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  • 1990-1994  (263)
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  • 1800-1809
  • 1993  (135)
  • 1992  (128)
  • crystal structure  (263)
  • 101
    Electronic Resource
    Electronic Resource
    Darstellung und Aufbau von BaLi[BO3] (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 976-982 
    Details
    ISSN: 0044-2313
    Keywords: Barium lithium orthoborate, BaLi[BO3] ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of BaLi[BO3]For the first time colourless lamellar single crystals of BaLi[BO3] have been prepared from intimate mixtures of BaO2, Li2O and B2O3. The structure determination from four-circle diffractometer data (MoKα, 882 independent reflections, R = 2.4%, Rw = 1.9%) confirms the space group P 21/c with Z = 4; a = 646.1(3), b = 710.7(2), c = 740.3(3) pm, β = 117.99(3)°. Characteristic units of the structure are layers ∞2{Li[BO3]} parallel to (100) consisting of trigonal planar [BO3] groups and distorted [LiO5] pyramids.Effective Coordination Numbers (ECoN), Mean Fictive Ionic Radii (MEFIR), the Madelung Part of Lattice Energy (MAPLE) and the Charge Distribution (CHARDI) are calculated and discussed.
    Notes: Erstmals wurde BaLi[BO3] aus BaO2, Li2O und B2O3 in Form von farblosen, plättchenförmigen Einkristallen erhalten. Die Strukturaufklärung (Vierkreisdiffraktometer, MoKα, 882 symmetrieunabhängige Reflexe, R = 2,4%, Rw = 1,9%) bestätigt die Raumgruppe P 21/c mit Z = 4; a = 646,1(3), b = 710,7(2), c = 740,3(3) pm, β = 117,99(3)°. Die charakteristischen Strukturelemente sind Schichten ∞2{Li[BO3]} parallel (100) aus trigonal planaren [BO3]-Gruppen und verzerrten [LiO5]-Pyramiden.Effektive Koordinationszahlen (ECoN), Mittlere Fiktive Ionenradien (MEFIR), der Madelunganteil der Gitterenergie (MAPLE) und die Ladungsverteilung (CHARDI) werden berechnet und diskutiert.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190603
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  • 102
    Electronic Resource
    Electronic Resource
    Preparation and crystal structure of the La2Ni12P5 and isotypic ternary lanthanoid - Nickel phosphides (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 587-592 
    Details
    ISSN: 0044-2313
    Keywords: Lanthanoid-nickel phosphides ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung und Kristallstruktur von La2Ni12P5 und isotypen ternären Lanthanoid-Nickel-PhosphidenDas neue ternäre Phosphid La2Ni12P5 wurde durch Aufschmelzen reiner Komponenten in einem Lichtbogenofen synthetisiert und seine Kristallstruktur durch Einkristalldaten belegt. La2Ni12P5 ist ein erster Vertreter eines neuen Strukturtyps: Raumgruppe P21/m, a = 10,911(3), b = 3,696(2), c = 13,174(4) Å, β = 108,02(2)°, V = 505,2(6) Å3, Z = 2. Die Lageparameter wurden “anisotrop” aus 1 284 Io(hkl) zu RF = 0,0278, RW = 0,0287 (I 〉 3s̰I; 116 Parameter) verfeinert. Charakteristisch für den Aufbau ist die trigonal-prismatische Koordination der Phosphoratome. Die isotypen Phosphide Ln2Ni12P5 (Ln = Ce, Pr, Nd und Eu) wurden ebenfalls dargestellt und durch Pulverdaten charakterisiert.
    Notes: The new ternary phosphide La2Ni12P5 has been prepared by direct arc melting of the components as pure metals and red phosphorus. The crystal structure has been determined using X-ray single crystal diffraction data. The compound exhibits a new type of crystal structure, P21/m with lattice parameters a = 10.911(3), b = 3.696(2), c = 13.174(4) Å, β = 108.02(2)°, V = 505,2(6) Å3, Z = 2. Atomic parameters least squares refinement of 116 independent variables (anisotropic approximation for thermal vibrations) employed 1 284 independent Io(hkl); RF = 0.0278 and RW = 0.0287. The crystal structure is characterized by trigonal prismatic arrangement of phosphorus atoms stacking variant of infinite (with phosphorus centered) columns built by metal trigonal prisms ‖ [010]. Two or three such columns are connected through common edges (lanthanum atoms). The compounds RE2Ni12P5 (where RE = Ce, Pr, Nd and Eu) display the same with La2Ni12P5 crystal structure. Lattice parameters of these compounds have been refined using powder diffraction data.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190326
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  • 103
    Electronic Resource
    Electronic Resource
    CsPr(CO3)2: Erste Einkristalle eines wasserfreien ternären Selten-Erd-Carbonats (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 2031-2037 
    Details
    ISSN: 0044-2313
    Keywords: Cesium praseodym carbonate ; synthesis ; crystal structure ; IR spectroscopy ; thermal behaviour ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: CsPr(CO3)2: First Single Crystals of an Anhydrous Ternary Rare-Earth CarbonateFor the first time, single crystals of CsPr(CO3)2 were obtained by thermolysis of Cs2(H3O)Pr(CH3COO)6 at 400°C under high CO2 pressure (300 bar) in a steel autoclave. The crystal structure (triclinic, P1, Z = 4, a = 860.2(3), b = 887.4(3), c = 892.6(3) pm, α = 98.56(2), β = 96.19(1), γ = 115.29(2)°, Vm = 90.03(6) cm3/mol, R = 0.033, Rw = 0.029) was determined from four-circle-diffractometer data. CsPr(CO3)2 forms an aragonite like layer structure. Layers containing Cs+ and Pr3+ in a 1 : 1 ratio are stacked in the fashion of the hexagonal closest packing in the [001] direction. They are separated through CO32- ion layers. The Pr3+ ions are surrounded by 8 or 9 oxygen atoms, the coordination numbers of Cs+ are 11 and 12. The site symmetry of the CO32- ions is C1. All bands of the internal vibrations are observed in the IR spectrum. CsPr(CO3)2 decomposes above in 435°C to Cs2CO3 and Pr2O2CO3.
    Notes: Erstmals wurden Einkristalle von CsPr(CO3)2 bei der Thermolyse von Cs2(H3O)Pr(CH3COO)6 bei 400°C unter erhöhtem CO2-Druck (300 bar) in einem Stahlautoklaven erhalten. Die Kristallstruktur triklin, P1, Z = 4, a = 860,2(3), b = 887,4(3), c = 892,6(3) pm, α = 98,56(2), β = 96,19(1), γ = 115,29(2)°, Vm = 90,03(6) cm3/mol, R = 0,033, Rw = 0,029 wurde anhand von Vierkreisdiffraktometerdaten bestimmt. CsPr(CO3)2 bildet eine dem Aragonit verwandte Schichtstruktur: Schichten, die Cs+ und Pr3+ im Verhältnis 1 : 1 enthalten, sind nach dem Motiv einer hexagonal-dichtesten Packung in Richtung [001] gestapelt. Dazwischen liegen Carbonat-Schichten. Die Pr3+-Ionen sind von 8 bzw. 9 Sauerstoffatomen umgeben, die Koordinationszahlen für Cs+ sind 11 bzw. 12. Im Gegensatz zu Aragonit ist in CsPr(CO3)2 die Symmetrie der Carbonat-Ionen C1: Die inneren Schwingungen des CO32--Ions werden alle im IR-Spektrum beobachtet. Thermoanalytische Untersuchungen in Argon-Atmosphäre zeigen, daß CsPr(CO3)2 oberhalb 435°C in Cs2CO3 und Pr2O2CO3 zerfällt.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936191211
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  • 104
    Electronic Resource
    Electronic Resource
    Preparation and crystal structure of Li6Zr2O7 and Li6Hf2O7Dedicated to Professor Dietrich Mootz on his 60th Birthday (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 2038-2042 
    Details
    ISSN: 0044-2313
    Keywords: Lithium zirconate Li6Zr2O7 ; lithium hafnate Li6Hf2O7 ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung und Kristallstruktur von Li6Zr2O7 und Li6Hf2O7Li6Zr2O7 wurde durch Tempern einer innigen Mischung von LiOH · H2O mit frisch hergestelltem ZrO2 im Argonstrom erhalten. Es ist monoklin: C2/c, a = 1 044,5(1), b = 598,9(1), c = 1 020,0(1) pm, β = 100,26(1)°, Z = 4, R = 0,016 für 1 218 F-Werte und 55 Variable. Die Struktur ist eng mit der von NaCl verwandt mit einer geordneten Verteilung der Metallatome auf den Natriumplätzen wobei die Sauerstoffatome sieben Achtel der Chlorpositionen besetzen. Li hat quadratisch-pyramidale, Zr oktaedrische Sauerstoff-Umgebung. Die entsprechende Hf-Verbindung ist isotyp: a = 1 040,2(1), b = 596,2(1), c = 1 015,0(1) pm, β = 100,36(1)°. Die 7Li Kernresonanzspektren von Li6Hf2O7 geben keinen Hinweis auf eine erhöhte Beweglichkeit der Lithiumionen.
    Notes: Li6Zr2O7 was obtained by annealing an intimate mixture of LiOH · H2O and freshly prepared ZrO2 in a stream of argon. It is monoclinic: C2/c, a = 1 044.5(1), b = 598.9(1), c = 1 020.0(1) pm, β = 100.26(1)°, Z = 4, R = 0.016 for 1 218 F values and 55 variables. The structure is closely related to that of NaCl with an ordered distribution of the metal atoms on the sodium sites while the oxygen atoms occupy seven eighths of the chlorine positions. Li has square pyramidal, Zr octahedral oxygen coordination. The corresponding Hf compound is isotypic: a = 1 040.2(1), b = 596,2(1), c = 1 015.0(1) pm, β = 100.36(1)°. 7Li nuclear magnetic resonance spectra of this compound give no indication for a high mobility of the Li+ ions.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936191212
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  • 105
    Electronic Resource
    Electronic Resource
    Darstellung und Kristallstruktur neuer AM2X2-Verbindungen in den Systemen Erdalkalimetall-Platinmetall-GermaniumProfessor Harald Schäfer zum 80. Geburtstage gewidmet. (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 13-16 
    Details
    ISSN: 0044-2313
    Keywords: Earthalkali metal rhodium/ruthenium germanide ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of New AM2X2 Compounds in the Systems Earthalkali Metal/Platinum Metal/Germanium.Four new ternary compounds in the systems earthalkali metal/platinum metal/germanium have been prepared and characterised by single crystal X-ray investigation. BaRu2Ge2 crystallizes orthorhombically, space group Fddd, a=634.4(1) pm, b=1 056.5(3) pm, c=1 273,1(3) pm. SrRu2Ge2 (a=430.6(1) pm, c=1 030.3(2) pm), BaRh2Ge2 (a=418.9(5) pm, c=1 175.7(10) pm) and SrRh2Ge2 (a=418.3(3) pm, c=1 071.8(6) pm) crystallize in the ThCr2Si2-type structure (tetragonal, space group I4/mmm).
    Notes: Vier neue ternäre Verbindungen im System Erdalkalimetall-Platinmetall-Germanium konnten dargestellt und röntgenographisch charakterisiert werden. BaRu2Ge2 kristallisiert orthorhombisch, Raumgruppe Fddd, a=634,4(1) pm, b=1 056,5(3) pm, c=1 273,1(3) pm. Im ThCr2Si2-Typ (tetragonal, Raumgruppe 14/mmm) kristalisieren SrRu2Ge2 (a=430,6(1) pm, c=1 030,3(2) pm), BaRh2Ge2 (a=418,9(5) pm, c=1 175,7(10) pm) und SrRh2Ge2 (a=418,3(3) pm, c=1 071,8(6) pm).
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190105
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  • 106
    Electronic Resource
    Electronic Resource
    Preparation and characterization of Fully stoichiometric SrCoO3 by electrochemical oxidationDedicated to Professor Harald Schäfer on his 80th Birthday. (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 7-12 
    Details
    ISSN: 0044-2313
    Keywords: Strontium cobaltiate(IV), SrCoO3 ; preparation ; crystal structure ; physical properties ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese und Charakterisierung der völlig formelreinen Verbindung SrCoO3 durch elektrochemische Oxidation.Fast formelreines SrCoO3 ist bisher nur unter Anwendung hohen Sauerstoffdrucks dargestellt worden. Es wird ein neues Verfahren zur Herstellung völlig formelreinem SrCoO3 durch elektrochemische Oxidation vorgeschlagen. SrCoO2,50 vom Brownmillerite-Typ wird zu einem vollkommen stöchiometrischen Perowskit oxidiert bei einem Potential von 500 mV in 180 h bei Raumtemperatur in alkalischem Medium (1 M KOH). Die oxidierte Phase hat eine kubische Einheitszelle (a=383,5 pm); sie ist metallisch und zeigt bei Temperaturen unter 280 K ferromagnetisches Verhalten. Das magnetische Moment bei 0 K beträgt 2, 1 μB. Die physikalischen Eigenschaften des SrCoO3,00 werden durch die teilweise Besetzung des σ*egα-Bands erklärt.
    Notes: A nearly stoichiometric SrCoO3 phase had been prepared up to now only using high oxygen pressure. A new method for preparing fully stoichiometric SrCoO3 has been proposed using electrochemical oxidation. Brownmillerite-type SrCoO2.50 is oxidized into a completely stoichiometric perovskite at a potential of 500 mV for 180 hours at room temperature in alkaline media (1 M KOH). The oxidized phase has a cubic unit cell (a=383.5 pm). It is metallic and, at temperatures below T=280 K, it shows ferromagnetic behavior. The magnetic moment at 0 K is 2.1 μB. The physical properties of SrCoO3.00 have been explained in terms of partial occupancy of a σ*egα band.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190104
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  • 107
    Electronic Resource
    Electronic Resource
    Eine Chlorosäure des dreiwertigen Rheniums: Hydroxonium-decachloro-diaqua-trirhenat(III)-pentahydrat, H3O[Re3Cl10(H2O)2] · 5H2O (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 695-698 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium ; crystal structure ; hydrogen-bonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Chloroacid of Trivalent Rhenium: Hydroxonium Decachloro Diaqua Trirhenate(III) Pentahydrate, H3O[Re3Cl10(H2O)2] · 5H2O.A chloroacid of rhenium(III), H3O[Re3Cl10(H2O)2] · 5H2O, was obtained at room temperature from a saturated solution of “ReCl3 · 2H2O” with an excess of NaCl in concentrated hydrochloric acid. The crystal structure (tetragonal, P41212 (Nr. 92); a = 1 150.9(2) pm; c = 1 592.2(6) pm; Z = 4; R = 0.086; Rw = 0.066) has been determined from four-circle diffractometer data. The structure contains isolated cluster anions, [Re3Cl3i,bCl6o,tCli,t (H2O)2i,t]-, which are enclosed by a cage of water molecules. These building units are connected with each other through a “strong” hydrogen-bonding system.
    Notes: Die Chlorosäure H3O[Re3Cl10(H2O)2] · 5H2O kristallisiert aus einer mit NaCl und „ReCl3 · 2H2O“ gesättigten Lösung in konz. Salzsäure bei Raumtemperatur aus. Die Kristallstruktur wurde aus Vierkreis-Diffraktometerdaten bestimmt: tetragonal, P41212 (Nr. 92); a = 1 150,9(2) pm; c = 1 592,2(6) pm; Z = 4; R = 0,086; Rw = 0,066. In der Struktur liegen isolierte, anionische, trimere Einheiten [Re3Cl3i,bCl6o,tCli,t(H2O)2i,t]- vor, welche über „starke“ Wasserstoffbrückenbindungen „käfigartig“ mit Wassermolekülen umgeben und durch diese Hydrathülle miteinander vernetzt sind.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190411
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  • 108
    Electronic Resource
    Electronic Resource
    Einbau von Metallfluoriden in Organoindiumfluoride (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 718-726 
    Details
    ISSN: 0044-2313
    Keywords: Organoindium fluorides ; organoindium fluoride cesium fluoride complexes ; syntheses ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Insertion of Metal Fluorides in Organoindium Fluorides.The reaction of i-Pr2InCl (1) with CsF in acetonitrile at room temperature yields [(i-Pr2InF)5(CsF · 2 MeCN)] ([2 · 2 MeCN]). {[(MesInF2)10MgF2] · 5 toluene} ({3 · 5 toluene}) can be isolated as a by-product in the reaction of Mes3In with BF3 · OEt2 in the presence of MgBrCl. [2 · 2 MeCN] and {3 · 5 toluene} were characterized by NMR spectroscopy as well as by X-ray structure determinations. [2 · 2 MeCN] forms infinite double chains of (i-Pr2InF)5-blocks and CsF-units. The coordination sphere of the cesium atom consists of three fluorine atoms and the nitrogen atoms of three acetonitrile molecules, which wrap the metal atom in a strongly distorted octahedral fashion. One of the acetonitrile molecules in [2 · 2 MeCN] has a μ2-bridging function. This results in the formation of four membered Cs2N2-rings.In {3 · 5 toluene}, ten molecules of MesInF2 are forming a cage in which a linear MgF2-unit is inserted.
    Notes: Die Reaktion von i-Pr2InCl (1) mit CsF in Acetonitril bei Raumtemperatur führt zu [(i-Pr2InF)5(CsF · 2 MeCN)] ([2 · 2 MeCN]).{[(MesInF2)10MgF2] · 5 Toluol} ({3 · 5 Toluol}) kann als Nebenprodukt bei der Umsetzung von Mes3In mit BF3 · OEt2 in der Gegenwart von MgBrCl erhalten werden. [2 · 2 MeCN] und {3 · 5 Toluol} wurden mittels NMR-Methoden sowie durch Röntgenstrukturanalysen charakterisiert. [2 · 2 MeCN] bildet unendliche Doppelstränge aus (i-Pr2InF)5-Blöcken und CsF-Einheiten. Die Koordinationssphäre des Cs-Atoms besteht aus drei F-Atomen und den N-Atomen von drei Acetonitril-Molekülen, was zu einer stark verzerrt oktaedrischen Umgebung des Metallatoms führt. Eines der Acetonitril-Moleküle in [2 · 2 MeCN] hat eine μ2-verbrückende Funktion, woraus sich die Ausbildung von Cs2N2-Vierringen ergibt.In {3 · 5 Toluol} wird ein Käfig aus zehn MesInF2-Einheiten geformt, in welchem eine lineare MgF2-Einheit eingelagert ist.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190414
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  • 109
    Electronic Resource
    Electronic Resource
    Kristall- und Molekülstruktur von SbI3 · 9S3 (9S3 = 1,4,7-Trithiacyclononan) (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 727-730 
    Details
    ISSN: 0044-2313
    Keywords: Antimonytriiodide complex with trithiacyclononane ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal and Molecular Structure of SbI3 · 9S3 (9S3 = 1.4.7-Trithiacyclononane).SbI3 forms a 1:1 adduct with 1.4.7-trithiacyclononane. The crystal structure exhibits discrete complexes with a distorted octahedral coordination of antimony(III). In comparison with molecular SbI3 the Sb—I distances are elongated from 271.9 to 290.4 pm (mean). The mean value of the Sb—S distances is 287.5 pm. The planes through iodine and sulfur atoms, respectively, are nearly coplanar. There is no significant stereochemical influence of the Sb(III) lone pair.
    Notes: SbI3 bildet ein 1:1-Addukt mit 1,4,7-Trithiacyclononan. Die Kristallstruktur enthält diskrete Komplexe mit verzerrt oktaedrischer Koordination von Antimon(III). Im Vergleich zum molekularen SbI3 ist der Sb—I-Abstand von 271,9 auf 290,4 pm aufgeweitet. Der mittlere Sb—S-Abstand beträgt 287,5 pm. Die Ebenen durch die drei Iod- und drei Schwefelatome sind nahezu koplanar. Ein signifikanter stereochemischer Einfluß des nichtbindenden Elektronenpaares von Sb(III) ist nicht zu erkennen.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190415
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  • 110
    Electronic Resource
    Electronic Resource
    Struktur und Eigenschaften von Gd3I3C (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 741-747 
    Details
    ISSN: 0044-2313
    Keywords: Gadolinium iodide carbide, Gd3I3C ; preparation ; X-ray single crystal investigation ; crystal structure ; condensed cluster ; double chain of condensed octahedra ; electrical resistivity ; magnetic susceptibility ; antiferromagnetic order ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structure and Properties of Gd3I3C.The compound Gd3I3C is prepared by reaction of Gd, GdI3 and C (2:1:1 mole) at 1 250 K in sealed Ta tubes. It is obtained as bronze-coloured needles which are air and moisture sensitive. The structure of Gd3I3C contains twin chains of C centered Gd6 octahedra surrounded by I atoms capping all free edges like in the M6X12 cluster. The one-dimensional units are oriented along [010] and linked according to (GdGd1/3Gd2/2Gd2/3C)2I2iI4/2i-iI2/2i-aI2/2a-i. Gd3I3C is metallic in the temperature range 300 K ≥ T ≥ 120 K, between 120 and 15 K the electrical resistance increases by 6 orders of magnitude. At high temperatures the susceptibility follows the Curie-Weiß law with a paramagnetic Curie temperature θ ≈ - 340 K. Two local maxima in the susceptibility at 100 K and 25 K indicate successive formation of antiferromagnetically ordered structures.
    Notes: Gd3I3C wird durch Reaktion von Gd, GdI3 und C (Molverhältnis 2:1:1) bei 1 250 K im verschlossenen Ta-Tiegel erhalten. Es bildet metallisch glänzende, bronzefarbene Nadeln, die gegen Luft und Feuchtigkeit empfindlich sind. Die Struktur von Gd3I3C enthält durch einzelne C-Atome zentrierte Gd6-Oktaeder, die zu Doppelketten kondensiert sind und von den Iod-Atomen über allen freien Kanten nach Art des M6X12-Clusters koordiniert werden. Diese eindimensionalen Einheiten verlaufen längs [010] und sind untereinander nach dem Schema (GdGd1/3Gd2/2Gd2/3C)2I2iI4/2i-iI2/2i-aI2/2a-i verknüpft. Gd3I3C besitzt im Temperaturbereich 300 K ≥ T ≥ 120 K metallisches Verhalten, zwischen 120 und 15 K steigt der elektrische Widerstand um 6 Größenordnungen an. Die magnetische Suszeptibilität läßt sich bei hohen Temperaturen durch das Curie-Weiß-Gesetz mit einer paramagnetischen Curie-Temperatur von θ ≈ - 340 K beschreiben. Zwei lokale Maxima der Suszeptibilität bei 100 K und 25 K weisen auf sukzessive Ausbildung antiferromagnetischer Ordnungsstrukturen hin.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190417
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  • 111
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    Electronic Resource
    (NH4)6Nd(NO3)9, ein ammoniumreiches ternäres Lanthanidnitrat mit einsamen Nitrationen: (NH4)6[Nd(NO3)6](NO3)3Herrn Professor J. Zemann zum 70. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 761-765 
    Details
    ISSN: 0044-2313
    Keywords: Synthesis ; crystal structure ; neodymium ; ternary ammonium nitrate ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: (NH4)6Nd(NO3)9, A Ternary Ammonium-Rich Lanthanide Nitrate with Lonesome Nitrate Ions: (NH4)6[Nd(NO3)6](NO3)3.Single crystals of the ternary ammonium neodymium nitrate (NH4)6Nd(NO3)9 are obtained from a solution of Nd2O3 in a melt of NH4NO3. In the crystal structure (monoclinic, C 2/c, Z = 4, a = 1 775.1(4), b = 912.7(3), c = 2 072.3(5) pm; β = 125.56(1)°; R = 0.059, Rw = 0.036) the Nd3+ ion is surrounded by six bidentate nitrate ligands so that anionic units [Nd(NO3)6]3- are formed. The units are isolated, but they are incorporated in layers parallel to (010). The structure is held together by a network of hydrogen bonds, built up by NH4+ and NO3- ions lying between the layers. Due to the structure, the compound may be described as a double salt like (NH4)3[Nd(NO3)6] · 3 NH4NO3 or, better, as (NH4)6[Nd(NO3)6](NO3)3.
