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  • 11
    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.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190320
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  • 12
    Electronic Resource
    Electronic Resource
    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.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936191102
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  • 13
    Electronic Resource
    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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  • 14
    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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  • 15
    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.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190520
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  • 16
    Electronic Resource
    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.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190602
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  • 17
    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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  • 18
    Electronic Resource
    Electronic Resource
    31P chemical shifts and 31P - -13C coupling effects in the stereochemical analysis of benzo-7-phosphanorbornene derivatives (1985)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 23 (1985), S. 929-934 
    Details
    ISSN: 0749-1581
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The first phosphines based on the benzo-7-phosphanorbornene system have been prepared and found to have extremely deshielded 31P nuclei. The phosphine with a P-tert-butyl group gives the most downfield value (δ +152.5) ever recorded for a tertiary phosphine. The lone-pair orientation in phosphines controls the magnitude of 2J (PC) and 3J (PC), and these effects were used to determine stereochemical features of the phosphines. These compounds were formed by HSiCl3—pyridine reduction of the Diels - Alder adducts of isophosphindole oxides with norbornadiene. 13C NMR was also used to confirm the assignment of these phosphine oxides.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1260231110
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