 1827,9 pm; b = 1694,4 pm; c = 1329,4 pm; α = 113,28°; β = 111,39°; γ = 105,20°; Z = 16. Für die Struktur sind „isolierte“ [InO4]5--Tetraeder charakteristisch. Der Madelunganteil der Gitterenergie, MAPLE, die mittleren fiktiven Ionenradien, MEFIR, Effektive Koordinationszahlen, ECoN, sowie die Ladungsverteilung werden berechnet.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200205
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