    Notes: Einkristalle des ternären Ammonium-neodymnitrates (NH4)6Nd(NO3)9 erhält man aus der Lösung von Nd2O3 in einer Schmelze von NH4NO3. Die Röntgenstrukturanalyse von (NH4)6Nd(NO3)9 (monoklin, C 2/c, Z = 4; a = 1 775,1(4); b = 912,7(3); c = 2 072,3(5) pm; β = 125,56(1)°; R = 0,059; Rw = 0,036) zeigt, daß Nd3+ von sechs zweizähnigen Nitratliganden in der anionischen Einheit [Nd(NO3)6]3- umgeben ist. Diese isolierten Einheiten sind in Schichten parallel (010) angeordnet. Durch die zwischen den Schichten liegenden NH4+- und NO3--Ionen wird ein Netzwerk von Wasserstoffbrückenbindungen gebildet, das für den Zusammenhalt der Struktur sorgt. Auf Grund des Aufbaus muß die Verbindung nach Art eines Doppelsalzes als (NH4)3[Nd(NO3)6] · 3 NH4NO3 bzw. besser gemäß (NH4)6[Nd(NO3)6](NO3)3 formuliert werden.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190420
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    Metallionenaustausch im System Acetylacetonat/Halogenid/Tetrahydrofuran (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 753-760 
    Details
    ISSN: 0044-2313
    Keywords: Metal bis(acetylacetonate) complexes ; binuclear complexes ; ligand exchange reactions ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Exchange of Metal Ions in the System Acetylacetonate/Halide/Tetrahydrofuran.As bifunctional Lewis bases metal bis(acetyl-acetonates) react with zinc(II) chloride under formation of binuclear complexes (THF)2M(acac)2ZnCl2 (M = Ni, Co, Mg). The octahedral and the tetrahedral centre of these compounds are connected by tridentate oxygen atoms of the two acetylacetonato ligands which are simultaneously part of a four-membered ring MOZnO. The addition is combined with a deformation of the octahedral centre, as a prerequisite of a closest package of the atoms within the MOZnO ring.With mercury(II) chloride the metal bis(acetylacetonates) react as tetrafunctional Lewis bases. In the trinuclear complexes (THF)2M(acac)2(HgCl2)2 (M = Co, Ni, Mg) the interaction between the three coordination centres is weak. No structural change of the octahedral centre (THF)2M(acac)2 is found, but the HgCl2 group diverge slightly from linearity.A ligand exchange was observed in the following cases: (a)Reaction of vanadium(III) chloride with Co(acac)2 under formation of [(THF)2V(acac)2][(THF)CoCl3] (transition of the acetylacetonato ligands to the higher valent central atom).(b)Reaction of magnesium halides with M(acac)2 and formation of (THF)3Mg(acac)2MX2(c)Formation von (THF)3Co(acac)(μ - C1)ZnC12 (V) by the reaction of Zn(acac)2 with cobalt(l1) chlorideIn the complex V the octahedral ccntrc of cobalt(II) is connected with the tetrahedral centre of zinc(I1) by tridentate oxygen atom of the acetylacetonato ligand and a chloro bridge (formation of the four-membered CoClZnO cycle with a closest package of the atoms).A driving force for reaction c is the formation of the stable tetrahedral OZnCI3 group. Important for the li- gand exchange according to c is the stability of the octa- hcdral MgO6 moiety and the easy formation of the tetra- hedral MO2X2 group with a transition metal ion.(THF)3Co(acac)(μ-CI)(HgCl2) (VI) is isoslruclural with V. But there is a marked diffcrence between the bond angles of the tetrahedral central atom including the termi- nal chloro ligands (120.7° for V; 143.7° for VI).The crystal structure of (THF)3Co(acac)(μ-CI)ZnCl2 (V) was determined by X-ray diffraction: monoclinic; space group P2,/n; Z = 4; a = 1 177.4(5); b = 1628.9(4); c = 1284.2(6) pm; β = 99.54(4)°; R = 6.71 % for 2160 observed reflections.
    Notes: Metall-bis(acetylacetonate) fungieren in THF gegenüber Zink(II)-chlorid als bifunktionelle Lewis-Basen und bilden binukleare Komplexe (THF)2M(acac)2ZnCl2 (M = Co, Ni, Mg). Ein oktaedrisches und ein tetraedrisches Zentrum sind über zwei dreibindige Sauerstoffatome der Acetylacetonatliganden miteinander verknüpft (Bildung eines viergliedrigen MOZnO-Rings). Die Addition ist mit einer Deformation des oktaedrischen Zentrums verbunden, die eine dichte Packung der vier Atome des MOZnO-Ringes ermöglicht.Gegenüber Quecksilber(II)-chlorid fungieren die Metall-bis(acetylacetonate) als tetrafunktionelle Lewis-Basen. In den trinuklearen Komplexen (THF)2M(acac)2(HgCl2)2 (M = Co, Ni, Mg) bleibt die Wechselwirkung zwischen den drei Koordinationszentren gering; das oktaedrische Zentrum wird strukturell nicht verändert, die beiden HgCl2-Bausteine weichen nur gering von der Linearität ab.Ein Ligandenaustausch wurde in folgenden Fällen beobachtet: (a)Umsetzung von Vanadium(III)-chlorid mit Co(acac)2 unter Bildung von [(THF)2V(acac)2][(THF)CoCl3] (übergang der Acetylacetonatliganden auf das höherwertige Zentralatom).(b)Umsetzung von Magnesiumhalogeniden mit M(acac)2 unter Bildung von (THF)2Mg(acac)2MX2(c)Bildung von (THF)3Co(acac) (μ - Cl)ZnCl2 (V) aus Zn(acac)2 und Cobalt(II)-chloridIm Komplex V ist das oktaedrische Zentrum am Cobalt über ein dreibindiges Sauerstoffatom des Acetylacetonatoliganden und eine Chlorobrücke mit dem tetraedrischen Zentrum am Zink verknüpft (Bildung eines viergliedrigen CoClZnO-Ringes mit dichtester Packung der Atome).Wesentliche Triebkraft für die Umsetzung gemäß c ist die Bildung der stabilen OZnCl3-Gruppierung. Für den Ligandenaustausch gemäß b ist die Stabilität der oktaedrischen MgO6-Gruppierung und die leichte Bildung der teraedrischen Baugruppe MO2X2 bei den übergangsmetallen maßgebend. (THF)3Co(acac)(μ - Cl)HgCl2 (VI) ist isostrukturell mit V. Deutlich verschieden sind allerdings die Valenzwinkel am tetraedrischen Zentralatom, in die die terminalen Chloroliganden einbezogen sind (120,7° für V; 143,7° für VI).Die Kristallstruktur von (THF)3Co(acac)(μ - Cl)ZnCl2 (V) wurde durch Röntgenbeugung bestimmt: monoklin, Raumgruppe P21/n, Z = 4; a = 1 177,4(5); b = 1 628,9(4); c = 1 284,2(6) pm; β = 99,54(4)°; R = 6,71% für 2 160 beobachtete Reflexe.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190419
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    Neue Alkalioxoarsenate(V): NaLi2[AsO4]  -  ein neuer Formeltyp [1] (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 766-770 
    Details
    ISSN: 0044-2313
    Keywords: Mixed alkali orthoarsenate, NaLi2[AsO4] ; crystal structure ; MAPLE calculation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Alkali Oxoarsenates(V): NaLi2[AsO4]  -  A New Type of Formula [1].By heating of well ground mixtures of the binary oxides As2O3, Na2O, and Li2O2, molar ratio As:Na:Li = 1.0:1.0:2.0, in a well closed Ni tube (650°C, 21 d) colourless single crystals of NaLi2[AsO4] were obtained for the first time. The new orthoarsenate(V) crystallizes orthorhombic (space group P mn21-C2v7, No. 31) with Z = 2. The structure determination showed that it is isostructural to βII-Li3[VO4] and that means the Li3[PO4]-type. The lattice constants a = 702.9(2) pm, b = 520.5(1) pm, c = 505.4(2) pm were taken from Guinier-Simon powder data. The structure was determined by four-circle diffractometer data [Philips PW 1 100, AgKα, 679 independent out of 2 373 Io(hkl), R = 3.03%, Rw = 2.29%; parameter see text]. The Madelung Part of Lattice Energy, MAPLE, and Effective Coordination Numbers, ECoN, these calculated via Mean Fictive Ionic Radii, MEFIR, are calculated and discussed.
    Notes: Zur Synthese von NaLi2[AsO4] wurden innige Gemenge der binären Ausgangskomponenten As2O3, Na2O und Li2O2 im Molverhältnis As:Na:Li = 1,0:1,0:2,0 in einer fest verschlossenen Ni-Bombe, diese in einer Ampulle aus Supremax-Glas eingeschmolzen, bei 650°C 21 Tage getempert. NaLi2[AsO4] fiel in Form plättchenförmiger, farbloser Einkristalle an. Das neue Orthoarsenat kristallisiert orthorhombisch (Raumgruppe P mn21-C2v7, Nr. 31) mit Z = 2. Die Strukturaufklärung ergab Isotypie zu βII-Li3[VO4] mit a = 702,9(2) pm, b = 520,5(1) pm, c = 505,4(2) pm (Guinier-Simon-Daten). Die Struktur wurde über Vierkreisdiffraktometerdaten [Philips PW 1 100, AgKα, 679 symmetrieunabhängige aus 2 373 Io(hkl), R = 3,03%, Rw = 2,29%; Parameter siehe Text] bestimmt. Der Madelunganteil der Gitterenergie, MAPLE, und Effektive Koordinationszahlen, ECoN, diese über fiktive Ionenradien, MEFIR, werden berechnet und diskutiert.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190421
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    Synthese und Kristallstruktur des tetrameren Nitridokomplexes [Cu(CH3CN)4]2[W4N4Cl14(CH3CN)2] (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 775-778 
    Details
    ISSN: 0044-2313
    Keywords: Nitrido complex of tungsten ; synthesis ; IR-spectrum ; 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 the Tetrameric Nitrido Complex [Cu(CH3CN)4]2[W4N4Cl14(CH3CN)2].The title compound has been prepared by the reaction of CuCl with WNCl3 in acetonitrile solution, forming red, moisture sensitive crystals. They were characterized by IR spectroscopy and by an X-ray structure determination. Space group I2/a, Z = 4, 2 027 observed unique reflections, R = 0.049. Lattice dimensions at -80°C: a = 2 527.0, b = 971.9, c = 2 137.5 pm, β = 106.01°. The compound consists of [Cu(CH3CN)4]+ ions, which are arranged to form strands, and of anions [W4N4Cl14(CH3CN)2]2-, in which the tungsten atoms were located at the vertices of a square and are linked with one another via linear W≡N—W bridges. Two of the four tungsten atoms have four chlorine atoms as terminal ligands, the other two tungsten atoms have three chlorine atoms and an acetonitrile molecule as terminal ligands.
    Notes: Die Titelverbindung wird durch Umsetzung von Kupfer(I)chlorid mit WNCl3 in Acetonitril in Form roter feuchtigkeitsempfindlicher Kristalle gewonnen. Sie wird durch das IR-Spektrum und eine röntgenographische Strukturanalyse charakterisiert. Raumgruppe I2/a, Z = 4, 2 027 beobachtete unabhängige Reflexe, R = 4,9%. Gitterkonstanten bei -80°C: a = 2 527,0; b = 971,9; c = 2 137,5 pm; β = 106,01°. Die Verbindung besteht aus [Cu(CH3CN)4]+-Ionen, die zu Strängen angeordnet sind, und Anionen [W4N4Cl14(CH3CN)2]2-, in denen die Wolframatome an den Ecken eines Quadrats angeordnet sind und über lineare W≡N—W-Brücken verknüpft sind. Zwei der Wolframatome haben je vier Chloratome als terminale Liganden, die beiden anderen je drei Chloratome und je ein N-Atom eines Acetonitrilmoleküls als terminale Liganden.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190423
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    Die Kristallstruktur von Bis(N,N-Diethyl-N′-benzoylselenoureato)zink(II) (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 786-790 
    Details
    ISSN: 0044-2313
    Keywords: Bis(N,N-diethyl-N′-benzoylselenoureato)-zinc(II) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Bis(N,N-Diethyl-N′-benzoylselenoureato)zinc(II).Zn(C12H15N2OSe)2 crystallizes in the acentric orthorhombic space group Pca21. The cell parameters are a = 16.914(5), b = 13.492(4), c = 11.705(5) Å and Z = 4. The structure was solved with Patterson and direct methods and was refined to a final R-value of 7,05%. ZnII is coordinated to two N,N-Diethyl-N′-benzoylselenoureato molecules, which are bidentately coordinated through their oxygen and selenium atoms to form a distorted tetrahedron. The Zn—Se bond lenghts are 2.394(3) and 2.369(4) Å, the Zn—O bond lengths are 1.971(11) and 1.974(12) Å.
    Notes: Zn(C12H15N2OSe)2 kristallisiert in der azentrischen orthorhombischen Raumgruppe Pca21 mit den Gitterkonstanten a = 16,914(5), b = 13,492(4), c = 11,705(5) Å, Z = 4. Die Struktur wurde mit Patterson und Direkten Methoden gelöst und bis zu einem R-Wert von 7,05% verfeinert. Zink bildet mit dem Liganden N,N-Diethyl-N′-benzoylselenoharnstoff einen bidental koordinierten Komplex, in dem zwei Ligandmoleküle über Selen und Sauerstoff in Form eines verzerrten Tetraeders an das Zentralatom gebunden sind. Die Zn—Se-Abstände betragen 2,394(3) und 2,369(4) Å, die Zn—O-Abstände 1,971(11) und 1,974(12) Å.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190425
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    Die Kristallstruktur von Bis(N,N-Diethyl-N′-benzoylselenoureato)cadmium(II) (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 791-795 
    Details
    ISSN: 0044-2313
    Keywords: Bis(N,N-Diethyl-N′-benzoylselenoureato)-cadmium(II) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Bis(N,N-Diethyl-N′-benzoylselenoureato)cadmium(II).Cd(C12H15N2OSe)2 exists in a dimeric oxygen bridged form and crystallized in the monoclinic space group P21/n. The cell parameters are a = 12.506(3), b = 11.563(2), c = 18.924(4) Å, β = 91.59(3)°, Z = 4. The structure was solved with Patterson and direct methods and was refined to a final R-value of 6.58%. Cadmium is coordinated by 3 oxygen and 2 selenium atoms and exhibits the unusual coordination number 5. The coordination polyhedron is a distorted trigonal bipyramid, to bipyramids are connected by a common edge. The Cd—Se bond lengths are 2.591(1) and 2.565(1) Å, the Cd—O bond lengths are 2.263(6), 2.272(5) und 2.438(5) Å.
    Notes: Cd(C12H15N2OSe)2 liegt als sauerstoff-verbrücktes Dimer vor und kristallisiert in der monoklinen Raumgruppe P21/n mit den Gitterkonstanten a = 12,506(3), b = 11,563(2), c = 18,924(4) Å, β = 91,59(3)°, Z = 4. Die Struktur wurde mit Patterson und Direkten Methoden gelöst und bis zu einem R-Wert von 6,58% verfeinert. Die Cadmiumatome sind von jeweils 3 Sauerstoff- und 2 Selenatomen koordiniert und besitzen die ungewöhnliche Koordinationszahl 5. Das Koordinationspolyeder ist eine verzerrte trigonale Bipyramide, zwei Bipyramiden sind über eine gemeinsame Kante miteinander verknüpft. Die Cd—Se Abstände betragen 2,591(1) und 2,565(1) Å, die Cd—O Abstände 2,263(6), 2,272(5) und 2,438(5) Å.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190426
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    Crystal structure of trans-pyH[MoBr4py2] and reactivity of Trans-pyH[MBr4py2] (M = Mo, W; py = pyridine) towards nitrogen ligands and bromine Oxidation (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 796-800 
    Details
    ISSN: 0044-2313
    Keywords: Molybdenum / tungsten complexes ; pyridinium molybdenum / tungsten tetrabromine complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kristallstruktur von trans-pyH[MoBr4py2] und die Reaktivität von trans-pyH[MBr4py2] (M = Mo, W; py = Pyridin) gegenüber Stickstoff-Liganden und zur Oxidation mit Brom.Die Kristallstruktur von trans-pyH[MoBr4py2] wurde bestimmt: orthorhombisch, Pnma (No. 62), a = 16,197(3), b = 13,995(3), c = 8,615(1) Å, Z = 4, Dgemess. = 2,20(3), Dröntg. = 2,23 g/cm3, V = 1953(1) Å3. R1, Rw = 0,057 and 0,053. Trans-[MoBr4py2]-, mit der gestaffelten Konformation der Pyridin-Liganden in der Spiegelebene. Mo—Br- und Mo—N(Pyridin)-Abstände sind 2,593(1), 2,573(1), 2,227(8) und 2,213(7) Å. Die Kationen befinden sich in den Symmetriezentren.Das Kation in trans-pyH[MBr4py2] ist ersetzbar; trans-NH4[MBr4py2] · H2O, Cs[MBr4py2], LH[MBr4py2] (M = Mo, W; L = 4-Methylpyridin, 4-pic; 2,2′-Bipyridyl, bipy) wurden dargestellt. Die Molybdän- und Wolfram-Verbindungen analoger Zusammensetzung sind isostrukturell. Alle Stoffe reagieren mit Pyridin und 4-Methyl-pyridin zu trans-MBr3L3 und im Fall des Molybdäns auch zu trans-MoBr3py2(4-pic). Brom oxidiert trans-MI[MBr4py2] zu trans-MBr4py2.
    Notes: The crystal structure of trans-pyH[MoBr4py2] has been determined: orthorhombic, Pnma (No. 62), a = 16.197(3), b = 13.995(3), c = 8.615(1) Å, Z = 4, Dc = 2.23, Do = 2.20(3) g/cm3, V = 1 953(1) Å3. R1, Rw = 0.057 and 0.053. Trans-[MoBr4py2]- anions with staggered conformation of pyridine rings are located on the mirror planes. Mo—Br, Mo—N(pyridine) distances are 2.593(1), 2.573(1), 2.227(8) and 2.213(7) Å. Cations are located on the symmetry centers.The cation in trans-pyH[MBr4py2] can be replaced. Trans-NH4[MBr4py2] · H2O, Cs[MBr4py2], LH[MBr4py2] (M = Mo, W; L = 4-methylpyridine, 4-pic; 2,2′-bipyridyl, bipy) were prepared. The compounds of molybdenum and tungsten with the same chemical composition are isostructural. All compounds react with pyridine and 4-methylpyridine. The products are trans-MBr3L3, and in the case of molybdenum, also trans-MoBr3py2(4-pic). Bromine oxidizes trans-MI[MBr4py2] to trans-MBr4py2.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190427
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    [Na · Triglyme]2[S(BH3)4]: Ein Salz des neuen Anions Tetrakis(boran)sulfat(2 - ) Kristallstruktur und theoretische Untersuchung der MolekülstrukturProfessor Heinrich Nöth zum 65. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1353-1359 
    Details
    ISSN: 0044-2313
    Keywords: Bis[triglymesodium(1+)][Tetrakis(borane)sulfate(2-)], [Na · Triglyme]2[S(BH3)4] ; preparation ; crystal structure ; SCF calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Na · Triglyme]2[S(BH3)4]: a Salt of the New Anion Tetrakis(borane)sulfate(2- ). Crystal Structure and Theoretical Investigation of the StructureNa[H3B-m̈2-S(B2H5)] 1 is produced by the reaction between NaSH and THF · BH3, under dehydrogenation. 1 is also formed as the first 11B-NMR-spectroscopically detectable reaction product by the reaction between anhydrous Na2S and THF · BH3. Adducts of BH3 with the S2- ion are not detectable in THF. The anion [S(BH3)4]2- can however be obtained, by the addition of NaBH4 to 1 in diglyme or triglyme respectively: [Na  -  Triglyme]2[S(BH3)4] 2. 2 crystallizes in the monoclinic space group P21/n (Nr. 14). Structural data of 1 and 2 have been calculated by SCF methods. The anion of 2 may be viewed either as an adduct of B2H6 with S2-, or as a bridge substituted thia derivative of B2H7-; furthermore the anion of 2 is isoelectronic and isostructural with the SO42- ion.
    Notes: Bei der Reaktion zwischen NaSH und THF · BH3 entsteht unter H2-Abspaltung Na[H3B-m̈2-S(B2H5)] 1. 1 entsteht auch als erstes 11B-NMR-spektroskopisch nachweisbares Reaktionsprodukt bei der Reaktion zwischen wasserfreiem Na2S und THF · BH3. Addukte von BH3 an das S2--Ion lassen sich in THF als Lösungsmittel nicht nachweisen. Das neue Anion [S(BH3)4]2- kann jedoch durch Addition von NaBH4 an 1 in Diglyme bzw. Triglyme erhalten werden: [Na · L]2[S(BH3)4] 2. 2 kristallisiert monoklin in der Raumgruppe P21/n (Nr. 14). Aus SCF-Rechnungen erhielten wir die Strukturparameter für 1 und 2. Das Anion von 2 kann sowohl als Addukt von B2H6 an S2- als auch als brückensubstituiertes Thia-Derivat des B2H7--Ions aufgefaßt werden; ferner ist es isoelektronisch und isostrukturell mit dem SO42-- Ion.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190806
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    Synthese und Bau von (4-Picolinium)2[LnCl4(H2O)3]Cl (Ln = Eu, Ho)Professor Hans Joachim Berthold zum 70. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1393-1396 
    Details
    ISSN: 0044-2313
    Keywords: Preparation ; crystal structure ; complex chlorides of lanthanides ; pentagonal bipyramid ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Structure of (4-Picolinium)2[LnCl4(H2O)3]Cl (Ln = Eu, Ho)The complex water containing chlorides (4-Picolinium)2[LnCl4(H2O)3]Cl (Ln = Eu, Ho) were prepared for the first time. The crystal structures were determined on single crystals by X-ray methods. The isotypic compounds crystallize with triclinic symmetry, space group P-1, Z = 2. Surprisingly the structures contain the complex anions [LnCl4(H2O)3]- (Ln = Eu, Ho) where the ligands form a distorted pentagonal bipyramid, which to our knowledge has not been observed in lanthanide compounds till now.
    Notes: Die komplexen wasserhaltigen Chloride (4-Picolinium)2[LnCl4(H2O)3]Cl (Ln = Eu, Ho) wurden erstmals dargestellt und die Kristallstrukturen anhand von röntgenographischen Einkristalluntersuchungen bestimmt. Die isotypen Verbindungen kristallisieren in der triklinen Raumgruppe P1, Z = 2. Überraschend sind die Liganden in den komplexen Anionen [LnCl4(H2O)3]- (Ln = Eu, Ho) in Form einer verzerrten pentagonalen Bipyramide angeordnet, die unseres Wissens bislang bei keiner Lanthanidverbindung beobachtet wurde.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190813
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    Synthese, Eigenschaften und Struktur von oktamerem Titanimidchlorid [Ti(NSiMe3)Cl2]8Professor Heinrich Nöth zum 65. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1526-1529 
    Details
    ISSN: 0044-2313
    Keywords: Octameric titanium imide chloride, [Ti(NSiMe3)Cl2]8 ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Properties, and Structure of Octameric Titanium Imide Chloride [Ti(NSiMe3)Cl2]8The reaction of TiCl4 with N(SiMe3)3 in sealed glas-tubes yields the titanium imide chloride [Ti(NSiMe3)Cl2]8 (1). It crystallizes in the space group C2/c with a = 2 704.5(4), b = 1 303.9(1), c = 2 205.4(2) pm, β = 112.78(1)°, Z = 4. In 1 six Ti atoms are linked together by chloro and trimethylsilylimido bridges to form a ring structure. Two TiCl2-groups are bound in addition to the ring by two imido bridges. Upon annealing at 250°C 1 transformes to the isomeric polymer [Ti(NSiMe3)Cl2]n. Above 250°C 1 decomposes under separation of Me3SiCl affording TiNCl.
    Notes: TiCl4 reagiert in zugeschmolzenen Glasampullen mit N(SiMe3)3 zum Titanimidchlorid [Ti(NSiMe3)Cl2]8 (1). Es kristallisiert monoklin in der Raumgruppe C2/c mit a = 2 704,5(4), b = 1 303,9(1), c = 2 205,4(2) pm, β = 112,78(1)°, Z = 4. In 1 sind sechs Titanatome über Chloro- und Trimethylsilylimido-Brücken zu einer Ringstruktur verknüpft. Zusätzlich sind zwei TiCl2-Gruppen über zwei Imidobrücken an dß Ring gebunden. Durch Tempern bei 250°C wird 1 in das isomere Polymer [Ti(NSiMe3)Cl2]n umgewandelt. Oberhalb 250°C zersetzt sich 1 unter Abspaltung von Me3SiCl zu TiNCl.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190906
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    Darstellung und Kristallstruktur von Cs8P8O24 · 8H2O (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1633-1638 
    Details
    ISSN: 0044-2313
    Keywords: Cesium cyclooctaphosphate octahydrate ; preparation ; 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 Cs8P8O24 · 8H2OCs8P8O24 · 8H2O was obtained from Na8P8O24 · 6H2O by cation exchange. Crystal growth was achieved by applying gel techniques (agar agar). The crystal structure (P1; a = 766.6(8); b = 1 156.9(9); c = 1 163.4(9) pm; α = 100,2(1)°; β = 106.5(2)°; γ = 92.2(1)°; Z = 1; 4 099 unique diffractometer data; R = 0.051; R(w) = 0.037) contains cyclo-octaphosphate anions with point symmetry C2h. The cesium atoms are coordinated irregularily by eight and ten oxygen atoms, respectively. The threedimensional linkage of the P8O248--rings is established via bonds to cesium atoms and hydrogen bonds Provided by H2O molecules.
