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Schwermetall- und chloridhaltige Filterstäube. I. Phasenanalysen und Modellversuche zum Recycling (1993)

Artelt, Holger M. ; Greinacher, Ekkehard ; Meyer, G.

New York, NY : Wiley-Blackwell

Journal für Praktische Chemie/Chemiker-Zeitung 335 (1993), S. 255-261

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ISSN: 0941-1216

Keywords: Chemistry ; Organic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Flue Dusts Containing Heavy Metal Ions and Chloride.I. Phase Analysis, Model Experiments for RecyclingFour flue dusts from a cement factory, an electric-furnace steelmaking plant and a municipal waste plant were analyzed by powder diffraction methods. Chloride combines above all with alkali ions or heavy metal ions, especially yielding PbCl2 and KPb2Cl5. The controlled sublimation of these chloride compounds in open crucibles was developed and optimized in our laboratory. Between 850°C and 1150°C and at reaction times from 30 min up to 12 h, the chloride content decreases to below 0.1 wt-%. The sublimed phase mainly consists of alkali and lead chloride. Zinc is found in the flue dust as oxide and is enriched during this process. Recent investigations with a small waelz kiln give analogous results. With our procedure, the manufacturer by himself is able to exploit flue dusts containing a large amount of heavy metal elements and chloride which cannot be deposited. The remaining product contains mainly zinc oxide which can be recycled in the zinc industry or returned to the production process. The sublimed chloride compounds may be recycled in the potash industry.

Additional Material: 2 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/prac.19933350307

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Cs2[Pr6(C2)]I12 - das erste quaternäre reduzierte Halogenid mit isolierten [M6(C2)]-ClusternProfessor Harald Schäfer zum 80. Geburtstage gewidmet (1993)

Artelt, Holger M. ; Meyer, Gerd

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 619 (1993), S. 1-6

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ISSN: 0044-2313

Keywords: Lanthanides ; Halides ; Clusters ; Cesium Praseodymium Iodide Dicarbide ; Crystal Structure ; Metal-Metal-Bonding ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: Cs2[Pr6(C2)]I12 - the First Quaternary Reduced Halide with Isolated [M6(C2)] Clusters.Cs2[Pr6(C2)]I12 is obtained as one of the major products from the reaction of PrI3, cesium and carbon in sealed tantalum containers at 850°C. The crystal structure triclinic, P 1; a=948.1(2), b=953.6(3), c=1 005.2(3) pm; α=71.01(2); β=84,68(3), γ=89.37(2)°; Z=1 contains discrete Pr6I12-type clusters elongated along the pseudo-four-fold axis to accommodate the C2 units (d(C - C)=139 pm). The clusters are connected through common i-aI and a-iI linkages at metal vertices and edges according to Cs2[Pr6(C2)iI6i-aI6/2]a-iI6/2. The cesium cations occupy interstices within the (distorted) iodide layers in a way that “Cs2I18” dimers are formed, in which Cs+ is surrounded by eleven I-. On the basis of the MO scheme of [Sc6(C2]I11, the bonding of the C2 unit is discussed and compared with other cluster compounds containing C2 units.

Notes: Cs2[Pr6C2)]I12 entsteht als ein Hauptprodukt bei der Reaktion von PrI3 mit Caesium und Kohlenstoff in verschweißten Tantalampullen bei 850°C. Die Kristallstruktur triklin, P 1; a =948,1(2); b = 953,6(3); c = 1 005,2(3) pm; α = 71,01(2); β = 84,68(3); γ=89,37(2)°; Z=1 beinhaltet isolierte monomere Pr6I12-Cluster, jeweils mit einer C2-Hantel als interstitieller Baueinheit. Aufgrund des Platzanspruches der C2-Einheit (d)(C - C)=139 pm entlang der pseudo-vierzähligen Achse sind die [M6(C2)]-Cluster gestreckt. Die Verbrückung untereinander erfolgt über “normale” Halogenbrücken (i-aI und a-iI), so daß als Verknüpfungsmuster Cs2[Pr6(C2)iI6i-aI6/2]a-iI6/2 resultiert. Die Cs+-Ionen besetzen reguläre Iodidplätze innerhalb der (verzerrten) Iodidschichten, wobei zwei Cs+-Ionen eine “Cs2I18”-Einheit bilden, in der jedes Cs+ von elf Iodid-Ionen umgeben ist. Die Bindungen innerhalb des Clusters werden auf der Basis des MO-Diagramms von [Sc6(C2)]I11 diskutiert und mit anderen Verbindungen verglichen, die ebenfalls eine C2-Hantel als interstitielle Einheit besitzen.

Additional Material: 5 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/zaac.19936190103

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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)

Artelt, Holger M. ; Schleid, Thomas ; Meyer, Gerd

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 620 (1994), S. 1521-1526

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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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Cs3[Tb10(C2)2]Cl21, ein neuer Formel- und Strukturtyp mit isolierten, dimeren Clustern (1994)

Artelt, Holger M. ; Meyer, Gerd

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 620 (1994), S. 1527-1531

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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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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)

Uhrlandt, Stefan ; Meyer, Gerd ; Artelt, Holger M.

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 620 (1994), S. 1532-1536

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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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