    Notes: Cs8P8O24 · 8H2O wurde durch Kationenaustausch aus dem entsprechenden Natriumsalz gewonnen. Die Kristallzüchtung erfolgte diffusionskontrolliert (Agar-Agar-Gel). Die Kristallstruktur (P1; a = 766,6(8); b = 1 156,9(9); c = 1 163,4(9) pm; α = 100,2(1)°; β = 106,5(2)°; γ = 92,2(1)°; Z = 1; 4 099 unabhängige Reflexe; R = 0,051; R(w) = 0,037) enthält cyclo-Octaphosphatanionen mit der Punktsymmetrie C2h. Caesium ist unspezifisch mit 8 bzw. 10 Sauerstoffatomen koordiniert. Die dreidimensionale Verknüpfung der Ringe erfolgt über Koordination an Caesium und über Wasserstoffbrückenbindungen ausgehend vom Kristallwasser.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190921
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    Structural links between zeolite-type and clathrate hydrate-type materials: Synthesis and crystal Structure of [N(CH3)4]6[AlxSi8-xO18-x(OH)2+x] · 44H2O (x = 3-4) (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1098-1104 
    Details
    ISSN: 0044-2313
    Keywords: Tetramethylammonium alumosilicate hydrate ; crystal structure ; zeolite ; clathrate hydrate ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Strukturelle Bindeglieder zwischen zeolithartigen und clathrathydratartigen Materialien: Synthese und Kristallstruktur von [N(CH3)4]6[AlxSi8-xO18-x(OH)2+x] · 44H2O (x = 3-4)Ein neues Tetramethylammoniumalumosilicat-Hydrat mit der ungefähren Zusammensetzung [NMe4]6[AlxSi8-xO18-x(OH)2+x] · 44H2O (x = 3-4) wurde mittels Röntgenpulverbeugung als eine Komponente eines mehrphasigen festen Gemisches erkannt, das bei Raumtemperatur aus einer wäßrigen NMe4OH—Al2O3—SiO2 Lösung kristallisierte. Große Kristalle der neuen Hydratphase konnten mechanisch aus dem Gemisch ausgelesen werden. Die Kristallstruktur wurde mit 1 196 unabhängigen MoKα-Beugungsdaten, gemessen bei 180 K, bestimmt: Tetragonales Kristallsystem; Zellkonstanten a = 16,181(4) und c = 17,450(4) Å; Raumgruppe P4/mnc mit Z = 2 Formeleinheiten pro Elementarzelle; R = 0,072. Die Wirt-Gast-Verbindung ist vom Typ eines polyedrischen Clathrats mit einem gemischten dreidimensionalen, (im wesentlichen) vierbindigen Netzwerk aus oligomeren Alumosilicat-Anionen [AlxSi8-xO18-x(OH)2+x]6- und H2O-Molekülen, die über Wasserstoffbrücken O—H … O miteinander verknüpft sind. Die Alumosilicat-Anionen besitzen würfelförmige (Doppelvierring-)Struktur. Orientierungsfehlgeordnete kationische Gastspezies NMe4+ befinden sich in den großen polyedrischen Hohlräumen, [4668] und [4151067], der Wirtstruktur; die kleinen [46] Käfige (d.h. die Doppelvierring-Anionen) und [4356] Käfige sind leer. Das Hydrat ist ein weiteres Glied in einer kürzlich aufgefundenen Serie von Clathraten mit gemischten tetraedrischen Netzwerken, wodurch strukturchemisch eine Verbindung zwischen zeolith- und clathrathydratartigen Wirt-Gast-Verbindungen hergestellt wird.
    Notes: A novel tetramethylammonium aluminosilicate hydrate with the approximate composition [NMe4]6[AlxSi8-xO18-x(OH)2+x] · 44H2O (x = 3-4) has been identified by powder X-ray diffraction as a component in a polyphasic solid mixture which crystallized at room temperature from an aqueous NMe4OH—Al2O3—SiO2 solution. Large crystals of the novel hydrate phase could be mechanically selected from that mixture. The crystal structure has been determined from 1 196 unique MoKα diffraction data measured at 180 K: Tetragonal crystal system, cell constants a = 16.181(4) and c = 17.450(4) Å, space group P4/mnc with Z = 2 formula units per unit cell, R = 0.072. The host-guest compound is of polyhedral clathrate type with a mixed three-dimensional, (mainly) four-connected network composed of oligomeric aluminosilicate anions [AlxSi8-xO18-x(OH)2+x]6- and H2O molecules linked via hydrogen bonds O—H … O. The aluminosilicate anions possess a cube-shaped (double four-ring) structure. Orientationally disordered cationic guest species NMe4+ are enclosed in the large [4668] and [4151067] polyhedral voids of the host framework; the small [46] cages (i.e. the double four-ring anions) and [4356] cages are empty. The hydrate is a further member in a recently discovered series of clathrates with mixed tetrahedral networks, which provides a structure-chemical link between zeolite- and clathrate hydrate-type host-guest compounds.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190622
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    Tris(trimethylsilyl)methanselenenylhalogenide und -chalkogenideProfessor Heinrich Nöth zum 65. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1693-1698 
    Details
    ISSN: 0044-2313
    Keywords: Tris(trimethylsilyl)methaneselenenyl halides ; Tris(trimethylsilyl)methaneselenyl chalcogenides ; 1H, 13C, 77Se n.m.r. sprectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tris(trimethylsilyl)methaneselenenyl Halides and Chalcogenides.Ditrisyldiselenide (1) (trisyl = TSi = (Me3Si)3C) reacts with SOCl2, Br2 and I2 to provide trisylselenenyl halides TSiSeX (2: X = Cl; 3: X = Br, 4: X = I). Insertion of S and Se into the Se—Se bond of 1 to yield (TSiSe)2Sn (5: n = 1; 6: n = 2) and (TSiSe)2Sen (7: n = 1; 8: n = 2) was catalysed by iodine. 5 was isolated in pure state and examined by X-ray diffraction. Triselenide 7 can be cleaved by I2 in CS2 to give 4 and Se2I2 (9). From 2 with Me3SiCN and Me3SiNCS, the new selenenyl pseudohalides TSiSeCN (10) and TSiSeSCN (11) were prepared. The compounds were characterised by 1H, 13C- and 77Se n.m.r. spectra.
    Notes: Ditrisyldiselenid (1) (Trisyl  -  Tsi  -  (Me3Si)3C—) reagiert mit SOCl2, Br2 und I2 zu Trisylselenenylhalogeniden TSiSeX (2: X = Cl; 3: X = Br, 4: X = I). Die Einschiebung von Schwefel und Selen in die Se—Se-Bindung von 1 zu (TSiSe)2 Sn (5: n = 1; 6: n = 2) bzw. (TSiSe)2Sen (7: n = 1; 8: n = 2) läßt sich mit Iod katalysieren. 5 wurde in reiner Form isoliert und durch Röntgenstrukturanalyse untersucht. Das Triselenid 7 wird durch Iod in CS2 zu 4 und Se2I2 (9) gespalten. Aus 2 lassen sich mit Me3SiCN bzw. Me3SiNCS das Trisylselenocyanat TSiSeCN (10) bzw. Trisylselenenylthiocyanat TSiSeSCN (11) gewinnen. 1H, 13C- und 77Se-NMR Spektren von 1 - 11 sind im Einklang mit den Strukturvorschlägen.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936191011
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    M3NS3, die ersten Nitridsulfide der Lanthanide (M = La—Nd, Sm) (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1771-1776 
    Details
    ISSN: 0044-2313
    Keywords: Lanthanides ; nitride sulfides ; La3NS3 ; Ce3NS3 ; Pr3NS3 ; Nd3NS3 ; Sm3NS3 ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: M3NS3, the First Nitride Sulfides of the Lanthanides (M = La—Nd, Sm).The oxidation of the “light” lanthanides (M = La—Nd, Sm) with equimolar amounts of sulfur in the presence of NaN3 as nitrogen source results in the formation of the first lanthanide nitride sulfides: M3NS3 (evacuated silica vessels, some NaCl as flux, 850°C, 7 d). NaCl is afterwards removed from the not moisture sensitive crude product (faint- or orange-yellow to amber-co- loured transparent needles, oftenly intergrown to feltlike bunches) upon rinsing with water.The crystal structure was determined from X-ray single crystal data for the example of Sm3NS3 (orthorhombic, Pnma (no. 62), a = 1 201.18(7), b = 394.32(3), c = 1 285.27(6) pm, Z = 4, R = 0.027, Rw = 0.024), and M3NS3 (M = La—Nd) proved to be isostructural from Guinier powder data. There are three crystallographically different M3+ cations in six- (1 X) and sevenfold (2 X) coordination of the N3- and S2- anions. [(N3-)(M3+)4] tetrahedra connected via two corners forming linear chains ∞1[N(M1)1/1(M2)1/1(M3)2/2] 6+ build up the main structural feature. Arranged in the manner of a closest packing of rods, they are held together by three crystallographically different S2- which take care for charge neutrality and three-dimensional interconnection.
    Notes: Die Oxidation der “leichten” Lanthanide (M = La—Nd, Sm) mit äquimolaren Mengen an Schwefel in Gegenwart von NaN3 als Stickstoff-Quelle liefert die ersten Nitridsulfide der Lanthanide: M3NS3 (evakuierte Quarzampullen, etwas NaCl als Flußmittel, 850°C, 7 d). NaCl wird anschließend mit Wasser aus dem hydrolyse-unempfindlichen Rohprodukt (sehr feine, blaß- bzw. orange-gelbe bis bernsteinfarbene, transparente Nadeln, oft zu filzartigen Büscheln verwachsen) her- ausgelöst.Die Kristallstruktur wurde über Einkristalldaten am Beispiel von Sm3NS3 (orthorhombisch, Pnma (Nr. 62); a = 1 201,18(7), b = 394,32(3), c = 1 285,27(6) pm, Z = 4, R = 0,027, Rw = 0,024) bestimmt. Alle dargestellten Nitridsulfide (M3NS3, M = La—Nd) sind nach Guinier-Pulveraufnahmen isotyp. In der Struktur liegen drei kristallographisch unterschiedliche M3+-Kationen in sechs (1 X) bzw. siebenfacher (2 X) Koordination der Anionen (N3- und S2-) vor. [(N3-)(M3+)4]-Tetraeder, über zwei Ecken zu linearen Ketten ∞1[N(M1)1/1(M2)1/1(M3)2/2]6+ verknüpft, bilden das strukturelle Hauptmerkmal. Nach Art einer dichtesten “Stabpackung” gebündelt, werden diese durch drei kristallographisch unterschiedliche S2- zusammengehalten, die für Ladungsausgleich und dreidimensionale Vernetzung sorgen.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936191025
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    Darstellung und Struktur der Zweikernigen tert-Butyliminovanadium(IV)-Komplexe [(μ—NtC4H9)2V2(CH2CMe3)2X2] (X = OtC4H9, CH2CMe3) (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1827-1833 
    Details
    ISSN: 0044-2313
    Keywords: Neopentyl complexes of vanadium(V,IV) ; syntheses ; 1H, 51V-NMR ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Molecular Structure of the Binuclear tert-Butyliminovanadium(IV) Complexes [(μ-NtC4H9)2V2(CH2CMe3)2X2] (X = OtC4H9, CH2CMe3)Syntheses of the neopentylvanadium(V) compounds tC4H9N=V(CH2CMe3)3-n(OtC4H9)n (n = 0 (7), 1 (6), 2) are described. 6 and 7 decompose by irradiation splitting off neopentane and yielding the binuclear diamagnetic neopentylvanadium(IV) complexes [(μ-NtC4H9)2V2(CH2CMe3)2X2] [X = OtC4H9 (8), CH2CMe3 (11)]. All compounds obtained are characterized by 1H and 51V NMR spectroscopy. 8 has been found by X-ray diffraction analysis to be a binuclear complex with bridging tert-butylimino ligands and a vanadium - vanadium single bond. The complexes tC4H9N=V(CH2C6H5)(OtC4H9)2 and [(μ-NtC4H9)2V2(CH2SiMe3)2(OtC4H9)2] (10) have been also prepared; the crystal structure of 8 and 10 are nearly identical.
    Notes: Die Darstellung der Neopentylvanadium(V)-Verbindungen tC4H9N=V(CH2CMe3)3-n(OtC4H9)n [n = 0 (7), 1 (6), 2] wird beschrieben. 6 und 7 zersetzen sich photochemisch unter Abspaltung von Neopentan und Bildung der zweikernigen, diamagnetischen Neopentylvanadium(IV)-Komplexe [(μ—NtC4H9)2V2(CH2CMe3)2X2] [X = OtC4H9 (8), CH2CMe3 (11)]. Alle dargestellten Verbindungen werden 1H— und 51V-NMR-spektroskopisch charakterisiert. Die Röntgenstrukturanalyse von 8 zeigt einen zweikernigen Komplex mit verbrückenden tert-Butylimino-Liganden und einer Vanadium - Vanadium-Einfachbindung. Darüber hinaus wurden die Verbindungen tC4H9N = V(CH2C6H5)(OtC4H9)2 und [(μ-NtC4H9)2V2(CH2SiMe3)2(OtC4H9)2] (10) synthetisiert; die Kristallstrukturen von 8 und 10 sind nahezu identisch.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936191104
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    Weitere Oxochlorotitanate LnTiO3Cl der Seltenen Erden (Ln=Sm—Lu) - Präparation, Kristallstruktur, elektronenmikroskopische UntersuchungProfessor Dietrich Mootz zum 60. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1214-1220 
    Details
    ISSN: 0044-2313
    Keywords: Rare earth oxychlorides and oxochlorotitanates ; preparation ; crystal structure ; chemical vapour transport ; electron microscopic investigation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Rare Earth Oxochlorotitanates LnTiO3Cl (Ln=Sm—Lu) - Preparation, Structure and Electron Microscopic InvestigationsAfter the preparation of SmTiO3Cl we made the attempt to prepare analogous compounds with the heavier rare earth elements.We present 2 methods to prepare powders of LnTiO3Cl (Ln = Sm—Lu) together with a new method to prepare the rare earth oxychlorides LnOCl (Ln = Tm—Lu). There will be also presented 2 methods to get single crystals of these compounds via chemical vapour transport.The new rare earth oxochlorotitanates LnTiO3Cl (Ln = Eu—Lu) are isotypic to SmTiO3Cl. They crystallize in the monoclinic space group: C2/m (No. 12). The lattice parameters (Å) are between a = 9.716(3), b = 3.942(2), c = 10.100(4) (SmTiO3Cl) and a = 9.748(1), b = 3.8454(5), c = 9.625(2) (LuTiO3Cl), Z = 4. We observed a permanent decay of the cell volume with the decay of the radii of the cations.The structure of EuTiO3Cl and DyTiO3Cl was refined to R = 3.4% and R = 5.8% respectively.The crystal structure which has a certain similarity to brannerite can be described in a simplified way by saying that the rare earth and chlorine particles are located between walls of Ti—O-double-octahedra.
    Notes: Anknüpfend an die Darstellung von SmTiO3Cl wurden weitere Verbindungen dieses Formeltyps mit den schwereren Seltenen Erden zugänglich. Eine neue Methode zur Darstellung von Seltenerd-Oxidchloriden LnOCl (Ln=Tm—Lu) sowie je 2 Wege zur Darstellung pulverförmiger Präparate LnTiO3Cl und zur Synthese von Einkristallen über den chemischen Transport werden vorgestellt.Die neuen, zu SmTiO3Cl isotypen, Oxochlorotitanate LnTiO3Cl (Ln = Eu—Lu) der Seltenen Erden kristallisieren monoklin: RG C2/m (No. 12). Die Gitterkonstanten (in Å) umfassen den Bereich von a = 9,716(3), b = 3,942(2), c = 10,100(4) (SmTiO3Cl) bis a = 9,748(1), b = 3,8454(5), c = 9,625(2) (LuTiO3Cl), Z = 4. Die Zellvolumina nehmen mit dem Kationenradius stetig ab. Die Struktur von EuTiO3Cl und DyTiO3Cl wurde bis zu R = 3,4% bzw. R = 5,8% verfeinert. In der mit dem Brannerittyp nahe verwandten Kristallstruktur erkennt man zwischen Wänden aus Ti - O-Doppeloktaedern angeordnete Seltenerd- und Chlorteilchen.
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    URL: http://dx.doi.org/10.1002/zaac.19936190711
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    Kristallstruktur von Tl4Fe(CN)6Professor Dietrich Mootz zum 60. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1231-1236 
    Details
    ISSN: 0044-2313
    Keywords: Thallium(I) hexacyanoferrate(II) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of Tl4Fe(CN)6Single crystals of Tl4Fe(CN)6 have been prepared for the first time and its crystal structure was determined. The pale yellow compound crystallizes in the triclinic space group P1 (No. 2) with the lattice parameters a = 726.6(1) pm, b = 797.4(8) pm, c = 1 336.0(1) pm, α = 104.7(9)°, β = 90.0(8)°, γ = 97.6(7)°, Z = 2 in a new structure type.
    Notes: Erstmals wurden Einkristalle von Tl4Fe(CN)6 dargestellt und deren Kristallstruktur gelöst. Die fahlgelbe Verbindung kristallisiert triklin, Raumgruppe P1 (No. 2), a = 726,6(1) pm, b = 797,4(8) pm, c = 1 336,0(1) pm, α = 104,7(9)°, β = 90,0(8)°, γ = 97,6(7)°, Z = 2 in einem neuen Strukturtyp.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190714
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    Synthese und Struktur der ternären Ammoniumnitrate (NH4)2[M(NO3)5] (M = Tb—Lu, YProfessor Dietrich Mootz zum 60. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1237-1240 
    Details
    ISSN: 0044-2313
    Keywords: Synthesis ; crystal structure ; lanthanides ; ternary ammonium lanthanide nitrates ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of the Ternary Ammonium Nitrates (NH4)2[M(NO3)5] (M = Tb—Lu, Y)Single crystals of the ternary ammonium nitrates (NH4)2[M(NO3)5] (M = Tb—Lu, Y) are obtained from the solution of the sesquioxides in a melt of NH4NO3 and sublimation of the excess NH4NO3. In the crystal structure of (NH4)2[Tm(NO3)5] (trigonal, P31, Z = 3; a = 1 123.76(8), c = 930.1(1) pm; R = 0.062; Rw = 0.034) Tm3+ is surrounded by five bidentate nitrate ligands. The isolated [Tm(NO3)5]2- groups are held together by ammonium ions.
    Notes: Einkristalle der ternären Ammoniumnitrate (NH4)2[M(NO3)5] (M = Tb—Lu, Y) erhält man durch Auflösen der Sesquioxide in einer Ammoniumnitrat-Schmelze und Entfernen des überschüssigen NH4NO3 durch Sublimation. Die Röntgenstrukturanalyse am Beispiel von (NH4)2[Tm(NO3)5] (trigonal, P31, Z = 3; a = 1 123,76(8), c = 930,1(1) pm; R = 0,062; Rw = 0,034) zeigt, daß Tm3+ von fünf zweizähnigen Nitratliganden umgeben ist. Die anionischen Baueinheiten [Tm(NO3)5]2- sind daher isoliert und werden nur durch die NH4+-Ionen zusammengehalten.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190715
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    Züchtung und röntgenographische Untersuchung von Einkristallen des Alumothiosilicats Mn1,84Al0,16Si0,84Al0,16S4Professor Dietrich Mootz zum 60. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1283-1286 
    Details
    ISSN: 0044-2313
    Keywords: Alumothiosilicate ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Growth and Structure of the Alumothiosilicate Mn1.84Al0.16Si0.84Al0.16S4Single Crystals of the alumothiosilicate Mn1.84Al0.16Si0.84Al0.16S4 were grown by chemical transport reaction. The compound represents the first example of this type of silicate. The crystals were characterized by electron microprobe analyses and X-ray methods. The compound crystallizes in the olivine type structure, space group Pnma, a = 1 266.9(2), b = 739.6(3), c = 592.8(1) pm. The mean bond lengths are very similar to those in Mn2SiS4. That part of aluminum which is situated at the octahedral sites is not equally distributed amongst both types of octahedral positions but is enriched on the smaller and more symmetric M(1) position.
    Notes: Durch Chemische Transportreaktion gelang die Züchtung von Einkristallen der Verbindung Mn1,84Al0,16Si0,84Al0,16S4, einem Alumothiosilicat; sie stellt das erste Beispiel für ein derartiges Silicat dar. Die Charakterisierung erfolgte mit der Elektronenstrahlmikrosonde sowie mit Röntgenmethoden. Die Verbindung besitzt Olivinstruktur, Raumgruppe Pnma, a = 1 266,9(2), b = 739,6(3), c = 592,8(1) pm. Die mittleren Bindungslängen sind mit denen in Mn2SiS4 vergleichbar. Der Anteil des Aluminiums auf den Oktaederplätzen ist nicht statistisch auf die beiden kristallographisch unterschiedlichen Plätze verteilt, sondern es findet eine Anreicherung auf der kleineren und höhersymmetrischen M(1)-Position statt.
    Additional Material: 5 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19936190722
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  • 130
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    Gemischtligandenkomplexe mit N-Acyl-thioharnstoffen: Die Struktur des [N-(Morpholinothiocarbonyl)-benzamidato] (3-amino-2-cyano-n-butyl-dithiocrotonato)nickel(II)Professor Dietrich Mootz zum 60. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1295-1299 
    Details
    ISSN: 0044-2313
    Keywords: Mixed ligand complexes ; N-acylthiourea complexes ; nickel(II) chelates ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Mixed Ligand Complexes of N-Acyl-thioureas: The Structure of [N-(Morpholinothiocarbonyl)-benzamidato] (3-amino-2-cyano-n-butyl-dithiocrotonato)nickel(II)The reaction of a solution of N-(morpholinothiocarbonyl)benzamide and 3-amino-2-cyano-n-butyl-dithiocrotonate with nickel(II)-acetate tetrahydrate yields the first mixed ligand complex of N-acyl-thioureas. Its structure has been determined by an X-ray structure analysis. The coordination geometry is square planar. Bond lengths and angles are in good agreement with those of other bis and tris N-acyl-thiourea chelates.
    Notes: Aus einer Lösung von N-(Morpholinothiocarbonyl)-benzamid und 3-Amino-2-cyano-dithiocrotonsäure-n-butylester konnte durch Umsetzung mit Nickel(II)-acetat-tetrahydrat der erste Gemischtliganden-komplex mit N-Acylthioharnstoffen synthetisiert werden. Seine Struktur wurde mittels Röntgenkristallstrukturanalyse bestimmt. Die Koordinationsgeometrie ist quadratisch-planar. Bindungslängen und -winkel im N-Acylthioharnstoff-Teil des Komplexes stimmen gut mit denen anderer Bis- und Tris-N-acyl-thioharnstoff-Chelatkomplexe überein.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190724
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    Gitterschwingungsspektren. LXXVI. Zur Kenntnis basischer Kupfersalze  -  Kristallstruktur und schwingungsspektroskopische Untersuchungen an Cu2(OH)3NO2Professor Dietrich Mootz zum 60. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1287-1294 
    Details
    ISSN: 0044-2313
    Keywords: Dicopper trihydroxide nitrite ; crystal structure ; i.r., Raman spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Lattice Vibration Spectra. LXXVI. On Basic Copper Salts  -  Crystal Structure, IR and Raman Spectra of Cu2(OH)3NO2Single-crystal X-ray as well as IR and Raman data of Cu2(OH)3NO2 are presented and discussed with respect to an order-disorder (OD) phase transition and the strength of hydrogen bonds. Cu2(OH)3NO2 crystallizes pseudosymmetrically in the monoclinic space group P21/m (Z = 2, a = 562.22(4), b = 605.94(5), c = 663.55(4) pm and β = 95.415(5)°) forming a layered structure of edge-connected, elongated CuO6 octahedra (final R value 2.5% for 1047 symmetry averaged reflections with I ≥ 2.5 μ1). The NO2- ions are on a split position with dynamic disordering at ambient temperature. On temperature lowering the disorder is frozen out with a symmetry decrease to space group P21. The disorder of the NO2- ions causes four different arrangements of OH(2)- with different strengths of the H…O hydrogen bonds present OD stretching modes in the spectra of isotopically dilute samples 2628, 2535, 2435, and 2343 cm-1 at 90 K. The OH(1)- ions form weak H…N H-bonds to the lone-pair of the nitrogen atoms of the NO2- ions (vOD 2563 cm-1).
    Notes: Die Kristallstruktur sowie die IR- und Raman-Spektren von Cu2(OH)3NO2 werden mitgeteilt und im Hinblick auf eine Ordnungs-Unordnungs(OD)-Phasenumwandlung sowie die Stärke der vorhandenen Wasserstoffbrücken diskutiert. Das basische Nitrit kristallisiert pseudosymmetrisch in der monoklinen Raumgruppe P21/m (Z = 2, R = 2,5%, 1047 symmetriegemittelte Reflexe mit 1 〉 2,5 μ1). Cu2(OH)3NO2 bildet eine Schichtenstruktur kantenverknüpfter, gestreckter CuO6-Oktaeder. Die Nitritionen befinden sich auf einer Splitlage mit dynamischer Fehlordnung bei Raumtemperatur. Bei niedrigeren Temperaturen friert die Fehlordnung unter Bildung von NO2--Zick-Zack-Ketten und Symmetrieerniedrigung zu P21 aus. Aufgrund der Fehlordnung der NO2--Ionen ergeben sich für die OH(2)--Ionen vier verschiedene Anordnungen mit entsprechend unterschiedlich starken H-Brücken (H…O). Die OH(1)--Ionen bilden H…N-Wasserstoffbrücken zum freien Elektronenpaar des N-Atoms der NO2--Ionen.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190723
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    Wasserstoffbrückenbindungen in o- und m-Phenylendiammonium-aquapentafluorometallaten(III) (MIII = Al, Cr, Fe)Professor Dietrich Mootz zum 60. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1307-1314 
    Details
    ISSN: 0044-2313
    Keywords: Fluorometallates ; crystal structure ; hydrogen bonds ; phenylenediammonium salts ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Hydrogen Bonds in o- and m-Phenylenediammonium Aquapentafluoro Metallates(III) (MIII = Al, Cr, Fe)m- and o-Phenylenediammonium-[MIIIF5(H2O)] compounds of Al, Cr and Fe were synthesized and characterized by X-ray single crystal structure analysis. All structures are described in the space group P212121 (Z = 4). m-Ph(NH3)22+ (Ph(NH3)22+ = phenylenediammonium) compounds: Al: a = 6.489(2), b = 7.943(2), c = 18.204(2) Å, R/wR = 0.084/0.050 for 1 533 reflections; Cr: a = 6.571(2), b = 8.006(2), c = 18.456(3) Å, R/wR = 0.050/0.040 for 1 571 reflections; Fe: a = 6.608(2), b = 8.052(2), c = 18.424(4) Å, R/wR = 0.042/0.034 for 1 947 reflections. o-Ph(NH3)22+ compounds: Al: a = 6.580(2), b = 7.891(2), c = 18.319(5) Å, R/wR = 0.050/0.045 for 2 370 reflections; Cr: a = 6.642(2), b = 7.954(2), c = 18.484(4) Å, R/wR = 0.065/0.043 for 2 041 reflections; Fe: a = 6.693(2), b = 7.995(4), c = 18.529(7) Å, R/wR = 0.035/0.033 for 2 651 reflections. Isolated distorted octahedral [MIIIF5(H2O)]2- anions are connected by double O—H⃛F hydrogen bonds of alternating strength to form chains in the b direction. Those chains, packed in a pseudohexagonal way, are further linked by the ammonium functions of the phenylenediammonium cations to a 3 D hydrogen bond network.
    Notes: m- und o-Phenylendiammonium-[MIIIF5(H2O)]-Verbindungen von Al, Cr und Fe wurden synthetisiert und durch Röntgenstrukturbestimmungen an Einkristallen charakterisiert. Die Strukturen werden alle in der Raumgruppe P212121 (Z = 4) beschrieben. m-Ph(NH3)22+-Verbindungen (Ph(NH3)22+ = Phenylendiammonium): Al: a = 6,489(2), b = 7,943(2), c = 18,204(2) Å, R/wR = 0,084/0,050 für 1 533 Reflexe; Cr: a = 6,571(2), b = 8,006(2), c = 18,456(3) Å, R/wR = 0,050/0,040 für 1 571 Reflexe; Fe: a = 6,608(2), b = 8,052(2), c = 18,424(4) Å, R/wR = 0,042/0,034 für 1 947 Reflexe. o-Ph(NH3)22+-Verbindungen: Al: a = 6,580(2), b = 7,891(2), c = 18,319(5) Å, R/wR = 0,050/0,045 für 2 370 Reflexe; Cr: a = 6,642(2), b = 7,954(2), c = 18,484(4) Å, R/wR = 0,065/0,043 für 2 041 Reflexe; Fe: a = 6,693(2), b = 7,995(4), c = 18,529(7) Å, R/wR = 0,035/0,033 für 2 651 Reflexe. Isolierte verzerrt oktaedrische [MIIIF5(H2O)]2- Anionen werden durch doppelte O—H…F H-Brückenbindungen alternierender Stärke zu Ketten in b-Richtung verknüpft.Diese pseudohexagonal gepackten Ketten werden durch die Ammoniumfunktionen der Phenylendiammonium-Kationen über weitere H-Brücken dreidimensional vernetzt.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190726
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    Sodium aluminogermanate hydroxosodalite hydrate Na6+x[Al6Ge6O24](OH)x · nH2O (x ≈ 1.6, n ≈ 3.0): Synthesis, phase transitions and dynamical disorder of the hydrogen dihydroxide anion, H3O2-, in the Cubic high-temperature formDedicated to Professor Dietrich Mootz on his 60th Birthday. (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1321-1329 
    Details
    ISSN: 0044-2313
    Keywords: Sodium aluminogermanate ; sodalite ; hydrogen dihydroxide anion ; crystal structure ; phase transition ; dynamical proton exchange ; MAS NMR ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Natriumalumogermanat-Hydroxosodalithhydrat Na6+x[Al6Ge6O24](OH)x · nH2O (x ≈ 1,6, n ≈ 3,0): Synthese, Phasenumwandlungen und dynamische Fehlordnung des Hydrogendihydroxid-Anions,H3O2-,in der kubischen HochtemperaturformKristallines Natriumalumogermanat-Hydroxosodalithhydrat Na6+x[Al6Ge6O24](OH)x · nH2O mit x ≈ 1,6 und n ≈ 3,0 wurde durch Reaktion von Al2O3, GeO2 und NaOH-Lösung unter hydrothermalen Bedingungen hergestellt und mit Hilfe der Simultanthermoanalyse, Dynamischen Differenz-Kalorimetrie (DSC), Röntgen- und Neutronenbeugung sowie 1H- und 23Na-MAS-NMR- und IR-Spektroskopie charakterisiert. Die Verbindung durchläuft eine reversible strukturelle Phasenumwandlung bei Tc = 166 K (Heizmodus), die tatsächlich, wie in DSC-Messungen festgestellt wurde, als komplexe Zweistufentransformation abläuft. Struktur-
    Notes: Crystalline sodium aluminogermanate hydroxosodalite hydrate Na6+x[Al6Ge6O24](OH)x · nH2O with x ≈ 1.6 and n ≈ 3.0 has been synthesized by reacting Al2O3, GeO2 and NaOH solution under hydrothermal conditions, and characterized by means of simultaneous thermal analysis, differential scanning calorimetry, X-ray and neutron diffraction as well as 1H and 23Na MAS NMR and IR spectroscopy. The material undergoes a reversible structural phase transition at Tc = 166 K (heating mode), which is actually a complex two-step transformation as detected in DSC measurements. Structure refinements of the cubic high-temperature form (cell constant a = 9.034(2) Å, room temperature) with single-crystal X-ray and powder neutron diffraction data have not yielded overall satisfactory results, probably due to the solid-solution character of the hydrosodalite. The refinements nevertheless demonstrate that (i) the sodalite host framework is a strictly alternating array of corner-linked AlO4 and GeO4 tetrahedra, and (ii) most polyhedral [4668] cavities are occupied by four sodium cations and one orientationally disordered hydrogen dihydroxide anion, H3O2-, which possesses a strong central hydrogen bond. Variable-temperature 1H MAS NMR spectra unambiguously confirm the presence of H3O2- ions and, in addition, reveal a dynamical intraionic exchange between the central and terminal protons and a rotational diffusion of those anions to occur in the high-temperature form. The nature of the guest complexes filling the remaining cages could not be unambiguously determined. Results are compared with those obtained in recent studies on the related sodium aluminosilicate hydrosodalite system of the general formula Na6+x[Al6Si6O24] (OH)x · nH2O.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190728
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    Die Kristallstruktur von (N,N-Diethyl-N′-benzoylselenoureato)thallium(I) (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1689-1692 
    Details
    ISSN: 0044-2313
    Keywords: Thallium(I) complex ; (N,N-Diethyl-N′-benzoylselenoureato) thallium(I) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of (N,N-Diethyl-N′-benzoylselenoureato)thallium(I).Tl(C12H15N2OSe) exists in a dimeric form and crystallizes in the triclinic space group P-1. The cell parameters are a = 6.501(6), b = 9.901(7), c = 12.233(9) Å, α = 91.59(2), β = 80.11(6), γ = 85.28(5)° and Z = 2. The structure was solved with Patterson and direct methods and was refined to a final R-value of 5.30%. Two complex molecules are connected by Tl—Se bonds to form a planar four membered ring with diagonally arranged Tl and Se atoms. The considerably bended chelate rings are nearly at right angle to the central four membered ring. The Tl—Se bond lengths are 3.105(3) and 3.118(3) Å, the Tl—O bond length is 2.532(9) Å.
    Notes: Tl(C12H15N2OSe) liegt als Dimer vor und kristallisiert in der triklinen Raumgruppe P-1 mit den Gitterkonstanten a = 6,501(6), b = 9,901(7), c = 12,233(9) Å, α = 91,59(2), β = 80,11(6), γ = 85,28(5)°, Z = 2. Die Struktur wurde mit Patterson und Direkten Methoden gelöst und bis zu einem R-Wert von 5,30% verfeinert. Zwei Komplexmoleküle sind über Tl—Se-Bindungen zu einem planaren Vierring aus diagonal angeordneten Thallium- und Selenatomen verknüpft. Die stark abgewinkelten Chelatringe sind nahezu rechtwinklig zum zentralen Vierring angeordnet. Die Tl—Se-Abstände betragen 3,105(3) und 3,118(3) Å, der Tl—O-Abstand beträgt 2,532(9) Å.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936191010
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    Wie steuert man die Koordination in Zinkkomplexen?? Untersuchungen mit Hydridotris(3-phenylpyrazolyl)borat als Ligand (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 2071-2076 
    Details
    ISSN: 0044-2313
    Keywords: Polypyrazolylborate ligand ; zinc complexes ; crystal structure ; zinc enzyme model ; insuline ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: How to Steer the Coordination of Zinc Complexes? Investigations with Hydridotris(3-phenylpyrazolyl)borate as a LigandThe crystal structure analyses of the zinc complexes LPhZnCl (A) and Zn(LPh)2 (B) of the potentially tridentate nitrogen ligand LPh- = HB(3-Phpz)3- Phpz = 3-Phenylpyrazolyl) unexpectedly show tetrahedral coordination of the metal ion in both cases. The bisligand zinc complex B is formed by decomposition of unstable hydroxy and alkoxy complexes of the formula LPhZnOR. As a further product of that reaction a complex of the formula [η3B(3-Phpz)3Zn(3-PhpzH)]+ClO4- could be identified which is a first example for the cationic species LPhZn(neutral ligand)+. A crystallizes in the trigonal system with lattice constants of a = 11.449(2) and c=11.365(2) Å, space group P3, Z = 2, dcalc. = 1.365mg/mm3. B crystallizes in the orthorhombic system with a = 22.675(3), b = 10.797(2), and c = 19.699(3) Å, space group Pbcn; Z = 4, dcalc. = 1.306 mg/mm3. The crystal structures were determined from 1 687 (A) and 2 341 (B) observed X-ray data and refined to R = 0.03 and 0.04, respectively. A was characterized as a chlorotripod complex with symmetry 3-C3 and a distorted tetrahedral coordination of the Zn atom (angle Cl—Zn—N 122.9(1)° and N—Zn—N′ 93.3(1)°), while B was identified as a bisligand complex with symmetry 2-C2 and again a distorted tetrahedral coordination of the Zn atom (angles N—Zn—N 101.5(1) up to 118.9(1)°).
    Notes: Kristallstrukturanalysen der Zinkkomplex LPhZnCl (A) und Zn(LPh)2 (B) des potentiell drei-Zänigen Stickstoffliganden LPh- = HB(3-Phpz)3- 3-Phpz = 3-Phenylpyrazolyl zeigen unerwartet in bei-den Fällen eine tetraedrische Metallkoordination. Der Bisligandzinkkomplex B bildet sich beim Zerfall in-stabler Hydroxy- und Alkoxykomplexe der Formel ZnOR. Als weiteres Produkt dieser Zerfallsreaktion konnte ein Komplex der Formel [η3HB(3-Phpz)3Zn(3-PhpzH)]+ClO4- identifiziert werden welcher ein erstes Beispiel für die kationische Spezies [LPhZn(Neutralligand)]+ ist. A kristallisiert trigonal a = 11,449(2) und c = 11,365(2) Å in der Raumgruppe P3, Z = 2, dber. = 1,396 mg/mm3. B kristallisiert orthorhombisch mit a = 22,675(3), b = 10,797(2) und c = 19,699(3) Å in der Raumgruppe Pbcn; Z = 4, dber. = 1,306 mg/mm3. Die Kristallstrukturen wurden mit 1 687 (A) und 2 341 (B) beobachteten Reflexen bestimmt und bis R = 0,03 bzw. 0,04 verfeinert. A stellt einen Chloro-Tripod-Komplex mit der Eigensymmetrie 3-C3 dar, die Koordination des Zn-Atoms ist verzerrt tetraedrisch (Winkel Cl—Zn—N 122,9(1) und N—Zn—N′ 93,3(1)°, B ist ein Bisligandkomplex mit der Eigensymmetrie 2-C2 mit ebenfalls verzerrt tetraedrischer Koordination des Zn-Atoms (Winkel N—Zn—N 101,5(1) bis 118,9(1)°.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936191217
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    Reversible formation of an intramolecular agostic CH interaction in a dimanganese complex (1992)
    Springer
    Journal of cluster science 3 (1992), S. 103-108 
    Details
    ISSN: 1572-8862
    Keywords: Manganese ; agostic ; crystal structure ; CH activation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract Agostic interactions of CH bonds with metal atoms are currently of great interest. UV irradiation of Mn2(CO)8 (PMe2Ph)2 in the presence of the HC≡COEt yielded the new compound Mn2(CO)6(PMe2Ph)2 [μ-C(OEt)=C(H)C=C(H)C=O(OEt)],1 that contains a strong agostic interaction of an olefinic CH bond to one of the managanese atoms, Mn...C=2.349(5), Mn...H=2.01(4). This interaction can be removed (reversibly) by CO addition (25°C/1000 psi) to1 to yield the new complex Mn2(CO)7(PMe2Ph)2[μ-C(OEt)=C(H)C=C(H)C=O(OEt)],2.
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    Further studies of M3(μ3-O)(μ-X)3(μ-O2CCH3)3L3 (M=Mo, W) type clusters with nine core electrons (1992)
    Springer
    Journal of cluster science 3 (1992), S. 123-144 
    Details
    ISSN: 1572-8862
    Keywords: Molybdenum ; tungsten ; crystal structure ; reduction ; acetate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract Four new compounds having nine cluster electrons and cores of the types Mo3OCl3, Mo3OBr3, and W3OCl3 are reported. Compound (1) prepared by reduction of [Bu4N][Mo3OCl6(OAc)3] in THF with metallic zinc, was shown by X-ray crystallography to be Mo3OCl4(OAc)3 (THF)2 (1). It forms crystals in space groupP21 with unit cell dimensionsa=9.472(2) Å,b=13.546(4) Å,c=9.652(2) Å, β=101.70(2)°,V=1201(1) Å3,Z=2. The [Mo3(μ3-O)(μ-Cl)3]4+ core is surrounded by three μ-O2CCH3 anions, one Cl−, and two THF and has Mo-Mo distances of 2.620(1) Å, 2.613(1) Å, and 2.530(1) Å, with the shortest bond between the two Mo atoms to which the THF molecules are coordinated. Compounds [Bu4N]2 [Mo3OBr6(O2CCH3)3] · Me2CO, (2) and [Mo3OBr3(O2CCH3)3(PMe3)3]3 · BF4, (3) are the first two nine-electron Mo3 species with a [Mo3(μ3-O) Br3]4+ core. Both were obtained by zinc reduction of [Mo3OBr6(O2CCH3)3]− in the presence of (NBu4) Br (2) or PMe3 and NaBF4 (3), and each was characterized crystallographically. Compound (2) crystallized in space group Cc with unit cell dimensionsa=25.037(5) Å,b=12.827(2) Å,c=21.484(4) Å, β=122.96(1)0,V=5790(3) Å3,Z=4. While the anion has no crystallographically required symmetry, its virtual symmetry is C3v . The Mo-Mo distances are 2.619(2) Å, 2.610(3) Å, 2.644(2) Å, with a mean value of 2.624[14] Å. Compound (3) crystallized in space groupP21/c with unit cell dimensionsa=10.846(2) Å,b=25.033(5) Å,c=12.641(5) Å, β=94.74(2)0,V=3420(2) Å3,Z=4. The cation occupies a general position but has virtual C3v symmetry, with Mo-Mo distances of 2.601(2) Å, 2.610(2) Å, 2.627(2) Å, with a mean value of 2.613[14] Å. Thus the anionic and cationic Mo3 clusters in (2) and (3), respectively, have average Mo-Mo distances that are equal within experimental error. Compound (4), [NEt4]2 [W3OCl6(O2CCH3)3] is the first 9-electron compound of this type containing tungsten. It was prepared by reduction of [Et4N][W3OCl6(OAc)3] in benzene with Na/Hg. It crystallized in space groupP212121 with unit cell dimensionsa=11.076(2) Å,b=14.345(2) Å,c=21.026(3) Å,V=3574(1) Å3,Z=4. The anion resides on a general position but has virtual C3v symmetry, with W-W distances of 2.577(1) Å, 2.612(1) Å, 2.584(1) Å and a mean value of 2.591[15] Å.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00702878
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  • 138
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    Synthesis, structural characterization and bonding properties of heterometallic-heterobridging cubane-type tetranuclear cluster compounds [CuMo3OS3]·I·(μ-OAc)[S2P(OC2H5)2]3·L (L=py, DMF) (1992)
    Springer
    Journal of cluster science 3 (1992), S. 179-199 
    Details
    ISSN: 1572-8862
    Keywords: Heterometallic-heterobridging cubane-type tetranuclear cluster ; preparation ; crystal structure ; molecular orbital calculation ; quasi-aromaticity ; copper ; molybdenum
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract By the reaction of cluster [Mo3OS3](dtp)4(H2O) used as starting material with CuI using [3+1] mode, two novel heterometallic-heterobridging cubane-type tetranuclear cluster compounds [CuMo3OS3]·I·(μ-OAc)[S2P(OC2H5)2]3·L [(I)L=py, (II)L=DMF] [dtp=S2P(OC2H5)2; OAc=OOCCH3] containing [CuMo3OS3] core have been obtained. Compounds (I) and (II) have been characterized by IR, EPR, UV-VIS, electrochemistry and X-ray crystallography. By comparison of these two compounds with the analogous [CuMo3S4] series in the structure and molecular orbital calculation, the influence of mixed S/O bridging on the structure is discussed. It is demonstrated that the {Mo3S3} cluster ring in [Mo3OS3]4+ possesses a similar quasi-aromaticity to [Mo3S4]4+. Crystal data: for (I), space group= $$P\overline 1 $$ ,a=13.781(8)Å,b=14.523(6)Å,c=12.098(6)Å, α=98.37(4)°, β=109.41(5)°, γ=105.00(5)°,V=2133(2)Å3,Z=2,R=0.058; for (II), space group= $$P\overline 1 $$ ,a=13.215(4)Å,b=17.818(8)Å,c=9.873(4)Å, α=106.06(4)°, β=109.78(3)°, γ=82.00(3)°,V=2100(2)Å3,Z=2,R=0.045.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00702882
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  • 139
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    Electronic Resource
    Packing analysis and the crystal chemistry of 2,5-dibenzylidenecyclopent-3-ene-1-one. Rationale for a non-topochemical solid-state reaction (1992)
    Springer
    Molecular engineering 2 (1992), S. 103-116 
    Details
    ISSN: 1572-8951
    Keywords: Non-topochemical reaction ; crystal structure ; lattice energy calculations ; thermal motion analysis ; disorder
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The molecular and crystal structure of 2,5-dibenzylidenecyclopent-3-ene-1-one has been studied in detail to explain the formation of a non-topochemical pseudo-mirror-symmetric dimer upon photoirradiation. Packing energy calculations, analysis of the thermal motion, and lattice energy calculations are employed to analyse and understand the observed dimerization reaction, crystal structure, and crystal properties.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00999702
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  • 140
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    The crystal and molecular structures of 1,1′-divinyl-2,2′-biimidazolyl (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 1076-1079 
    Details
    ISSN: 1573-9171
    Keywords: X-ray crystallographic analysis ; 1,1′-divinyl-2,2′-biimidazolyl ; crystal structure ; molecular structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal and molecular structures of 1,1′-divinyl-2,2′-biimidazolyl (L) were determined by x-ray crystallographic analysis. It was established that the molecule of L has crystallographic symmetry 2 and a cisoid conformation with an angle of rotation of 128° between the imidazole rings. The length of the C2-C2′ bond is increased to 1.485(11) Å compared with the length of the analogous bond in unsubstituted 2,2′-biimidazolyl (1.423 Å). Localization of the N=C multiple bond is observed [1.297(9) Å]. The other N-C bonds of the ring are almost equalized (1.374 Å) and are close to the standard values for bonds of the C sp 2-N type in imidazoles. The angle between the plane of the heterocycle and the plane passing through the atoms of the vinyl group amounts to 7°.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00866589
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  • 141
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    Photo- and thermochromic mannich bases. 1. Mannich bases from 3,5-di-tert-butyl-4-hydroxybenzaldehyde and 2-naphthols (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 1875-1883 
    Details
    ISSN: 1573-9171
    Keywords: synthesis ; crystal structure ; UV spectra ; 2,6-di-tert-butyl-4-[α-(2-hydroxy-1-naphthyl)methyl]phenol ; 2,6-di-tert-butyl-4-[α-morpholino-α-(2-hydroxy-6-bromo-1-naphthyl)methyl]phenol ; 2,6-di-tert-butyl-4-α-(2-hydroxy-1-naphthyl)-1,4-methylenequinone ; 2,6-di-tert-butyl-4-α-(2-acetyloxy-1-naphthyl)-1,4-methylenequinone
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Mannich bases exhibiting photo- and thermochromic properties in solutions were synthesized from 3,5-di-tert-butyl-4-hydroxybenzaldehyde and 2-naphthols. An investigation of an acetyl derivative of methylenequinone, modeling a product of photo- and thermochromic transformations, proved that the color change of solutions of the Mannich bases is due to reversible dissociation into colored methylenequinones and morpholine. On the basis of data of x-ray diffraction analysis of one of the Mannich bases, characteristics of their molecular structure were determined, and reasons were stated for their effect on the dissociation mechanism.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00863826
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  • 142
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    Electronic Resource
    Synthesis and physicochemical investigation of LiMTif6 (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 1950-1956 
    Details
    ISSN: 1573-9171
    Keywords: hexafluorotitanates ; synthesis ; crystal structure ; 19F NMR ; IR spectroscopy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Mixed alkali hexafluorotitanates of the composition LiMTiF6 are synthesized, which crystallize with the orthorhombic symmetry. The lattice parameters of these materials are determined. It is shown that substitution of the Li+ cation in Li2TiF6 by Na+, K+, Rb+, and Cs+ leads to various degrees of distortion of the hexafluoroion. It is determined (19F NMR data) that the change in the dynamic state of the octahedral [TiF6]2− ions is related to their transition from the hindered-rotational to the isotropic state.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00863353
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  • 143
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    Macrocyclic amidophosphoryl polyethers: Biological activity, molecular structure, and structure of the complex with calcium thiocyanate (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 2211-2216 
    Details
    ISSN: 1573-9171
    Keywords: macrocyclic polyethers ; crystal structure ; biological activity ; IR spectra ; complex with calcium thiocyanate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The antihypoxic and anticonvulsant activity of eight new amidophosphoryl derivatives of crown ethers was investigated. It was found that some of them exhibit pronounced antihypoxic activity. The results of an x-ray structural and IR spectroscopic study of dibenzo-N-phenylphosphonyl-14-crown-5 (a=9.818,b=16.062,c=15.925 Å; γ=124.90°;V=2072 Å3;M=417.2;d=1.33 g/cm3 forZ=4, 1955 independent reflections [I〉3σ(I)] in a DAR-UM inCuK α radiation,P2 1/b space group,R=5.2%) and dibenzo-N-adamantylphosphonyl-14-crown-5 compounds (a=11.077,b=15.936,c=16.771 Å; γ=56.05°;V=2456 Å3;M=486.3;d=1.31 g/cm3 forZ=4, 2164 independent reflections [I〉3σ(I)] in a DAR-UM inCuK α radiation,P21/b space group,R=5.1%) are reported. Some details of the structure of the dibenzo-N-phenylphosphonyl-14-crown-5-complex with calcium thiocyanate and water are discussed; a polyhedron with a coordination number of six was found for the first time for calcium complexes with macrocyclic ligands. The combined examination of the results of the biological, x-ray structural, and IR spectroscopic study of macrocyclic, 14-member ligands suggested that the nature of the substituents at phosphorus affect the conformational state of the macrocycle, which remains unchanged in complexation in the investigated conditions.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01150749
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  • 144
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    Crystal and molecular structure of 1:1 molecular complexes of triphenyl-N-(4-methylpyridyl-2)phosphinimine and triphenyl-N-(3-methylpyridyl-2)phosphinimine with perchloric acid (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 495-499 
    Details
    ISSN: 1573-9171
    Keywords: crystal structure ; molecular complexes ; phosphinimines ; protonation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract X-ray diffraction analysis has been used to determine the crystal structures of the 1:1-composition products of protonation by perchloric acid of isomeric triphenyl-N-(4-methylpyridyl-2)phosphinimine (1) and triphenyl-N-(3-methylpyridyl-2)phosphinimine (2). The structures were refined toR=0.048 andR=0.052, respectively, using 2274 (1) and 2647 (2) reflections. The protonation centers are located at the sites of N atoms of the pyridine ring (1) and the phosphinimino group (2). The distribution of the bond lengths in the cations suggests that a significant contribution is made by a phosphonic structure with positive charges localized on the P atoms. N-H...O hydrogen bonds, with lengths of 2.890(4) and 3.020(3) Å, connect cations and anions in both structures.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00863071
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  • 145
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    1,1,4,4-Tetranitrobutane-2,3-diol and its derivatives. 4. Study of the reaction of 1,1,4,4-tetranitrobutane-2,3-diol with N-(methoxymethyl)-2-fluoro-2,2-dinitroethylamine; synthesis and crystalline structure of 1,12-difluoro-1,1,3,5,5,8,8,10,12,12-decanitro-3,10-diazadodecane-6,7-diol dinitrate (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 528-530 
    Details
    ISSN: 1573-9171
    Keywords: synthesis ; crystal structure ; 1,12-difluoro-1,1,3,5,5,8,8,10,12,12-decanitro-3,10-diazadodecane-6,7-diol dinitrate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A two-step synthesis has been proposed to obtain 1,12-difluoro-1,1,3,5,5,8,8,10,12,12-decanitro-3,10-diazadodecane-6,7-diol dinitrate, starting from 1,1,4,4-tetranitrobutane-2,3-diol and N-(methoxymethyl)-2-fluoro-2,2-dinitroethyl-amine, followed by nitration of the Mannich base formed. An x-ray-diffraction investigation of the dinitrate obtained was carried out.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00863077
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  • 146
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    X-ray structure of the organic conductor (ET)8[Hg2Br6·PhBr]2 (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 697-703 
    Details
    ISSN: 1573-9171
    Keywords: organic metals ; radical-cation salts ; bis(ethylenedithio)tetrathiafulvalene = ET ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The electrochemical oxidation of ET [bis(ethylenedithio)tetrathiafulvalene] in bromobenzene (electrolyte Bu 4 N[HgBr 3 ]) gave the radical-cation salt (ET) 8 [Hg 2 Br 6 ·PhBr] 2 (1), a new organic metal with a temperature range of 300–125 K. At 125 K a metal—dielectric transition is observed. Crystallographic data for (1):a=19.171(6),b=12.668(4),c=17.777(6) Å, α=118.03(3), β=89.45(2), γ=101.21(3)°, P $$\overline 1 $$ ,Z=1,d calc=2.30 g/cm 3 . The crystal structure of (1) is laminar. In the conducting organic layer the ET radical cations are linked into bands by shortened intermolecular S···S contacts of the “side-to-side” type. The anionic layer consists of centrosymmetric complexes [Hg 2 Br 6 ·C 6 H 5 Br] 2 4− . The Hg 1 and Hg 2 atoms are characterized by a trigonal configuration of the Hg-Br bond which is built up, on account of secondary Hg···Br interactions, into trigonal-bipyramidal for Hg 1 and trigonal-pyramidal (tetrahedral) for Hg 2 . Interaction between the anionic and cationic layers is effected through Br 6 ...S 8 contacts [3.491(7) Å)].
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01150895
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  • 147
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    Crystal structure of the organic metal (ET)2[Hg(SCN)2Cl] withT M-D=50 K (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 704-709 
    Details
    ISSN: 1573-9171
    Keywords: organic metals ; bis(ethylenedithio)tetrathiafulvalene (ET) ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The composition and structure of the radical-ion salt (ET) 2 [Hg(SCN) 2 Cl], a new organic metal withT M-D=50 K, were established in an x-ray structure investigation. Principal crystallographic data:a=36.69(1),b=8.302(8),c=11.732(8) Å, β=90.02(6)°, space groupCc, Z=4,d calc=2.08 g/cm 3 ,R=0.067. The crystal structure of the salt consists of an alternation of organic (cationic) and inorganic (anionic) layers along the axisa. The anionic layer consists of the polymeric chains in which the [Hg(SCN) 2 Cl]− ions are linked together along the axisc through secondary Hg···N bonds with lengths of 2.75(3) and 2.98(8) Å. On account of these interactions the trigonal configuration of the bonds of the Hg atom is built up to trigonal-bipyramidal. In the organic layer with a structure of the κ type the ET cations form dimers with an interplanar distance of 3.53 Å. ET cations belonging to neighboring dimers are linked together through shortened intermolecular S...S contacts with lengths of 3.40–3.50(2) Å.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01150896
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  • 148
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    Calixarenes as second-sphere ligands for transition metal ions. Synthesis and crystal structure of [(H2O)5 Ni(NC5H5)]2(Na)[calix[4]arene sulfonate] · 3.5 H2O and [(H2O)4Cu(NC5H5)2]-(H3O)3 [calix[4]arene sulfonate] · 10 H2O (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 14 (1992), S. 37-46 
    Details
    ISSN: 1573-1111
    Keywords: Calix[4]arene ; crystal structure ; second-sphere coordination ; nickel(II) ; copper(II) ; pyridine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The title compounds crystallize such that bilayers of calixarenes are separated by hydrophilic layers. In each case the transition metal has, in addition to a primary sphere of ligands, a second-sphere coordination by a calixarene. [(H2O)5Ni(NC5H5)]2(Na)[calix[4]arene sulfonate]·3.5 H2O,1, crystallizes in the triclinic space groupP $$\bar 1$$ witha = 12.487(4),b = 14.281(2),c = 15.055(5) Å, α = 85.66(2), β = 80.07(2), γ = 80.48(2)°, andD c = 1.64 g cm−3 forZ = 2. Refinement based on 2441 observed reflections led to a finalR value of 0.066. There are two different environments for the nickel-containing cations: one is positioned within the hydrophilic layer with the pyridine ligand intercalated into the hydrophobic calixarene bilayer and the other is also positioned within the hydrophilic layer, but the pyridine ligand is inserted into the hydrophobic cavity of the calix[4]arene. [(H2O)4Cu(NC5HS)2](H3O)3[calix[4]arene sulfonate]·10 H2O,2, crystallizes in the triclinic space groupP $$\bar 1$$ witha = 15.438(4),b = 15.727(6),c = 12.121(9) Å, α = 112.74(4), β = 102.02(4), γ = 85.34(4)°, andD c = 1.57 g cm−3 forZ = 2. Refinement based on 3925 observed reflections led to a finalR value of 0.107. The structure is similar to that of 1 except that the one copper-containing cation spans the hydrophilic layer and is intercalated into the bilayer of calixarenes on one side and positioned into the calixarene cavity on the other.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01041364
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  • 149
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    Isomerization processes in inclusion compounds: Xylenes in deoxycholic acid (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 14 (1992), S. 55-64 
    Details
    ISSN: 1573-1111
    Keywords: Host-guest inclusion compound ; p-,m-,o-xylene ; deoxycholic acid ; symmetry factor ; energy transfer ; photophysical factor ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The isomerization processes induced by UV photons in inclusion compounds of the host-guest type are examined, with special attention to the photophysics of the energy transfer process between the host and the guest, as well as to the influence of the host molecular cavity symmetry and the guest molecular symmetry. In particular, the experimental study has been carried out on the isomerization processes ofp-,m-, ando-xylene inside the molecular cavities of deoxycholic acid. The results have been compared with those obtained by irradiating the xylenes in an inert solution of hexane. The main difference is the elimination of by-products when the photochemical process is carried out in the solid state inclusion compound; however, the high purity of the isomerization product corresponds to a decrease in its yield with respect to the reaction in solution, due to the energy transfer process from the host to the guest moiety.
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    URL: http://dx.doi.org/10.1007/BF01041366
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  • 150
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    Crystal structure analysis of Y2Cu2O5 (1992)
    Springer
    Journal of superconductivity 5 (1992), S. 33-38 
    Details
    ISSN: 1572-9605
    Keywords: Yttrium ; copper ; X-ray ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Physics
    Notes: Abstract Single crystals of Y2Cu2O5 were obtained in the flux growth process by controlled heating of a mixture of Y2O3, BaO, and CuO in a molar ratio of 1∶8∶20. These crystals were analyzed by a single-crystal X-ray diffraction analysis. The crystal contains polymeric chains of Cu2O5 interspersed by yttrium ions surrounded by octahedral arrangements of oxygen atoms. Crystal data: space group=Pna21,a=10.799(2) Å,b=3.4990(5) Å,c=12.459(2) Å,Z=4, 380 reflections,R=0.026,R w=0.030.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00617994
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  • 151
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    Three-dimensional structure of the quinoprotein methylamine dehydrogenase from Paracoccus denitrificans determined by molecular replacement at 2.8 Å resolution (1992)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 14 (1992), S. 288-299 
    Details
    ISSN: 0887-3585
    Keywords: amino acid-derived cofactor ; crystal structure ; methylamine dehydrogenase ; molecular replacement ; oxidoreductase ; Paracoccus denitrificans ; pyrroloquinoline quinone ; quinoprotein ; tryptophan tryptophylquinone ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The three-dimensional structure of the quinoprotein methylamine dehydrogenase from Paracoccus denitrificans (PD-MADH) has been determined at 2.8 Å resolution by the molecular replacement method combined with map averaging procedures, using data collected from an area detector. The structure of methylamine dehydrogenase from Thio-bacillus versutus, which contains an “X-ray” sequence, was used as the starting search model. MADH consists of 2 heavy (H) and 2 light (L) subunits related by a molecular 2-fold axis. The H subunit is folded into seven four-stranded β-segments, forming a disk-shaped structure, arranged with pseudo-7-fold symmetry. A 31-residue elongated tail exists at the N-terminus of the H subunit in MADH from T. versutus but is partially digested in this crystal form of MADH from P. denitrificans, leaving the H subunit about 18 residues shorter. Each L subunit contains 127 residues arranged into 10 β-strands connected by turns. The active site of the enzyme is located in the L subunit and is accessible via a hydrophobic channel between the H and L subunits. The redox cofactor of MADH, tryptophan tryptophylquinone is highly unusual. It is formed from two co-valently linked tryptophan side chains at positions 57 and 107 of the L subunit, one of which contains an orthoquinone. © 1992 Wiley-Liss, Inc.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prot.340140214
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  • 152
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    Physicochemical Properties of Salts of p-Aminosalicylic Acid. I. Correlation of Crystal Structure and Hydrate Stability (1992)
    Springer
    Pharmaceutical research 9 (1992), S. 1428-1435 
    Details
    ISSN: 1573-904X
    Keywords: pharmaceutical salt selection ; salts of p-aminosalicylic acid ; hydrates ; crystal structure ; thermal stability
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The potassium (K), sodium (NA), calcium (CA), and magnesium (MG) salts of p-aminosalicylic acid were obtained, and their thermal behavior was characterized by means of differential scanning calorimetry (DSC) and thermogravimetric analysis (TG). Their crystal and molecular structures were determined by single-crystal X-ray diffraction after powder patterns had shown them to be nonisomorphous. Different degrees of hydration were observed for the solid salts, and an assessment of hydrate stability to dehydration was made from thermogravimetric studies. The onset temperature of dehydration (T t) of each salt varied within the series and exhibited correlation with X-ray determined structure. The observed onset of dehydration of MG and CA was higher than that of NA and is consistent with stronger ion-dipole interactions for the divalent salts. Crystallographic determination of the bond lengths between the metal ion and the water oxygens were 2.4 and 2.9 Å for NA, between 2.0 and 2.1 Å for MG, and 2.4 Å for CA. The open nature and presence of a channel feature in the structure of the sodium salt may have facilitated escape of water molecules from the crystal. Particle presentation (e.g., size, crystallinity) was also shown to affect dehydration behavior.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1015806812349
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  • 153
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    The Structure of Celiprolol (1992)
    Springer
    Pharmaceutical research 9 (1992), S. 365-371 
    Details
    ISSN: 1573-904X
    Keywords: celiprolol ; crystal structure ; two-dimensional nuclear magnetic resonance (2D NMR)
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structure and nuclear magnetic resonance (NMR) spectra and assignments of celiprolol, N′-[3-acetyl-4[3-[N-t-butylamino-2-hydroxypropoxy]phenyl]-N, N-diethylurea, are reported. Celiprolol crystallizes in the monoclinic space group, P2l/a, with a = 9.081(2), b = 13.800(4), and c = 17.471(5) Å and β = 95.04(2)°. Structure was solved by direct methods; structure refinement to R of 0.058. Intermolecular hydrogen-bonding in the crystal is discussed. The 1H, 13C, and two-dimensional (2D) NMR spectra of the hydrochloride have been obtained and definitive signal assignments made.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1015895019791
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  • 154
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    Solid state structure of the hydrated potassium thiocyanate complex of benzodinaphthopyridino 21-crown-7, C37H31NO6·KSCN·H2O (1 : 1 : 1) (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 13 (1992), S. 29-36 
    Details
    ISSN: 1573-1111
    Keywords: Crown compound ; potassium thiocyanate ; crown cation complex ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Single crystal X-ray analysis of the hydrated KSCN complex of benzodinaphthopyridino-21-crown-7 (1) (1 : 1 : 1) is reported. Crystals of the complex are orthorhombic,Pnma, withα = 16.946(4),b = 22.298(4),c = 10.390(8) Å andD c = 1.184 g cm−1,Z = 4. The host macroring (1) has a mirror symmetry and exists in a so-called ‘dentists chair’ conformation. The cation (K−) is coordinated to all the six ether oxygen atoms and also weakly to the pyridine N atom. The SCN− anion group has a statistical type of disorder with opposite orientations of S and N such that nitrogen and sulphur are coordinated to K+. Packing of the host molecules is in columns to form quasi channels with K+, SCN−, and H2O being located inside the stacks.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01076668
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  • 155
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    Complexation with hydroxy host compounds, part 5. Structures and thermal analyses of 1,2,3,4,5-pentaphenylcyclopenta-2,4-dien-1-ol and its inclusion compounds with water and dimethylsulphoxide (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 13 (1992), S. 301-310 
    Details
    ISSN: 1573-1111
    Keywords: Inclusion compound ; hydroxy compound ; crystal structure ; thermal analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal and molecular structures of the title host compound (I), C35H26O, and its inclusion complexes with water (II), C35H26O·H2O and dimethylsulphoxide (III), C35H26O·C2H6OS are reported. (I) is monoclinicC2/c,a = 9.725(1),b = 20.031(3),c = 26.545(3) Å, β = 90.60(1)0,V = 5170 Å3,Z = 8; (II) is triclinic, $$P\bar 1$$ ,a = 10.206(1),b = 10.324(2),c = 14.425(2) Å, α = 101.68(1), β = 89.92(2), γ = 116.34(1)0,V = 1327 Å3,Z = 2; (III) is monoclinicP21/n,a = 17.832(5),b = 10.109(3),c = 17.901(5) Å, β = 111.93(2)0,V = 2993 Å3,Z =4. The structures were solved by direct methods and refined to final residuals of 0.045, 0.048, and 0.071, respectively. Thermal analysis of the complexes corroborates the crystallographic results.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01133229
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  • 156
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    X-ray structural study of a zinc(II) inclusion complex of a phenolate-pendant cyclam (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 12 (1992), S. 377-387 
    Details
    ISSN: 1573-1111
    Keywords: Charles Pedersen ; crown ethers ; phenol-pendant cyclam-zinc(II) complex ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The molecular structure of phenol-pendant cyclam-zinc(II) complex,4a, has been determined by X-ray structure analysis. Crystals of4a · ClO4 · CH3OH (C16H27N4OZn · ClO4 · CH3OH) are monoclinic, space groupP21/nn, with four molecules in the unit cell of dimensionsa=31.198(2) Å,b=8.426(1) Å,c=8.214(1) Å, andβ=93.96(1)°. The structure was solved by the heavy atom method and refined anisotropically toR=0.044,R w=0.062 for 1551 independent reflections. The complex assumes a five-coordinate, square pyramidal geometry, where zinc(II) is surrounded by the cyclam moiety in a planar fashion with the pendant phenolate anion occupying an axial position. An extremely short Zn-O(phenolate) bond distance of 1.983(5) Å, in conjunction with the 0.288 Å displacement of Zn(II) above the cyclam N4 plane toward the phenolate, accounts for the extremely low pK a value of 5.8 for the pendant phenol. These facts about4a, in comparison with the previous findings for the Ni(II) (4b) and Cu(II) complexes (4c) with the same ligand, illustrate well the characteristics of zinc(II) ion coordination properties.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01053875
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  • 157
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    Synthesis and crystal structure of a new paramagnetic complex salt of diprotonated dioxocyclam with PtCl 2− 4 and water (1:1:1) (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 13 (1992), S. 195-202 
    Details
    ISSN: 1573-1111
    Keywords: Dioxocyclam ; 5,7-dioxo-1,4,8,11-tetra-azacyclotetradecane ; platinum tetrachloride ; crystal structure ; paramagnetic properties of ionic stacked structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The paramagnetic complex salt of diprotonated dioxocyclam (1,11-dihydro-5,7-dioxo-1,4,8,11tetra-azacyclotetradecane), Pt(II) tetrachloride and water has been synthesized in strongly acidic medium and identified by X-ray structure analysis. The crystals of [(C10H22N4O2)2+(PtCl4)2−]·H2O are monoclinic, space groupP21 c,M r=585.23,a=9.516(1) Å,b=11.926(1) Å,c=16.622(2) Å,β=102.88(2)°,V=1839(1)Å3,Z=4,D x=2.114 g cm−3, λ(MoK α)=0.70930 Å,μ=83.1 cm−1,F(000)=1128,T=292 K,R=0.019 for 2808 observed reflections withI 〉 3δ(I). Alternating moieties of diprotonated dioxocyclam and a PtCl 2− 4 anion form columns running down the c axis. Water molecules are localized in the intercolumnar space and contribute to the extensive hydrogen bond network. The macrocycle conformation is characterized by two sequences of torsional angles, corresponding to two different subunits. The shorter sequence idealized as (-sc, ap, -ac, + ac, ap, +sc) [sc( ±60°), ac( ±120°), ap(180°)], describing the C pseudosymmetric part of the molecule, is centered on a -CH2 group between the two peptide O-C-N-H fragments. The opposite C pseudosymmetric subunit has a nearly (-sc, ac, -SC, ap)2 conformation. Pt is square planar coordinated by four Cl atoms, Pt-Clαve = 2.306(8) Å. The shortest Pt ... Pt distance is 7.200(1) Å.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01053643
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  • 158
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    A hydrogen bond between a calixarene (as host and its guest: Crystal and molecular structure of thep-t-butyldihomooxacalix[4]arene : Triethylamine (1 : 2) complex/clathrate (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 14 (1992), S. 247-256 
    Details
    ISSN: 1573-1111
    Keywords: Inclusion compounds ; calixarene ; crystal structure ; hydrogen bonding ; amines
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The structure of thep-t-butyldihomooxacalix[4]arene triethylamine (1 : 2 complex has been determined by X-ray crystallography. Crystals are monoclinic, space groupCc,a = 22.821(3),b = 15.257(3),c = 16.365(2) Å,β = 97.44(1)°,V = 5650(1) Å3,Z = 4,D calc = 1.03 g cm−3. One triethylamine (Et3N) molecule has one of its ethyl groups pointing inside the cavity of a calixarene molecule; its nitrogen atom is directed exo to this calixarene molecule and is involved in a hydrogen bond with one of the hydroxy groups of a neighbouring calixarene molecule. This scheme leads to columns of alternating host and guest molecules. The other Et3N molecule is in the interhost space. This feature allows us to define the title compound as a complex/clathrate hybrid.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01045984
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  • 159
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    The crystal structure of the syn-proximal-5,11,17,23-tetra-tert-butyl-25,26-bis[(2-pyridylmethyl)oxy]-27,28-dihydroxy-calix[4]arene ethanol 1 : 1 Inclusion Complex (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 14 (1992), S. 349-356 
    Details
    ISSN: 1573-1111
    Keywords: 1,2-Dialkylated calix[4]arene ; crystal structure ; ethanol inclusion complex ; intramolecular hydrogen bonding patterns
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structure of the title compound (1 · C2H5OH) has been determined by single-crystal X-ray analysis and refined to anR-value of 0.074 for 2732 observed reflections [I 〉 2.0σ(I)]. Crystals are triclinic, space group P $$\bar 1$$ , witha = 13.6150(18),b = 13.7195(11),c = 16.5497(16) Å, α = 73.132(7),β = 66.165(9), γ = 65.580(8)° andZ = 2. Calix[4]arene (1) adopts a relatively open distorted cone conformation in the solid state, with two pendantsyn-proximal O-CH2-Py groups. The major conformation determining features in (1 · C2H5OH) are the presence of (a) an intramolecular O-H...O hydrogen bond between adjacent proximal phenolic oxygens, O...O 2.719(7) Å and (b) an intramolecular O-H...N hydrogen bond between a phenolic oxygen and a proximal pyridinyl nitrogen, O...N 2.810(8) Å. The intramolecular hydrogen bonding and the interplanar angles of 65.1(3) and 50.7(3)° between opposite aromatic rings facilitate the inclusion of an ethanol molecule within the calixarene cup.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01045993
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  • 160
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    Tribracchial lariat ethers: Syntheses, binding, and formation of an intramolecular macroring-sidearm complex in the absence of any cation (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 12 (1992), S. 187-197 
    Details
    ISSN: 1573-1111
    Keywords: Cation binding ; crown ether ; crystal structure ; lariat ether ; synthesis ; triaza-18-crown-6
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Details of a new synthetic approach to 4,10,16-triaza-18-crown-6 (‘triaza-18-crown-6’) are reported, along with the preparation and binding properties of the following derivatives having the indicated sidearms: CH2C≡CH, CH2CH2OH, CH2CH2OCH3, COCH2OCH3,CH2COOCH2CH3, CH2C6H5, and CH2C6H4−2−NO2. A key intermediate in the synthesis of triaza-18-crown-6 is 4-N-toluenesulfonyl-1,7,13-trioxa-4,10,16-triazacyclooctadecane-9,17-dione. This compound is found by solid state structure analysis to fold to form an intramolecular, doubly-hydrogen bonded complex in which the two N-H protons interact with the two tosyl group oxygens. Details of the structure are reported.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01053861
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  • 161
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    Absolute configuration and conformation of the pure opioid antagonist (+)-2,9α-dimethyl-5-(m-hydroxyphenyl)morphan (1992)
    New York, NY [u.a.] : Wiley-Blackwell
    Chirality 4 (1992), S. 377-383 
    Details
    ISSN: 0899-0042
    Keywords: crystal structure ; molecular mechanics ; MM2-87 ; phenylmorphan ; phenyl-equatorial ; opioid ligand model ; μ-receptors ; K-receptors ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: (+)-2,9α-Dimethyl-5-(m-hydroxyphenyl)morphan is the only phenylmorphan analog whose affinity for opioid K-receptors is greater than its affinity for opioid κ-receptors. Pharmacologically, the compound is a pure opioid antagonist devoid of agonist activity in in vivo assays of antinociception. The absolute configuration of the compound has been determined to be (1R,5S,9R) from an X-ray crystallographic study of the chloride salt. Thus, the absolute configuration corresponds to that of the atypical opioid agonist (-)-phenylmorphan while the weak atypical agonist (-)-2,9α-dimethyl-5-(m-hydroxyphenyl)morphan corresponds to the potent morphine-like (+)-phenylmorphan. The preferred orientations of the phenyl ring for the two stereoisomers were determined using the molecular mechanics program MM2-87 and found to vary from that of the two parent compounds. The atypical properties of the two 9α-methyl analogs is consistent with an opioid ligand model which proposes that morphine-like properties require a particular range of phenyl orientations. There was good agreement between the structure obtained from X-ray crystallography and computed with the MM2-87 program. © 1992 Wiley-Liss, Inc.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/chir.530040608
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  • 162
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    Lamellar and whisker single crystals of poly(2,6-oxynaphthoate) (1992)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 30 (1992), S. 1469-1482 
    Details
    ISSN: 0887-6266
    Keywords: poly(2,6-oxynaphthoate) ; crystal structure ; whiskers ; lamellae ; unit cell ; transitions ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Electron diffraction from single crystal lamellae and whiskers of poly(2,6-oxynaphthoate) reveals the presence of at least 3 unit cells. The equatorial reflections in the patterns from the whiskers correspond to the dominant (phase I) hk0 diffraction pattern from the lamellae; phase I is monoclinic with 2 chemical repeats per physical repeat. The intensity distributions in the hk0 patterns of phase I and II resemble those of the same phases in poly(p-oxybenzoate). The hk0 reflections of phase III suggest a common internapthalene unit spacing, but variable lateral (and possibly axial) shifts; apparently related orthorhombic and monoclinic patterns, with variable γ*, are observed. At elevated temperature, above the crystalliquid crystal transition (ca. 330°C), quadrant reflections are retained; the change in the hk0 pattern from any given crystal is gradual, extending over some 40°C. Above the liquid crystal-liquid crystal transition (ca. 460°C) the pattern can be interpreted in terms of nematic or possibly smectic A packing. © 1992 John Wiley & Sons, Inc.
    Additional Material: 19 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/polb.1992.090301306
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  • 163
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    Ein neues Syntheseverfahren für die Wolframbronze Cs0,29WO3 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 95-98 
    Details
    ISSN: 0044-2313
    Keywords: Tungsten bronze, Cs0.29WO3 ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Novel Synthetic Access to the Tungsten Bronze Cs0.29WO3 and its Crystal StructureThe hexagonal tungsten bronze Cs0.29WO3 was obtained in form of black, prismatic crystal by the reduction of WO3 with molten cesium iodide at 700°C. Its crystal structure was determined by X-ray diffraction (399 unique observed reflexions, R = 0.058). Crystal data: a = 741.2(3), c = 760.0(5) pm, space group P6322, Z = 6. It corresponds to the known structure of hexagonal tungsten bronzes, having tungsten atoms displaced from the octahedra centres by 11.9 pm and with three different W—O bond lengths (198, 191, 187 pm). The WO6 octahedra are slightly titled mutually.
    Notes: Bei der Reaktion von WO3 in einer Caesiumiodid-Schmelze bei 700°C entsteht die hexagonale Wolframbronze Cs0.29WO3 in Form schwarzer, hexagonal-prismatischer Kristalle. Ihre Struktur wurde durch Röntgenbeugung bestimmt (399 beobachtete unabhängige Reflexe, R = 5,8%). Kristalldaten: a = 741,2(3), c = 760,0(5) pm, Raumgruppe P6322, Z = 6. Es handelt sich um die bekannte Struktur der hexagonalen Wolframbronzen mit Wolframatomen, die aus den Oktaedermitten um 11,9 pm herausgerückt sind und mit drei verschiedenen W—O-Bindungslängen (198, 191, 187 pm). Die WO6-Oktaeder sind leicht gegeneinander verkippt.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926090318
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  • 164
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    Röntgenstrukturanalyse des 1,3-Bis(diethylamino)-1,3-dibenzyl-2,4-diphenyl-1λ5, 3λ5-diphosphets (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 99-102 
    Details
    ISSN: 0044-2313
    Keywords: Diphosphete ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: X-Ray Crystal Structure Determination of 1,3-Bis(diethylamino)-1,3-dibenzyl-2,4-diphenyl-1λ5, 3λ5-diphospheteBenzylidene-diethylamino-benzylfuorophosphorane, 1, reacts with lithium bis(trimethylsilyl)amide to give the title compounds 2 and 1-diethylamino-2,3-diphenylphosphirane, 3. Only one of the stereoisomers of 2 is formed in which the two benzyl groups are located on the same side of the planar four-membered ring. 2 crystallizes in the monoclinic space group P21/n.
    Notes: Benzyliden-diethylamino-benzylfuorphosphoran, 1, reagiert mit Lithium-bis(trimethylsilyl)-amid zur Titelverbindung 2 und 1-Diethylamino-2,3-diphenylphosphiran, 3. Von 2 wird nur das Stereoisomer gebildet, bei dem die beiden Benzylgruppen auf der gleichen Seite des ebenen viergliedrigen Rings angeordnet sind. 2 kristallisiert in der monoklinen Raumgruppe P21/n.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926090319
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  • 165
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    Structures of Xenon Oxygen Compounds (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 153-156 
    Details
    ISSN: 0044-2313
    Keywords: Xenon oxygen compounds ; Xe(OTeF5)4 ; O2Xe(OTeF5)2 ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Strukturen von Xenon-Sauerstoff-VerbindungenDie Struktur des lange bekannten Xe(OTeF5)4 wurde durch die Kristallstrukturanalyse aufgeklärt. Das Xenonatom ist von vier Sauerstoffatomen in einer regelmäßigen quadratisch planaren Anordnung umgeben. O2Xe(OTeF5)2 ensteht gemäß O — Xe(OTeF5)4 → O2Xe(OTeF5)2 + F5Te—O—TeF5. Die Struktur - wiederum mit Hilfe der Röntgenstrukturanalyse bestimmt - zeigt das Xenonatom in einer sehr verzerrten tetraedrischen oder pseudo-trigonal bipyramidalen Umgebung. Das Elektronenpaarabstoßungsmodell versagt hier bei der Erklärung der Feinheiten dieser Struktur.
    Notes: The structure of long known Xe(OTeF5)4 is established by x-ray crystallography. The xenon atom is surrounded by four equidistant oxygen atoms in a square planar manner. O2Xe(OTeF5)2 is formed according to OXe(OTeF5)4 → O2Xe(OTeF5)2 + F5TeOTeF5, Its structure, again established by x-ray crystallography, shows a very distorted tetrahedral or pseudo-trigonal bipyramidal xenon environment. The electron pair repulsion models fails here in explaining the details of this geometry.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926090327
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  • 166
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    Synthese und Kristallstruktur von Hydronium-tris-ethylendiamin-cobalt(rhodium)-μ-trichloro-nonachlorotrirhenat(II)-chlorid, H3O[MEn3][Re3Cl12]Cl (M=Co, Rh) (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 607 (1992), S. 91-95 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium complexes ; synthesis ; 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 Hydronium-tris-ethylenediamine-cobalt(rhodium)-μ-trichloro-nonachlorotrirhenate(III)-chloride, H3O[MEn3][Re3Cl12]Cl (M=Co, Rh)The chlorides H3O[MEn3][Re3Cl12]CI (M = Co, 1; Rh, 2) crystallize from hydrochloric acid solutions of ReCl3 and MEn3 · 3H2O as deep red hexagonal columns. They are isotypic and crystallize with the hexagonal system (P6, Z = 1; 1: a = 1010.87(3); c = 794.30(4) pm, R = 0.023, Rw = 0.016; 2: a = 1018.58(3); c = 794.74(4) pm, R = 0.026, Rw = 0.018). The anions [Re3Cl12]3- are connected via H3O+ cation (C.N. 3). The large channels that run in the [001] direction contain, alternatively, the cations [MEn3]3+ and the lonesome Cl--anions
    Notes: Die Chloride H3O[MEn3][Re3CI12]CI(M = Co, 1; Rh, 2) Kristallisieren in Form tiefroter hexagonaler Säulen aus salzsauren Lösungen von ReCI3 und MEn3CI3 · 3H2O aus. Sie sind isotyp und Kristallisieren im hexagonalen System (P6, Z = 1; 1: a = 1010,87(3); C = 794,30(4)pm, Rw = 0,016; : a = 1018,58(3); c = 794,74(4)pm, R = 0,026, Rw = 0,018). Die Anionen [ Re3Cl12]3- werden über H3O+ (C.N. 3) verknüpft; in die entstehenden Kanäle sind längs [001] abwechselnd die Kationen [MEn3]3+ und die einsamen Cl--Ionen eingelagert.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926070115
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  • 167
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    Neue Untersuchungen an quaternären Fluoriden (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 607 (1992), S. 121-123 
    Details
    ISSN: 0044-2313
    Keywords: Quaternary fluorides ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Investigations on Quaternary FluoridesFor the first time the quaternary fluorides M12MIILnF7 (M1 = Na, Ag; MII = Ca, Cd; Ln = Er—Lu) had been prepared and examined with with X-ray diffraction. All these compounds crystallize in a cubic face-centered lattice. Colourless single crystals of Na2CdYbF7 were obtained and the structure was determined. Na2CdYbF7 crystallizes in the space group Fm3M-O5h, No. 225. The single-crystal diffraction data refer to a Defect-Fluorite-Structure. The R-value for 332 observed (29 independend) reflections is 2.2%.
    Notes: Erstmals wurden die quarternären Fluoride M12M11LnF7 (M1 = Na, Ag; M11 = Ca, Cd; Ln = Er—Lu) dargestellt und röntgenographisch untersucht. Alle Verbindungen kristallisieren kubisch flächenzentriert. An farblosen Einkristallen von Na2CdYbF7 wurde eine Strukturbestimmung durchgeführt. Na2CdYbF7 kristallisiert in der Raumgruppe Fm3m-O5h, Nr. 225. Die Meßwerte verweisen auf eine Defekt-Fluorit-Struktur. Der R-Wert fär 332 beobachtete (29 unabhängige) Röntgenreflexe beträgt 2,2%.
    Additional Material: 3 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19926070120
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    Zur Addition von Übergangsmetallhalogeniden an Acetylacetonate zweiwertiger Metallionen (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 614 (1992), S. 65-72 
    Details
    ISSN: 0044-2313
    Keywords: Transition metal halides acetylacetonate complexes ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Addition of Transition Metal Dihalides to Acetylacetonates of Divalent Metal IonsTransition metal dihalides aMIIX2 (FeCl2, CoCl2 NiBr2 etc.) are added by the chelates MII(acac)2 under formation of binuclear complexes (THF)2MII(acac)2(aMIIX2). The octahedral and the tetrahedral centre of these compounds are connected by tridentate oxygen atoms of the two acetylacetonato ligands which are simultaneously included in four-membered rings (MIIO2aMII). The addition is combined with a deformation of the octahedral centre, as a prerequisite of a closest package of the atoms within the MIIO2aMII-ring.In the trinuclear complex (THF)2Ni(acac)2(HgCl2)2 III the interaction between the three coordination centres is weak. No structural change of the octahedral centre (THF)2Ni(acac)2 is found, but the HgCl2-groups diverge slightly from linearity (Cl—Hg—Cl 171.1°).No binuclear complexes with a central ion of the oxidation state III in the octahedral centre were obtained. One reason is the lowered donor strength of the bidentate Lewis base function of the octahedral centre [(THF)2Mn+(acac)2]n-2 with M+3 as a centralatom. Reacting systems with di- and trivalent ions prefer ionic complexes, as it is shown by the formation of [(THF)2V(acac)2][(THF)CoCl3] IV from VCl3 and Co(acac)2.The crystal structures of (THF)2Co(acac)2CoCl2II and [(THF)2V(acac)2][(THF)CoCl3] IV were determined by x-ray diffraction. II: orthorhombic-primitive; space group P212121, Z = 4; a = 967.4(2), b = 1453.4(3), c = 1715.9(4) pm; R = 0.049 for 3084 observed reflections. IV: triclinic; space group P1, Nr. 2; Z = 2; a = 871,5(2), b = 930,6(3), c = 1865,6(6) pm; α = 101,70(2), b̃ = 92,45(2), γ = 91,06(2)°; R = 0,060 für 4221 observed reflections.
    Notes: Bis(acetylacetonate) von Magnesium(II), Cobalt(II) oder Nickel(II) addieren Dihalogenide wie FeCl2, CoCl2 oder NiBr2 (aMIIX2) unter Bildung binuklearer Komplexe (THF)2MII(acac)2(aMIIX2), in denen ein oktaedrisches und ein tetraedrisches Zentrum über zwei dreibindige Sauerstoffatome der Acetylacetonatliganden miteinander verknüpft sind (Bildung eines viergliedrigen MIIO2aMII-Ringes). Die Addition ist mit einer Deformation des oktaedrischen Zentrums verbunden, die eine dichte Packung der vier Atome des MIIO2aMII-Ringes ermöglicht.Im trinuklearen Komplex (THF)2Ni(acac)2(HgCl2)2 III bleibt die Wechselwirkung zwischen den drei Koordinationszentren gering. Das oktaedrische Zentrum (THF)2Ni(acac)2 wird strukturell nicht verändert, allerdings weichen die beiden HgCl2-Bausteine (Valenzwinkel 171,1°) von der Linearität ab.Es gelang nicht, binukleare Komplexe mit einem Zentralatom der Oxidationsstufe III im oktaedrischen Zentrum darzustellen. Ein Grund dafür ist die verringerte Donorstärke der zweizähligen Lewisbasen-Funktion im oktaedrischen Zentrum [(THF)Mn+(acac)2]n-2 für M+3 als Zentralion. Reaktive Systeme mit zwei- und dreiwertigen Kationen weichen auf die Seite von ionischen Komplexen aus, wie die Bildung von [(THF)2V(acac)2][(THF)CoCl3] IV aus VCl3 und Co(acac)2 zeigt.Die Kristallstrukturen von (THF)2Co(acac)2CoCl2 II und [(THF)2V(acac)2][(THF)CoCl3] IV wurden durch Röntgenbeugung bestimmt.II: orthorhombisch primitiv, Raumgruppe P212121, Z = 4; a = 967,4(2), b = 1453,4(3), c = 1715,9(4) pm; R = 0,049 für 3084 beobachtete Reflexe.IV: triklin, Raumgruppe P1, Nr.2; Z = 2; a = 871,5(2), b = 930,6(3), c = 1865,6(6) pm; α = 101,70(2), b̃ = 92,45(2), γ = 91,06(2)°; R = 0,060 für 4221 beobachtete Reflexe.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926140813
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    Die Kristallstrukturen von Me3SiI · β-Picolin und Me3SiI · γ-Picolin Vergleich der Lewis-Basen Pyridin, β-Picolin und γ-Picolin (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 145-150 
    Details
    ISSN: 0044-2313
    Keywords: Iodinetrimethylsilane · β-picoline ; -.γ-picoline ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Me3SiI · β-Picoline and Me3SiI · γ-Picoline A Comparison between the Lewis-Bases Pyridine, β-Picoline, and γ-PicolineThe reaction of Iodinetrimethylsilane with β- und γ-Picoline (Pic) leads to solid 1 : 1 compounds Me3SiI · β-Picoline 1, Me3SiI · γ-Picoline 2. The reaction was performed at room temperature. Yellow single crystals were obtained by sublimation. Single crystal X-ray investigations confirm that both compounds are ionic [Me3SiPic]+I-. The comparison of β-Picoline with γ-Picoline and Pyridine (Py) demonstrates that the presence of a methyl group and also its position has no significant influence on the Si—N bond length in compound 1, 2 and on the adduct Me3SiI · Py.
    Notes: Iodtrimethylsilan reagiert mit β- und γ-Picolin (Pic) bei Raumtemperatur zu festen 1 : 1 Addukten (M3SiI · β-Picolin 1, Me3SiI · γ-Picolin 2), die durch Sublimation leicht gelblich gefärbte Einkristalle bilden. Die Röntgenstrukturanalyse beider Verbindungen beweist eine ionische Struktur des Typs [Me3SiPic]+ I-. Der Vergleich von β-Picolin mit γ-Picolin und Pyridin (Py) zeigt, daß die Anwesenheit einer Methylgruppe und auch deren Position keinen signifikanten Einfluß auf die Si—N-Bindungslänge in Verbindung 1, 2 und dem Addukt Me3SiI · Py hat.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926100124
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    Hydrate schwacher und starker Basen. VII. Zum System Caesiumhydroxid-Wasser: Die Kristallstrukturen von CsOH · 2H2O und CsOH · 3H2OHerrn Professor Joseph Grobe zum 60. Geburtstage am 2. November 1991 gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 608 (1992), S. 123-130 
    Details
    ISSN: 0044-2313
    Keywords: Cesium hydroxide hydrates ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Hydrates of Weak and Strong Bases. VII. Concerning the System Cesium Hydroxide - Water: The Crystal Structures of CsOH · 2H2O and CsOH · 3H2OIn the context of structural studies of hydrates of the alkali metal hydroxide the crystal structure of CsOH · 2H2O and CsOH · 3H2O have been determined for the first time. The diffractometer data, obtained at -150 · C,made it possible to locate and refine also all the H-atoms. The dihydrate was found to probably form only one phase, melting incongruently at 2,5 · C. It is orthorhombic with space group Pca21 and Z = 8 formula units per unit cell. The lattice constants are a = 13.238, b = 6.747 and c = 9.121 A. With 1870 independent observed reflection a final R value of 0.013 was obtained. The trihydrate, melting congruently et -5.5 ·C, is monoclinic with space group P21/n,Z = 4 and lattice constants a = 8.637, b = 5.984, c = 10.061 Å and ß = 96.57 ·. With 2098 independent observed reflection the final R is 0.026. In both hydrate structures there are no simple characteristic coordination polyhedra for the cations; in each case it is rather the hydrogen-bonded and fully ordered anionic water structure which shows up as the determining building principle. Both these water structures are altogether three-dimensional, but primarily contain layers. The anionic layers are formed by condensation of small and medium rings, namely four-, five- and seven-membered rings in CsOH · 2H2O and four-, five- and six membered ones in CsOH · 3H2O. They are linked together by one set each of extra H2O molecules between the layers as well as by the Cs+ ions.
    Notes: In Zusammenhang mit Untersuchungen zur Struktur von Hydraten der Alkalimetallhydroxide wurden die Kristallstrukturen von CsOH · 2H2O und CsoH · 3H2O erstmalig bestimmt. Die bei - 150°C erhaltenen Diffraktometerdaten erlaubten dabei auch die Lokalisierung und Verfeinerung Sämtlicher H-Atome. Das nach eigenen Untersuchungen wahrscheinlich nur einphasig vorliegende Dihydrat schmilzt inkongruent bei 2,5°C und kristallisiert orthorhombisch mit der Raumgruppe Pca21 und Z = 8 Formeleinheiten pro Elementarzelle sowie den Gitterkonstanten a = 13,238, b = 6,747 und c = 9,121 ß. Mit 1870 unabhängigen beobachteten Reflexen wurde ein abschließender R-Wert von 0,013 erreicht. Das bei - 5,5°C kongruent schmelzende Trihydrat ist monoklin mit der Raumgruppe P21/n und Z = 4. Die Gitterkonstanten betragen a = 8,637, b = 5,984, c = 10,061 A und ß = 96,57°. Mit 2098 unabhängigen beobachteten Reflexen liegt der abschließende R-Wert bei 0,026. In beiden Hydratstrukturen gibt es keine einfachen charakteristischen Koordinationspolyeder für die Kationen; vielmehr wird jeweils die durch H-Brücken gebildete und vollständig geordnete anionische Wasserstruktur zum bestimmenden Bauprinzip. Beide Wasserstrukturen sind insgesamt dreidimensional, enthalten primär aber Schichten. Die aus Kondensierten Kleinen und mittleren Ringen, nämlich Vier-, Fünf - und Siebenringen (CsOH · 2H2O) bzw. Vier-, Fünf- und Sechsringen (CsOH · 3H2O), bestehenden anionischen Schichten werden jeweils über einen Satz weiterer H2O-Moleküle zwischen den Schichten sowie über die Cs+-Ionen miteinander verknüpft.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926080218
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    Bis(triphenylphosphaniminato)niobtrichlorid, [NbCl3(NPPh3)2], ein Komplex mit fünffach koordiniertem NiobProfessor Osvald Knop zum 70. Geburtstage am 11. Juli 1992 gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 7-10 
    Details
    ISSN: 0044-2313
    Keywords: Phosphorane iminato complex of niobium ; synthesis ; IR spectrum ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Bis(triphenylphosphorane-iminato)niobium Trichloride, [NbCl3(NPPh3)2], a Complex with Coordination Number Five at the Niobium AtomThe title compound has been prepared from niobium pentachloride with Me3SiNPPh3 in acetonitrile solution, forming colourless, moisture sensitive crystals. They were characterized by IR spectroscopy and by an X-ray structure determination. [NbCl3(NPPh3)2] crystallizes monoclinically in the space group Cc with four formula units per unit cell, 3682 observed, unique reflections, R = 0.042%. Lattice dimensions at 20°C: a = 1025.1(2); b = 1870.6(6); c = 1832.5(5) pm, β = 91.83(2)°. The niobium atom of the complex is coordinated in a distorted trigonal bipyramidal fashion, while the nitrogen atoms of the two phosphorane iminato ligands are in equatorial position along with one chlorine atom. NbN and PN distances accord with double bonds; with a mean value of 242.0 pm the Nb—Cl distances are remarkably long.
    Notes: Die Titelverbindung entsteht in Form farbloser, feuchtigkeitsempfindlicher Kristalle bei der Reaktion von Niobpentachlorid mit Me3SiNPPh3 in Acetonitrillösung. Sie wird durch das IR-Spektrum und eine röntgenographische Strukturanalyse charakterisiert. [NbCl3(NPPh3)2] kristallisiert monoklin in der Raumgruppe Cc mit vier Formeleinheiten pro Elementarzelle, 3682 beobachtete unabhängige Reflexe, R = 4,2%. Gitterabmessungen bei 20°C: a = 1025,1(2); b = 1870,6(6); c = 1832,5(5) pm, β = 91,83(2)°. In dem Komplex ist das Niobatom verzerrt trigonal-bipyramidal koordiniert, wobei die N-Atome der beiden Phosphaniminatoliganden zusammen mit einem Chloratom äquatorial angeordnet sind. NbN- und PN-Abstände entsprechen Doppelbindungen; die Nb—Cl-Abstände sind mit dem Mittelwert von 242,0 pm auffällig lang.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926150902
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    Die Kristallstruktur von Na2NiAlF7 - ein Beitrag zum Problem der wahren Raumgruppe orthorhombischer WeberiteProfessor Osvald Knop zum 70. Geburtstage am 11. Juli 1992 gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 11-15 
    Details
    ISSN: 0044-2313
    Keywords: Weberite ; crystal structure ; nickel aluminium fluoride ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Na2NiAlF7  -  a Contribution to the Problem of the True Space Group of Orthorhombic WeberitesThe X-ray single crystal structure determination of the orthorhombic weberite Na2NiAlF7 (a = 707.4(2), b = 1003.8(2), c = 731.5(1) pm; Z = 4) was performed in space group Imma, after all reflections hk0 with h(k) = 2n + 1 could be eliminated, as they proved simulated by Renninger effect and/or λ/2 reflections. The alternative space groups Imm2 resp. I212121 of former weberite structure determinations thus became obsolete. The refinement using 880 independent reflections ended at wR = 0.0232. The resulting average distances within the framework of octahedra are Ni—F = 197.3, Al—F = 180.4 pm.
    Notes: Die Röntgen-Einkristallstrukturbestimmung des orthorhombischen Weberits Na2NiAlF7 (a = 707,4(2), b = 1003,8(2), c = 731,5(1) pm; Z = 4) wurde in der Raumgruppe Imma vorgenommen, nachdem alle Reflexe hk0 mit h(k) = 2n + 1 eliminiert werden konnten, weil sie sich durch Renninger-Effekt und/oder λ/2-Reflexe als vorgetäuscht erwiesen. Damit wurden die alternativen Raumgruppen Imm2 bzw. I212121 früherer Weberit-Strukturbestimmungen obsolet. Die Verfeinerung mit 880 unabhängigen Reflexen schloß ab mit wR = 0,0232. Die resultierenden Mittelwerte für die Abstände im Oktaedernetz betragen Ni—F = 197,3 pm, Al—F = 180,4 pm.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926150903
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    Molekül- und Kristallstruktur von Ytterbium(III)-triaqua-trinitrat, Yb(H2O)3(NO3)3 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 16-18 
    Details
    ISSN: 0044-2313
    Keywords: Ytterbium nitrates ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Molecular and Crystal Structure of Ytterbium(III)-triaqua-trinitrate, Yb(H2O)3(NO3)3Yb(H2O)3(NO3)3 crystallizes from a concentrated solution of Yb2O3 in nitric acid in a vacuum desiccator at ambient temperature as colourless single crystals. The crystal structure was determined from single crystal four-circle diffractometer data (R3, Z = 6, a = 1175.5(1), c = 1117.7(2) pm, Vm = 134.25 cm3/mol, R = 3.0%, Rw = 2.9%). The structure may be viewed at as a heavily compressed packing of [Yb(H2O)3(NO3)3] molecules. Yb3+ is coordinated by three bidentate nitrate ligands and three water molecules so that a tricapped trigonal prism (C.N. 9) of oxygen atoms results as the coordination polyhedron.
    Notes: Yb(H2O)3(NO3)3 kristallisiert aus einer konzentrierten Lösung von Yb2O3 in Salpetersäure im Vakuumexsikkator bei Raumtemperatur in Form farbloser Einkristalle aus. Die Kristallstruktur wurde aus Einkristall-Vierkreis-Diffraktometer-Daten bestimmt (R3, Z = 6, a = 1175,5(1), c = 1117,7(2) pm, Vm = 134,25 cm3/mol, R = 3,0%, Rw = 2,9%). Sie kann als stark gestauchte Kugelpackung von [Yb(H2O)3(NO3)3]- Molekülen aufgefaßt werden. In diesen ist Yb3+ von drei zweizähnigen Nitratliganden und drei Wassermolekülen in Form eines dreifach bekappten trigonalen Prismas (C. N. 9) von Sauerstoffatomen umgeben.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926150904
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    Chelate von Chinolin-8-ol-Derivaten. XIIXI. Mitt. s. [1].. Die Kristall- und Molekülstruktur von Bis(7-isopropylchinolin-8-olato)nickel(II) (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 39-42 
    Details
    ISSN: 0044-2313
    Keywords: Bis(7-isopropyl-8-quinolinato)nickel(II) ; crystal structure ; association of nickel 8-quinolates ; steric hindrance ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chelates of 8-Quinolinol Derivatives. XII. Crystal and Molecular Structure of Bis(7-isopropyl-8-quinolinato)nickel(II)The crystal and molecular structure of bis(7-isopropyl-8-quinolinato)nickel(II) was determined by X-ray diffraction. The structure is monoclinic with the space group P21/n (Z = 2, 1403 observed independent reflections, R = 0.049. Lattice dimensions at 20°C: a = 1328.3(5) pm, b = 632.8(2) pm, c = 1330.0(5) pm, β = 112.99(3)°). The coordination of the nickel atom is planar with the quinoline rings in trans position.
    Notes: Die Kristallstruktur von Bis(7-isopropylchinolin-8-olato)nickel(II) wurde durch eine Röntgenkristallstrukturuntersuchung bestimmt. Es liegt ein monoklines Kristallsystem mit der Raumgruppe P21/n vor (Z = 2, beobachtete unabhängige Reflexe 1403, R = 4,9%, Gitterabmessungen bei 20°C: a = 1328,3(5) pm, b = 632,8(2) pm, c = 1330,0(5) pm, β = 112,99(3)°). Das Nickelatom ist planar koordiniert mit den beiden Chinolinringen in trans-Stellung.
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    URL: http://dx.doi.org/10.1002/zaac.19926150908
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    Zur Kristallstruktur von Ba2ZnO3 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 17-20 
    Details
    ISSN: 0044-2313
    Keywords: Barium ; zinc ; oxygen ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Crystal Structure of Ba2ZnO3Single crystals of Ba2ZnO3 were prepared by solid state reaction. It crystallizes monoclinic: space group C62h — C12/c1; a = 5.833; b = 11.376; c = 12.585 Å; β = 93.63°; Z = 8. The crystal structure is characterised by 1∞[ZnO3] chains along [100]. They are connected by Ba2+ in seven fold oxygen coordination.
    Notes: Ba2ZnO3 wurde durch Festkörperreaktion in einkristalliner Form dargestellt. Es kristallisiert in der Raumgruppe C62h — C12/c1; a = 5,833; b = 11,376; c = 12,585 Å, β = 93,63°; Z = 8. Die Kristallstruktur ist durch 1∞[ZnO3]-Ketten längs [100] gekennzeichnet. Diese werden durch Ba2+ (siebenfach durch O2- koordiniert) verknüpft.
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    Ein neues Oxometallat mit Mangan(II): Ba5Mn4Nd8O21 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 21-24 
    Details
    ISSN: 0044-2313
    Keywords: Barium ; manganese ; neodymium ; oxygen ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On a New Oxometallate of Manganese (II): Ba5Mn4Nd8O21Single crystals of Ba5Mn4Nd8O21 were prepared for the first time by CO2-Laser technique using H2-atmosphere. It was investigated by a single crystal X-ray diffractometer study. Ba5Mn4Nd8O21 crystallizes with tetragonal symmetry space group: C54h—I4/m; a = 14.2104 Å; c = 5.8581 Å; Z = 2. Mn2+ is found in square pyramids of oxygen.
    Notes: Ba5Mn4Nd8O21 wurde erstmals mit CO2-Lasertechnik in H2-Atmosphäre dargestellt und an Einkristallen röntgenographisch untersucht. Es kristallisiert tetragonal in der Raumgruppe C54h—I4/m; a = 14,2104 Å; c = 5,8581 Å; Z = 2. Mn2+ liegt in tetragonal pyramidaler Sauerstoffkoordination vor.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926120105
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    Synthese und Strukturuntersuchungen von Iodocupraten(I). XV Iodocuprate(I) mit solvatisierten Kationen: [Li(CH3CN)4]1∞[Cu2I3] und [Mg{(CH3)2CO}6][Cu2I4] (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 45-50 
    Details
    ISSN: 0044-2313
    Keywords: Iodocuprates(I) ; solvated cations ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure Investigations of Iodocuprates(I). XV Iodocuprate(I) with Solvated Cations: [Li(CH3CN)4]1∞[Cu2I3] and [Mg{(CH3)2CO}6][Cu2I4][Li(CH3CN)4]1∞[Cu2I3] 1 and [Mg((CH3)2CO)6][Cu2I4] 2 were prepared by reactions of CuI with LiI in acetonitrile and of CuI with MgI2 in acetone. 1 crystallizes orthorhombic, Pnma, a = 552.7(2), b = 1258.8(8), c = 2516(1) pm, z = 4. [Li(CH3CN)4]+ cations are located between rod packings of CuI4 tetrahedra double chains 1∞ [(CuI2/2I2/4)2]- parallel to the axis. Short intermolecular anion/cation contacts were observed. The crystal structure of 2 (monoclinic, P21/n, a = 1840(2), b = 1059.2(2), c = 1879(2)pm, β = 112.94(4)°, z = 4) is built up by [Mg((CH3)2CO)6]2+ cations forming a simple hexagonal sphere packing. The binuclear anions [Cu2I4]2- occupy holes in the trigonal prismatic channels formed by the cations.
    Notes: [Li(CH3CN)4]1∞[Cu2I3] 1 und [Mg((CH3)2CO)6][Cu2I4] 2 wurden durch Umsetzung von CuI mit LiI in Acetonitril bzw. von CuI mit MgI2 in Aceton dargestellt. 1 kristallisiert orthorhombisch, Pnma, a = 552,7(2), b = 1258,8(8), c = 2516(1) pm, z = 4. Zwischen Stabpackungen von CuI4-Tetraederdoppelketten 1∞[(CuI2/2I2/4)2]- parallel zur a-Achse sind [Li(CH3CN)4]+ -Kationen unter Ausbildung kurzer, intermolekularer Anionen-Kationen-Kontakte eingelagert. In der Kristallstruktur von 2 (monoklin, P21/n, a = 1840(2), b = 1059,2(2), c = 1879(2) pm, β = 112,94(4)°, z = 4) sind [Mg((CH3)2CO)6]2+ -Kationen in der Art einer hexagonal einfachen Kugelpackung angeordnet. In die dabei gebildeten, trigonal prismatischen Kanäle sind die zweikernigen Anionen [Cu2I4]2- eingebaut.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926120109
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  • 178
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    Vorstufen für polymere Silazane mit Fluoralkyl-Seitenketten und ihr Kondensationsverhalten (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 101-106 
    Details
    ISSN: 0044-2313
    Keywords: (Trifluoroethyl)aminosilane ; silane tetramin; alkylsilazalane ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preliminary Stages of Polymeric Silazanes with Fluoroalkyl Side Chains and their Condensation BehaviourTetrakis(2,2,2-trifluoroethyl)aminosilane has been synthesized by aminolysis of silicon tetrachloride with 2,2,2-trifluorethylamine. The characterisation of the silane tetramine was carried out spectroscopically and by X-ray-methods. The thermal condensation has been investigated between 60°C and 300°C. At 300°C the formation of oligospirocycloorganoazanes was observed which have been identified spectroscopically. The new silane tetramine reacts with trimethylalumina in toluene. The product has been characterized by crystal structure analysis to be a dimeric (C18H26N8F24Si2Al2). (P1; a = 920.39(9), b = 943.32(2), c = 1235.4(1) pm, α = 68.8(7)°, β = 86.9(4)°, γ = 62.6(4)°, Z = 1, 3923 independent reflections; R = 0.059, Rw = 0.054)
    Notes: Tetrakis[(2,2,2-trifluorethyl)amino]-silan wurde durch Aminolyse von Siliciumtetrachlorid mit 2,2,2-Trifluorethylamin dargestellt, spektroskopisch und röntgenographisch charakterisiert, sowie das thermische Kondensationsverhalten im Bereich von 60 - 300°C untersucht. Bei 300°C konnte die Bildung von Oligospirocyclo-silaorganoazanen massenspektrometrisch nachgewiesen werden. Das neu erhaltene Silantetramin wurde bei 80°C mit Trimethylaluminium im Verhältnis 1 : 1 in Toluol umgesetzt. Nach der Kristallstrukturanalyse liegt das erhaltene Alkylsilazalan im Kristall als Dimeres C18H26N8F24Si2Al2 vor. (P1; a = 920,39(9), b = 943,32(2), c = 1235,4(1) pm, α = 68,8(7)°, β = 86,9(4)°, γ = 62,6(4)°; Z = 1, 3923 unabhängige Reflexe, R = 0,059, Rw = 0,054)
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926120117
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  • 179
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    Korrektur zur Kristallstruktur von „Cs4PbO3“ und die Strukturverwandtschaft zwischen den Modifikationen von Cs4PbO4 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 143-148 
    Details
    ISSN: 0044-2313
    Keywords: Caesium tetraoxoplumbate ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Correction of the Crystal Structure of “Cs4PbO3” and the Structural Relationship between the Modifications of Cs4PbO4The compound that has been described as Cs4PbO3 really is Cs4PbO4. It does not crystallize in the space group P21, as assumed, but in P21/c. The observed fictitiuous violation of the extinction law for the c glide plane is due to twinning. The structure was refined using the original data as well as new data from an untwinned crystal. The denomination β-Cs4PbO4 is used to distinguish this structure from another known modification (α-Cs4PbO4). Both structures, α-Cs4PbO4 and β-Cs4PbO4, can be derived from the sphere packing of γ-plutonium when certain voids in its packing are occupied with oxygen atoms.
    Notes: Bei der früher als Cs4PbO3 beschriebenen Substanz handelt es sich tatsächlich um Cs4PbO4. Dieses kristallisiert nicht, wie angenommen, in der Raumgruppe P21, sondern in P21/c. Die beobachtete scheinbare Verletzung des Auslöschungsgesetzes für die c-Gleitspiegelebene ist auf Verzwillingung zurückzuführen. Die Struktur wurde sowohl mit den ursprünglichen Daten wie auch mit neuen Daten eines unverzwillingten Kristalls verfeinert. Die Bezeichnung β-Cs4PbO4 dient zur Unterscheidung von einer bereits bekannten Modifikation (α-Cs4PbO4). Beide Strukturen, α-Cs4PbO4 und β-Cs4PbO4, lassen sich von der des γ-Plutoniums ableiten, wenn bei dieser bestimmte Lücken mit Sauerstoffatomen besetzt werden.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926120124
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  • 180
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    Darstellung und Kristallstruktur von LnAl3Br12 (Ln = La, Ce, Pr, Nd, Sm, Gd) und thermischer Abbau zu LnBr3 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 613 (1992), S. 45-48 
    Details
    ISSN: 0044-2313
    Keywords: Lanthanoide bromoaluminates ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of LnAl3Br12 (Ln = La, Ce, Pr, Nd, Sm, Gd) and Thermal Decomposition to LnBr3LnAl3Br12 (Ln = La, Ce, Pr, Nd, Sm, Gd) was prepared in crystalline form for the first time. The crystal structures of LaAl3Br12, PrAl3Br12, and NdAl3Br12 were determined on single crystals by X-ray methods. The isotypic compounds crystallize with trigonal symmetry, space group P 3112, Z = 3. A structural comparison to lanthanoide chloroaluminates of equal composition is given and thermal decomposition of LnAl3Br12 (Ln = Nd) to the corresponding lanthanoide tribromide is described.
    Notes: Die Bromide LnAl3Br12 (Ln = La, Ce, Pr, Nd, Sm, Gd) wurden erstmals in kristalliner Form dargestellt und die Kristallstrukturen von LaAl3Br12, PrAl3Br12 anhand von röntgenographischen Einkristalluntersuchungen bestimmt. Alle kristallisieren in der trigonalen Raumgruppe P 3112, Z = 3. Ein struktureller Vergleich mit Lanthanoidchloroaluminaten der gleichen Zusammensetzung und der thermische Abbau von LnAl3Br12 (Ln = Nd) zum entsprechenden Lanthanoidtribromid werden beschrieben.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926130107
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  • 181
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    Zur Kristallstruktur von Cu3NbTaO8 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 613 (1992), S. 60-62 
    Details
    ISSN: 0044-2313
    Keywords: Copper ; tantalum ; niobium ; oxygen ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Crystal Structure of Cu3NbTaO8Single crystals of Cu3NbTaO8 were prepared by solid state reaction. X-ray investigations led to triclinic symmetry, space group C1i—P1 with a = 5.179; b = 5.474; c = 6.003 Å; α = 72.85°; β = 83.39°; γ = 65.77°; Z = 1. Nb5+ and Ta5+ occupy one point position statistically. Both ions show an octahedral oxygen surrounding. Cu(1) is inside an elongated CuO6 octahedra and Cu(2) is coordinated by 5 O2- forming a distorted square pyramid. The polyhedra connection is shown and discussed.
    Notes: Einkristalle von Cu3NbTaO8 wurden durch Feststoffreaktion dargestellt. Die röntgenographische Untersuchung führte zu trikliner Symmetrie, Raumgruppe C1i  -  P1 mit a = 5,179; b = 5,474; c = 6,003 Å; α = 72,85°; β = 83,39°; γ = 65,77°; Z = 1. Nb5+ und Ta5+ besetzen eine Punktlage statistisch. Beide Ionen sind oktaedrisch von O2- koordiniert. Cu(1) zeigt ein stark gestrecktes CuO6-Oktaeder, während Cu(2) tetragonal pyramidal koordiniert ist. Die Polyederverknüpfung wird gezeigt und diskutiert.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926130110
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    Chelatkomplexe von Rheniumtetrachlorid. Die Kristallstrukturen von ReCl4(DME) und ReCl4(DPPE) · Tolan (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 613 (1992), S. 49-54 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium tetrachloride chelate complexes ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chelate Complexes of Rhenium Tetrachloride. The Crystal Structures of ReCl4(DME) and ReCl4(DPPE) · TolanBright green crystals of ReCl4(DME) have been prepared by the reaction of rhenium pentachloride with dimethoxyethane (DME) in dichloromethane. ReCl4(DPPE) · tolan was obtained in form of red crystals by the reaction of the alkyne complex [ReCl4(Ph—C≡C—Ph)(POCl3)] with bis(diphenylphosphino)ethane (DPPE) in dichloromethane. The complexes were characterized by X-ray structure determinations.ReCl4(DME): Space group I42d, Z = 8, 829 observed unique reflexions, R = 0.022. Lattice dimensions at 19.5°C: a = b = 960.60(6), c = 2337.2(6) pm. The complex forms monomeric molecules with DME as chelating ligand; the Re—O bond lengths are 213.1 pm. The chlorine atoms, arranged in trans position to the chelating ligand, have slightly shorter Re—Cl bonds than the chlorine atoms in cis position (232,1 pm).ReCl4(DPPE) · tolan: Space group P21/n, Z = 4,4313 observed unique reflexions, R = 0.040. Lattice dimensions at -80°C: a = 1095.7(1), b = 1764.2(2), c = 1898.0(2) pm, β = 99.229(8)°. The compound consists in form of monomeric molecules [ReCl4(DPPE)] and diphenylacetylene molecules, which are incorporated in the lattice. The two phenyl rings of the tolan molecules are twisted towards each other along the C—C axis with a dihedral angle of 21°. The DPPE molecules are bonded to the rhenium atom in a chelating fashion with medium Re—P lengths of 250.4 pm. The chlorine atoms, arranged in trans position to this ligand, with Re—Cl bond lengths of 234.5 pm are slightly longer than the Re—Cl bonds in cis position with 232.3 pm.
    Notes: ReCl4(DME) wird in Form leuchtend grüner Kristalle durch Reaktion von Rheniumpentachlorid mit Dimethoxyethan (DME) in Dichlormethan hergestellt. ReCl4(DPPE) · Tolan erhielten wir als rote Kristalle bei der Reaktion des Alkinkomplexes [ReCl4(Ph—C≡C—Ph)(POCl3)] mit Bis(diphenylphosphino)ethan (DPPE) in Dichlormethan. Die Komplexe wurden durch röntgenographische Strukturanalysen charakterisiert.ReCl4(DME): Raumgruppe I42d, Z = 8, 829 beobachtete unabhängige Reflexe, R = 2,2%. Gitterkonstanten bei 19,5°C: a = b = 960,60(6); c = 2337,2(6) pm. Der Komplex bildet monomere Moleküle mit dem DME-Liganden als Chelat und Re—O-Abständen von 213,1 pm. Die hierzu trans-ständig angeordneten Chloratome haben mit 228,1 pm etwas kürzere Re—Cl-Bindungen als die cis-ständigen Cl-Atome (232,1 pm).ReCl4(DPPE) · Tolan: Raumgruppe P21/n, Z = 4, 4313 beobachtete, unabhängige Reflexe, R = 4,0%. Gitterkonstanten bei -80°C: a = 1095,7(1); b = 1764,2(2); c = 1898,0(2) pm, β = 99,229(8)°. Der Komplex bildet monomere Moleküle [ReCl4(DPPE)] und in das Gitter eingelagerte Diphenylacetylenmoleküle, deren Phenylringe einen Diederwinkel von 21° zueinander bilden. Die DPPE-Moleküle sind chelatartig am Rheniumatom gebunden mit Abständen Re—P von im Mittel 250,4 pm. Die hierzu trans-ständig angeordneten Chloratome sind mit Re—Cl—Abständen von 234,5 pm etwas länger als die cis-ständigen Re—Cl-Bindungen mit 232,3 pm.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926130108
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    Kristallstrukturverfeinerungen an Natriumtrifluorometallaten NaMF3 (M = Mg, Co, Ni, Zn): Oktaederkippung und Toleranzfaktor orthorhombischer FluorperowskiteProfessor Rudolf Hoppe zum 70. Geburtstage gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 616 (1992), S. 133-140 
    Details
    ISSN: 0044-2313
    Keywords: Sodium trifluorometallates ; fluoroperovskites ; crystal structure ; tolerance factor ; antiferromagnetism ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure Refinements of Sodium Trifluorometallates NaMF3 (M = Mg, Co, Ni, Zn): Tilting of Octahedra and Tolerance Factor of Orthorhombic FluoroperovskitesBased on newly measured X-ray single crystal data the crystal structures of the orthorhombic fluoroperovskites NaMF3 (M = Mg, Co, Ni, Zn) were refined in space group Pbnm (GdFeO3 type, Z = 4). The octahedra are but slightly distorted; the average distances (and bridge angles M—F—M) are: Mg—F = 197.8 pm (150.9°), Co—F = 203.8 pm (146.1°), Ni—F = 200.3 pm (148.0°) and Zn—F = 202.3 pm (147.4°). With respect to the axes of the pseudocell (Z = 1) the octahedra are rotated by tilt angles which vary, including NaMnF3 and NaFeF3, between 14.6 and 18.8°. The tilting becomes the more pronounced, the smaller the tolerance factor of the compound, so as to yield uniformly average values of Na—F = 232 pm for the four shortest distances within the [NaF8] coordination (distorted tetrahedron and bicapped trigonal prism, respectively). Measurements of magnetic powder susceptibilities show that tilting of octahedra is no sufficient cause to produce spin canting resulting in ferromagnetism: This property is confirmed only for NaNiF3 (TN = 150 K), whereas NaCoF3 exhibits a sharp minimum in its χ-l-T curve (TN = 75 K) and remains uncanted antiferromagnetic then down to 4.2 K.
    Notes: Auf der Basis neu gemessener röntgenographischer Einkristalldaten wurden die Kristallstrukturen der orthorhombischen Fluorperowskite NaMF3 (M = Mg, Co, Ni, Zn) in der Raumgruppe Pbnm verfeinert (GdFeO3-Typ, Z = 4). Die Oktaeder sind kaum verzerrt; die mittleren Abstände (und Brückenwinkel M—F—M) betragen: Mg—F = 197,8 pm (150,9°), Co—F = 203,8 pm (146,1°), Ni—F = 200,3 pm (148,0°) und Zn—F = 202,3 pm (147,4°). Unter Einbeziehung von NaMnF3 und NaFeF3 ergeben sich von 14,6 bis 18,8° variierende Kippungswinkel der Oktaeder gegen die Achsen der Pseudozelle (Z = 1). Die Oktaeder sind um so stärker gekippt, je kleiner der Toleranzfaktor der Verbindungen ist, so daß einheitlich ein Mittelwert von Na—F = 232 pm für die vier kürzesten Abstände innerhalb der [NaF8]-Koordination resultiert (verzerrtes Tetraeder bzw. zweifach überkapptes trigonales Prisma). Messungen der magnetischen Pulversuszeptibilität zeigen, daß die Oktaederkippung kein ausreichender Grund für Spinverkantung und daraus resultierenden Ferromagnetismus ist: Dieser kann nur für NaNiF3 (TN = 150 K) bestätigt werden, während NaCoF3 ein scharfes Minimum in der χ-1-T-Kurve zeigt (TN = 75 K) und dann bis herab zu 4,2 K unverkantet antiferromagnetisch bleibt.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926161020
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    Organoruthenaborane Chemistry. X. The SM2-catalysed formation of [ l-(η6-C6Me6)-isocloso-RuB9H9], and some B-phenylamino derivatives. NMR and X-ray diffraction studiesDedicated to Professor Rudolf Hoppe on his 70th Birthday (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 616 (1992), S. 79-85 
    Details
    ISSN: 0044-2313
    Keywords: Organoruthenaboranes ; ruthenium ; boranes ; n.m.r. spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Organoruthenaboran-Chemie. X. Die SMe2-katalysierte Bildung von [1-(η6-C6Me6)-isocloso-RuB9H9] und einige B-Phenylamino-Derivate. NMR- und Röntgen-UntersuchungenDie Einwirkung von SMe2, auf das zehneckige nido-Ruthenaboran [1-(η6-C6Me6)RuB9H13] (1) führt in hoher Ausbeute zum unsubstituierten isocloso-Ruthenaboran [1-(η6-C6Me6)RuB9H9] (2). Die analoge Verbindung mit Benzol [1-(η6-C6Me6)RuB9H9] wird entsprechend erhalten. Im Gegensatz dazu führt die Reaktion von (1) mit PhNH2 zu einer Reihe von B-Phenylamino-isocloso-Derivaten wie [1-(η6-C6Me6)-2-(PhNH)-isocloso-1-RuB9H8] (3) (orange Kristalle), [1-(η6-C6Me6)-2,3-(PhNH)2-isocloso-1-RuB9H7] (4) (rotorange) und [1-(η6-C6Me6)-5,6,7-(PhNH)3-isocloso-l-RuB9H6] (5) (dunkelrot). Detaillierte 1H- und 11B-NMR-Spektren werden angegeben. Die Struktur von (3) wird durch eine Einkristall-Röntgen-Strukturanalyse des Solvats [1-(η6-C6Me6)-2-(PhNH)-isocloso-1-RuB9H8] · 1/2 CH2C12 ermittelt; die Kristalle sind monoklin, Raumgruppe C2/c, mit a = 1895,1(3), b = 1556,6(3), c = 1716,4(3)pm, β = 104,37(1)° und Z = 8.
    Notes: The action of SMe2 on the ten-vertex nido-ruthenaborane [6-(η6-C6Me6)RuB9Hl3] (1) provides a high-yield route to the unsubstituted isocloso-ruthenaborane [1-(η6-C6Me6)RuB9H9] (2). The benzene analogue [1-(η6-C6Me6)RuB9H9] is prepared similarly. By contrast, reaction of (1) with PhNH2 gives a variety of B-phenylamino isocloso derivatives, including orange crystals of [1-(η6-C6Me6)-2-(PhNH)-isocloso-1-RuB9H8] (3), red-orange [1-(η6-C6Me6)-2,3-(PhNH)2-isocloso-1-RuB9H7] (4) and dark-red [1-(η6-C6Me6)-5,6,7-(PhNH)3-isocloso-1-RuB9H6] (5). Detailed 1H and 11B nmr properties of these various compounds are described. The structure of (3) has been established by a single-crystal X-ray diffraction study of the solvate [1-(η6-C6Me6)-2-(PhNH)-isocloso-1-RuB9H8] · 1/2 CH2Cl2; the crystals were monoclinic, space group C2/c, with a = 1895.1(3), b = 1556.6(3), c = 1716.4(3) pm, β = 104.37(1)° and z = 8.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926161013
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    Temperaturabhängige Phasenumwandlungen natriumreicher AmalgameProfessor Rudolf Hoppe zum 70. Geburtstage gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 616 (1992), S. 35-38 
    Details
    ISSN: 0044-2313
    Keywords: Amalgams ; sodium-rich amalgams ; phase transitions ; crystal structure ; DTA measurements ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Temperature Dependent Phase Transitions of Sodium-rich AmalgamsStarting from thermoanalytical measurements the temperature dependent phase transitions of the microcrystalline, sodium rich amalgams Na8Hg3 (= Na2.67Hg) and Na3Hg are investigated using a fast, position sensitive X-Ray detector in combination with a modified counter Guinier system. Near the melting point (64°C) Na8Hg3 shows two phase transitions.At 54°C α-Na8Hg3 forms a slightly distorted monoclinic defect variant of the cubic Li3Bi-structure (β-Na8Hg3). At 62°C this modification transforms into the corresponding undistorted cubic phase (γ-Na8Hg3). The increase of symmetry results mainly from the fact, that small deviations of the mercury atoms from the positions of an ideal close packing vanish due to strong thermal vibrations.The “literature-melting point” of Na3Hg (33°C) corresponds to a phase transition from α-Na3Hg (hexagonal, modified Na3As type) into β-Na3Hg (monoclinic distorted Li3Bi type, corresponding to β-Na8Hg3). The actual melting point of Na3Hg is 59°C.
    Notes: Ausgehend von thermoanalytischen Messungen werden die temperaturabhängigen Phasenumwandlungen der mikrokristallinen natriumreichen Amalgame Na8Hg3 (Na2.67Hg) und Na3Hg mit einem schnellen, ortsempfindlichen Röntgendetektor in Kombination mit einer modifizierten Zählrohr-Guinierkamera untersucht. Na8H3 zeigt dicht unter dem Schmelzpunkt (64°C) zwei Phasenumwandlungen: Bei 54°C wandelt sich α-Na8Hg3 zunächst in eine monoklin verzerrte Defektvariante (β-Na8Hg3) der kubischen Li3Bi-Struktur um. Daraus entsteht bei 62°C die entsprechende unverzerrte kubische Phase (γ-Na8Hg3). Die Symmetrieerhöhung resultiert aus der Aufhebung geringfügiger Abweichungen der Hg-Atompositionen von einer dichtesten Kugelpackung infolge starker thermischer Schwingung.Der „Literaturschmelzpunkt“ von Na3Hg (33°C) entspricht einer Phasenumwandlung von α-Na3Hg (hexagonal, modifizierte Na3As-Struktur) in β-Na3Hg (monoklin verzerrter Li3Bi-Typ, entsprechend β-Na8Hg3). Der Schmelzpunkt der Verbindung Na3Hg liegt dagegen tatsächlich bei 59°C.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926161006
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    Zur Kenntnis von Ba6Ru2PtO12Cl2 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 59-62 
    Details
    ISSN: 0044-2313
    Keywords: Ruthenium ; oxygen ; chlorine ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: About Ba6Ru2PtO12Cl2Single crystals of Ba6Ru2PtO12Cl12 were prepared by a BaCl2 flux and investigated by X-ray methods (D3d3—P3M1; a = 5,805; c = 15.006 Å; Z = 1). The characteristic face shared M3O12-octahedratriples show an ordered (Ru/Pt/Ru) occupation. Calculation of the Coulomb term of lattice energy support the charge distribution (5+/4+/5+) ions engage three point sites with different coordinations. The connection to other compounds are discussed.
    Notes: Durch Schmelzmittelreaktion mit BaCl2 wurde Ba6Ru2PtO12Cl2 an Einkristallen dargestellt und röntgenographisch untersucht (D3d3-P3m1; a = 5,805; c = 15,006 Å; Z = 1). Die charakteristischen flächenverknüpften M3O12-Oktaedertripel weisen eine geordnete Besetzung mit Ru/Pt/Ru auf. Berechnungen des Coulombanteils zur Gitterenergie unterstützen eine Ladungsverteilung in den M3O12-Baugruppen von (5+/4+/5+). Ba2+ -Ionen besetzen drei Punktalgen mit jeweils unterschiedlicher Koordination. Der Zusammenhang mit anderen Strukturen wird diskutiert.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926090311
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  • 187
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    Crystal and magnetic structures of the layer Compound TlMnF4 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 71-76 
    Details
    ISSN: 0044-2313
    Keywords: Thallium tetrafluoromanganate(III), TlMnF4 ; crystal structure ; magnetic structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kristall- und magnetische Struktur von TlMnF4, einer Verbindung mit SchichtstrukturDie Kristallstruktur und die magnetischen Eigenschaften des Fluoromanganates(III) TlMnF4 wurden untersucht. Die Struktur wurde in der monoklinen Raumgruppe I2/a, Elementarzelle mit a = 539,7(2); b = 544,1(2); c = 1248,4(5) pm, β = 90,19(3)° (Z = 4) auf R/wR 0,057/0,043 verfeinert. TlMnF4 zeigt eine Schichtstruktur, die durch Eckenverknüpfung von MnF6-Oktaedern über ihre vier äquatorialen Ecken gebildet wird. Die Mn—F-Abstände innerhalb des Oktaeders liegen im Bereich von 178 bis 215 pm. Die magnetische Austauschenergie (J/K) innerhalb der Schicht wurde durch Anpassung der experimentellen Suszeptibilitätsdaten im Temperaturbereich von 10-300 K auf der Basis des Heisenbergmodells für quadratische Schichten zu -0,45 K bestimmt. Dreidimensionale antiferromagnetische Ordnung tritt bei 4,2(5) K ein. Die magnetische Zelle entspricht der kristallographischen, jedoch mit primitivem Translationsgitter. Die magnetische Struktur wurde auf R = 0,058 in der magnetischen Raumgruppen P2′/a′ verfeinert. Die magnetischen Momente an MnIII sind colinear zur b-Achse und zeigen antiparallele Ordnung innerhalb der Schichten.
    Notes: The crystal structure and the magnetic properties of the fluoromanganate(III) TlMnF4 have been investigated. The structure has been refined down to R/wR of 0.057/0.043 in the monoclinic I2/a space group with the unit cell constants a = 539.7(2) pm; b = 544.1(2) pm; c = 1248.4(5) pm; β = 90.19(3)° (Z = 4). TlMnF4 is characterized by a layer structure formed of MnF6 octahedra sharing their four equatorial corners. Within each octahedron the Mn—F distances range from 178 pm to 215 pm. The intralayer magnetic interaction (J/K) has been evaluated to be approximately -0.45 K by fitting the experimental susceptibility in the 10-300 K range using the quadratic layer Heisenberg model. A 3 D-antiferromagnetic ordering occurs at Tn = 4.2(5) K. The magnetic cell corresponding to the nuclear one but with a primitive symmetry. The magnetic structure has been refined down to R = 0.0528 in the P2′/a′ magnetic group. The MnIII moments are colinear to the b-axis and show antiparallel ordering within the layers.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926090314
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  • 188
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    Über Perrhenate. 3über Perrhenate. 2  -  siehe [4]. Zum Aufbau des Mesoperrhenates Na3[ReO5]Herrn Dr. Werner Hanke zum 60. Geburtstage am 14. April 1992 gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 7-14 
    Details
    ISSN: 0044-2313
    Keywords: Na3ReO5 ; crystal structure ; ReO5 groups ; Na3Re frame analogous to Li3Bi type ; MAPLE of perrhenates ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: About Perrhenates. 3 On the Structure of the Mesoperrhenate Na3[ReO5]By tempering powder samples (prepared from mixtures of binary oxides: Na2O2/ReO2 and Na2O/ReO3 respectively, Na : Re = 3 : 1, Ar and O2 atmosphere respectively, 400-450°C, corundum boat) in a closed Ag cylinder (500-550°C, 10 d) yellow single crystals of Na3ReO5, sensitive to moisture, were grown. The compound crystallizes trigonal, space group P31, P32 respectively, with a = 5.544(1), c = 13.580(7) Å, Z = 3, drö. = 4.62 g/cm3. The crystal structure [4-circle diffractometer data, 1091 I0(hkl), AgKα, R = 6.14, Rw = 6.08%] is characterized by “isolated” bipyramids ReO5. Na+ ions are occupying all the tetrahedral (Na2, Na3) and octahedral (Na1) holes of the pseudocubic face centred (c/a = 2.441) Re part of the lattice; resulting in a Na3Re kation framework corresponding to the Li3Bi type of structure. Effective Coordination Numbers (ECoN), the Madelung Part of Lattice energy (MAPLE) and the charge distribution (CHARDI) are computed and discussed.
    Notes: Durch Tempern von Pulverproben (erhalten aus Gemengen binärer Oxide: Na2O2/ReO2 bzw. Na2/ReO3, Na : Re = 3 : 1, Ar- bzw. O2-Atmosphäre, 400-450°C, Korundschiffchen) in verschlossenen Ag-Bomben (500-550°C, 10 d) wurden feuchtigkeitsempfindliche, gelbe Einkristalle von Na3ReO5 gezüchtet, die trigonal, Raumgruppe P31 bzw. P32, mit a = 5,544(1), c = 13,580(7) Å, Z = 3, drö. = 4,62 g/cm3 kristallisieren. Die Kristallstruktur [4-Kreisdiffraktometerdaten, 1091 I0(hkl), AgKα, R = 6,14, Rw= 6,08%] zeigt “isolierte” Bipyramiden ReO5.Na+ besetzt Tetraeder-(Na2, Na3) und Oktaeder-(Na1) Lücken des pseudokubisch-flächenzentrierten (c/a = 2,449) Re-Teilgitters; das Na3Re-Kationengerüst entspricht somit dem Li3Bi-Typ. Effektive Koordinationszahlen (ECoN), der Madelunganteil der Gitterenergie (MAPLE) sowie die Ladungsverteilung (CHARDI) werden berechnet und diskutiert.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926100102
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  • 189
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    Synthese, Kristallstruktur und thermischer Abbau von Cs1,5[Re3I3Cl7,5(H2O)1,5] (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 15-19 
    Details
    ISSN: 0044-2313
    Keywords: Mixed ternary ReIII-halides ; synthesis ; crystal structure ; infrared spectroscopy ; thermal behaviour ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Crystal Structure and Thermal Behaviour of Cs1,5[Re3I3Cl7,5(H2O)1,5]Dark brown tetrahedra of Cs1,5[Re3I3Cl7,5(H2O)1,5] crystallize on slow cooling of a hot saturated solution of ReI3 and CsCl in conc. hydrochlorid acid. The crystal structure (cubic, P43m (No. 215), a = 1241.06(3)pm, Vm = 287.8(1) cm3mol-1, Z = 4, R = 0.067, Rw = 0.037) is built up from isolated building units [Re3I3Cl7,5(H2O)1,5]1,5- with statistical distribution of chloride ions and water molecules in the in plane, terminal positions. Consistent with the result based on the X-ray analysis, the IR-spectrum shows one band for the OH stretching frequencies of the water molecules coordinated to the Re3 triangle at 3240 cm-1. The anions are arranged in the fashion of a cubic closest packing with the cesium ions occupying all octahedral and one quarter of the tetrahedral interstices. Temperature-dependent Guinier-Simon photographs in connection with DTA/TG investigations reveal that Cs1,5[Re3I3Cl7,5(H2O)1,5] releases water at 190°C accompanied with a structural transition and the dehydration product decomposes at 370°C to Cs2ReCl6-xIx, Re3I3+yCl6-y and rhenium metal.
    Notes: Tiefdunkelbraune Tetraeder von Cs1,5[Re3I3Cl7,5(H2O)1,5] Kristallisieren beim langsamen Eindunsten einer heißen, gesättigten Lösung von ReI3 und CsCl in konz. Salzsäure. In der Kristallstruktur (kubisch, P43m (Nr. 215), a = 1241,06(3) pm, Vm = 287,8(1) cm3mol-1, Z = 4, R = 0,067, Rw = 0,037) sind isolierte Baugruppen [Re3I3Cl7,5(H2O)1,5]1,5- mit statistischer Verteilung von Chlorid-Ionen und Wassermolekülen in den in plane, terminal-Positionen strukturbestimmend. übereinstimmend mit diesem röntgenographischen Befund beobachtet man im IR-Spektrum eine Bande für die Valenzschwingungen des Koordinationswassers bei 3240 cm-1. Die Anionen sind nach dem Motiv einer kubisch-dichtesten Packung angeordnet, die Caesium-Ionen besetzen in ihr sämtliche Oktaeder- und ein Viertel der Tetraederlücken. Heiz-Guinier-Simon-Aufnahmen und DTA/TG-Untersuchungen zeigen, daß Cs1,5[Re3I3Cl7,5(H2O)1,5] bei 190°C zunächst Koordinationswasser unter Änderung der Struktur abgibt und sich bei 370°C zu Cs2ReCl6-xIx, Re3I3+yCl6-y und Rhenium zersetzt.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926100103
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  • 190
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    A4N2O5 (A = Na, K), neue Oxidnitrite der Alkalimetalle und eine Bemerkung zum quasi-binären System K3NO3/K3OBr (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 28-32 
    Details
    ISSN: 0044-2313
    Keywords: Alkali metal oxide nitrites ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A4N2O5 (A = Na, K) Novel Alkali Metal Oxide Nitrites, and a Comment on the System K3NO3/K3OBrK4N2O5 and Na4N2O5 have been prepared for the first time: the respective alkali metal nitrites and -oxides in molar ratios 2 : 1 have been reacted in the solid state. Their crystal structure (for crystallographic data see „Inhaltsübersicht“) derive from the anti-K2NiF4 type of structure. Na4N2O5 undergoes two phase transitions (at -15°C and -60°C) upon cooling.The behavior of solid solutions in the system K3NO3/K3OBr at cooling gives support for the phase transition being driven by the OK3-framework, where as in Na3NO3 order-disorder transitions of the NO2- group seem to induce the phase transitions.
    Notes: K4N2O5 und Na4N2O5 wurden erstmals erhalten durch Festkörperreaktionen der entsprechenden Alkalimetallnitrite und Alkalimetalloxide im Mol-Verhältnis 2 : 1. Die Kristallstrukturen (K4N2O5: I4/m; a = 520,4(2), c = 1592,6(8) pm; 150 Reflexe; R = 0,035. Na4N2O5: Pulverdaten; a = 457,2(1), 903,5(1), 1495,3(3) pm; orthorhombisch) leiten sich von dem anti- K2NiF4-Typ ab. Na4N2O5 durchläuft zwei Phasentransformationen bei -15°C und -60°C.Das Tieftemperaturverhalten der Mischkristalle im quasibinären System K3NO3/K3OBr (vollständige Mischbarkeit) stützt die Auffassung, daß die Phasenumwandlung durch das OK3-Gerüst getrieben wird, während dafür in Na3NO3 Ordnungs-Unordnungsübergänge der NO2--Anionen verantwortlich sind.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926100106
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  • 191
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    Quecksilberverbindungen mit Cyancarbanionen. II. Synthese und Kristallstruktur von Diquecksilber(I)-bis(1,1,3,3-tetracyanpropenid) (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 46-50 
    Details
    ISSN: 0044-2313
    Keywords: Mercury compounds ; dimercury(I)-bis-(1,1,3,3-tetracyanpropenide) ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Mercury Compounds with Cyancarbanions. II Synthesis and Crystal Structure of Dimercury(I)-bis(1,1,3,3-tetracyanpropenide)The structure of dimercury(I)-bis(1,1,3,3-tetracyanpropenide), Hg2(tcp)2, has been determined by single-crystal X-ray diffraction methods. The crystals are monoclinic, space group P 21/n. The unit cell dimensions are: a = 9.9193(3) Å, b = 5.6912(6) Å, c = 13.3806(4), β = 92.544(4)° and Z = 2. The mercury atoms in the centrosymmetric cation are three-coordinate with Hg—Hg 2.503, Hg—N 2.207, 2.207, 2.560 Å. tcp behaves as a bidentate ligand forming infinite chains running parallel to the a-axis.
    Notes: Die Struktur von Diquecksilber(I)-bis(1,1,3, 3-tetracyanpropenid), Hg2(tcp)2, wurde durch Einkristall-Röntgenstrukturanalyse ermittelt. Die Kristalle sind monoklin, Raumgruppe P 21/n. Die Zelldimensionen sind a = 9,9193(3) Å, b = 5,6912(6) Å, c = 13,3806(4) Å, β = 92,544(4)° und Z = 2. Die Quecksilberatome im zentrosymmetrischen Kation werden dreifach koordiniert mit Hg—Hg 2,503; Hg—N 2,207; 2,560 Å. tcp fungiert als zweizähniger Ligand unter Ausbildung unendlicher Ketten parallel zur a-Achse.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926100108
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  • 192
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    Verfeinerung der Kristallstruktur von K2O2 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 64-66 
    Details
    ISSN: 0044-2313
    Keywords: Dipotassium peroxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Refinement of the Crystal Structure of K2O2The crystal structure of K2O2 has been refined using 241 diffractometer data (Cmca; a = 6.733(1), b = 6.996(1), c = 6.474(1) Å; Z = 4; Rw = 0.050). The distance O—O (1.541(6) Å) is significantly larger than that one assumed for alkali metal peroxides, so far.
    Notes: Die Kristallstruktur von K2O2 wurde auf der Basis von Vierkreisdiffraktometerdaten (241 unabhängige Strukturfaktoren) verfeinert (Cmca; a = 6,733(1), b = 6,996(1), c = 6,474(1) Å; Z = 4; Rw = 0.050). Der gefundene O—O-Abstand weist mit 1,541(6) Å einen deutlich größeren Wert auf als bisher für die Alkalimetallperoxide angenommen.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926100111
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  • 193
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    Copper Weberites: Crystal Structure and Magnetic Investigation of Na2CuGaF7 and Na2CuInF7 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 67-74 
    Details
    ISSN: 0044-2313
    Keywords: Copper weberites, Na2CuGaF7, Na2CuInF7 ; crystal structure ; magnetic investigation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kupferweberite: Kristallstruktur und magnetische Untersuchung von Na2CuGaF7 und Na2CuInF7Die Kristallstruktur von zwei neuen Kupferweberiten Na2CuGaF7 und Na2CuInF7 wurde bestimmt. Na2CuGaF7: monokline Raumgruppe C2/c; a = 1232,5(5), b = 731,8(1), c = 1278,0(5) pm, β = 109,29(2)°, Z = 8. Na2CuInF7: orthorhombische Raumgruppe Pmnb; a = 731,8(1) pm, b = 1060,2(2) pm, c = 771,2(1) pm Z = 4. Die Strukturen wurden verfeinert mit 1175 Reflexen bis zu R = 0,043 (wR = 0,035) für Na2CuGaF7 und mit 1917 Reflexen bis zu R = 0,034 (wR = 0,025) für Na2CuInF7. Die Strukturen bestehen aus [CuF5]n3n--Ketten, die im Na2CuInF7 parallel zur a-Achse orientiert sind und in zwei alternierenden Richtungen im Na2CuGaF7. Die Natriumatome besitzen entweder siebenfache oder achtfache Koordination. Obwohl starke antiferromagnetische Wechselwirkungen innerhalb der Ketten beobachtet werden, gibt es keine Hinweise auf eine dreidimensionale Ordnung.
    Notes: The crystal structures of two new copper weberites Na2CuGaF7 and Na2CuInF7 have been determined. Na2CuGaF7 has the monoclinic space group C2/c: a = 1232.5(5) pm, b = 731.8(1) pm, c = 1278.0(5) pm, β = 109.29(2)° and Z = 8. Na2CuInF7 crystallizes in the orthorhombic space group Pmnb: a = 731.8(1) pm, b = 1060.2(2) pm, c = 771.2(1) pm and Z = 4. The structures have been refined from 1175 reflections to R = 0.043 (wR = 0.035) for Na2CuGaF7, and from 1917 reflections to R = 0.034 (wR = 0.025) for Na2CuInF7. The structures consist of [CuF5]n3n- chains which are parallel the a-axis in Na2CuInF7 and oriented in two alternating directions in Na2CuGaF7. Sodium atoms exhibit either seven-fold or eight-fold coordination. Although strong antiferromagnetic interactions are observed inside the chains, there is no evidence for three-dimensional ordering.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926100112
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  • 194
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    Quecksilberverbindungen mit Cyancarbanionen. I. Synthese und Kristallstruktur von Diquecksilber(I)-bis(tricyanmethanid)Herrn Professor Wolfgang Beck zum 60. Geburtstage am 5. Mai 1992 gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 29-34 
    Details
    ISSN: 0044-2313
    Keywords: Mercury compounds ; dimercury(I)-bis(tricyanmethanide) ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Mercury Compounds with Cyancarbanions. I . Synthesis and Crystal Structure of Dimercury(I)-bis(tricyanmethanide)With the triclinic unit cell, space group P1, with the lattice constants a = 5.2794(1) Å, b = 9.9279(1) Å, c = 11.3376(2) Å, α = 71.004(4)°, β = 76.459(2)° and γ = 74.601(4)° are two formula units. The three-dimensional network, which characterizes the structure, results from dimercury(I) ions with sp3 hybridization, which form beside the homonuclear metal bonding three covalent bonds to cyanonitrogen atoms. The tricyanmethanide ion acts by losing symmetry as a tridentate ligand.
    Notes: Innerhalb der triklinen Elementarzelle, Raumgruppe P1, mit den Gitterkonstanten a = 5,2794(1) Å, b = 9,9279(1) Å, c = 11,3376(2) Å, α = 71,004(4)° und β = 74,601(4)° befinden sich zwei Formeleinheiten. Das den Strukturaufbau charakterisierende dreidimensionale Netzwerk resultiert aus sp3-hybridisierten Diquecksilber(I)-ionen, die neben der homonuklearen Metallbindung drei weitere kovalente Bindungen zu Cyanstickstoffatomen ausbilden. Das Tricyanmethanidion wirkt unter Symmetrieverlust als dreizähniger Ligand.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926090305
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  • 195
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    Darstellung und NMR-spektroskopische Untersuchungen der tert-Butylimino-cyclopentadienylvanadium (V)-Verbindungen tC4H9N=VCpX2 (X=SR, SeC6H5, Br, I)Herrn Professor Paul Binger zum 60. Geburtstage gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 45-50 
    Details
    ISSN: 0044-2313
    Keywords: Thiolato ; selenolato ; bromo ; iodo complexes of vanadium(V) ; 1H, 51V NMR ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and NMR Spectroscopic Studies of tert-Butylimino-cyclopentadienylvanadium(V) Compounds tC4H9N=VCpX2 (X=SR, SeC6H5, Br, I)Syntheses of the cyclopentadienylvanadium(V) compounds tC4H9N=VCpX2 (X=SR, SeC6H5, Br, I) tC4H9N=VCp (StC4H9) and tC4H9N=VCp[S—(CH2)3—S] (4) are described starting from tC4H9N=VCpCl2. tC4H9N=VCl3 reacts with BBr3 and BI3 by halogen exchange forming the trihalogenides tC4H9N=VX3 (X=Br, I). All compounds obtained are characterized by 1H and 51V NMR spectroscopy. 4 has been found by X-ray diffraction analysis to be a distorted tetrahedral vanadium complex with a chair conformation of the VS2C3-ring.
    Notes: Die Darstellung der Cyclopentadienyl-vanadium(V)-Verbindungen tC4H9N=VCpX2 (X=SR, SeC6H5, Br, I), tC4H9N=VCp(StC4H9) und tC4H9N=VCp[s—(CH2)3—S] (4) wird beschrieben; als Ausgangsverbindung wird tC4H9N=VCpCI2 eingesetzt. tC4H9N=VCl3 reagiert mit BBr3 und Bl3 unter Halogenaustausch und Bildung der Trihalogenide tC4H9N=VX3 (X=Br, I). Alle dargestellten Verbindungen werden 1H- und 51V-NMR-spektroskopisch charakterisiert. Die Röntgenstrukturanalyse von 4 zeigt das Vanadiumatom in einer verzerrt tetraedrischen Anordnung der Liganden; der VS2C3-Ring liegt in der Sesselkonformation vor.
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    URL: http://dx.doi.org/10.1002/zaac.19926090308
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    Zur Reaktion von Makrozyklen mit Lanthanoiden. I. Die Struktur von [Li(thf)][(C22H22N4)2Ce] · THF (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 77-80 
    Details
    ISSN: 0044-2313
    Keywords: CeIII double decker complex ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Reaction of Macrocycles with Lanthanoids. I. The Crystal Structure of [Li(thf)][(C22H22N4)2Ce] · THFIn THF CeBr3 forms with [(TMTAA)Li2] the paramagnetic doubledecker complex [Li(thf)][(TMTAA)2Ce]. The complex crystallizes with 1 Mol THF per formula unit. The structure was characterized by X-ray single crystal structure analysis (space group C2 (No. 5), z = 6, a = 1741.8(2) pm, b = 1622.1(2) pm, c = 2540.4(3) pm, β = 104.72(1)°). The sandwich-like arrangement of the heterocyclic ligands leads to a quadratic-prismatic coordination of the Ce3+ ion. One macrocyclic ligand is additionally coordinated by a [Li(thf)]+ fragment. The coordination of the Li ion is square pyramidal.
    Notes: CeBr3 reagiert mit [(TMTAA)Li2] in THF zu dem paramagnetischen Doppeldeckerkomplex [Li(thf)][(TMTAA)2Ce], der mit 1 Mol THF pro Formeleinheit kristallisiert. Der Aufbau konnte durch eine Kristallstrukturanalyse aufgeklärt werden (Raumgruppe C2 (Nr. 5), Z = 6, a = 1741,8(2) pm, b = 1622,1(2) pm, c = 2540,4(3) pm, β = 104,72(1)°). Durch die sandwichartige Anordnung der TMTAA-Liganden erhält das Ce3+-Ion eine quadratisch-prismatische Koordination. An einen der makrozyklischen Liganden koordiniert zusätzlich ein [Li(thf)]+-Fragment. Das Li-Ion besitzt tetragonal-pyramidale Umgebung.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926150915
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    Zur Reaktion von Makrozyklen mit Lanthanoiden. II. Die Strukturen von [K(thf)3]2[(C22H28N4)2Sm2] · 4THF und [(C22H22N4)Co] · DME (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 81-85 
    Details
    ISSN: 0044-2313
    Keywords: SmIII polynuclear complex ; CoII complex ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Reaction of Macrocycles with Lanthanoids. II. The Crystal Structures of [K(thf)3]2[(C22H28N4)2Sm2] · 4 THF and [(C22H22N4)Co] · DMEIn a complicated redox reaction [(TMTAA)K2] and [SmI2(thf)2] form the polynuclear metal complex [K(thf)3]2[(TMTAT)2Sm2]. This complex crystallizes with four molecules THF per formula unit and its structure was determined by single crystal X-ray investigation (spacegroup P21/c (No. 14), z = 4, a = 998.0(2) pm, = b = 2618.3(6) pm, c = 1619.4(3) pm, β = 96.52(2)°). In the dimeric unit [(TMTAT)2Sm2]2- the Sm3+ ions are bonded to the four N atoms of the macrocyclic ligand and one C6H4 ring of the second ligand is attached η6 like to one metal ion. Additionally two [K(thf)3]+ fragments are bonded to this central unit, and therefor coordination number seven results for the K+ ion. [TMTAA]2- is not reduced by [Cp2Co] in a similar reaction. The monomeric paramagnetic complex [(TMTAA)Co] (μeff = 2,76 μB) is formed instead. The structure reveils a square planar coordination of the Co atom by the four N atoms of the TMTAA ligand (spacegroup C2/c (No. 15), z = 4, a = 1945.1(4) pm, b = 1165.6(2) pm, c = 1144.7(2) pm, β = 116.38(1)°).
    Notes: [(TMTAA)K2] und [SmI2(thf)2] reagieren in einer unübersichtlichen Redoxreaktion zu dem mehrkernigen Metallkomplex [K(thf)3]2[(TMTAT)2Sm2]. Der Aufbau dieser mit vier Molekülen THF pro Formeleinheit kristallisierenden Verbindung konnte durch eine Röntgenstrukturanalyse aufgeklärt werden (Raumgruppe P21/c (Nr. 14), Z = 4, a = 998,0(2) pm, b = 2618,3(6) pm, c = 1619,4(3) pm, β = 96,52(2)°). In der dimeren Einheit [(TMTAT)2Sm2]2- sind die Sm3+-Ionen außer an die vier N-Atome eines makrozyklischen Liganden auch η6-artig an einen C6H4-Ring des zweiten Liganden gebunden. Zusätzlich koordinieren an die zentrale Einheit zwei [K(thf)3]+-Fragmente. Dies führt zu einer Koordinationszahl von 7 für das K+-Ion. [TMTAA]2- wird in einer analogen Reaktion mit [Cp2Co] nicht reduziert. Statt dessen bildet sich der monomere paramagnetische Komplex [(TMTAA)Co] (μeff = 2,76 μB). Nach der Kristallstrukturanalyse ist das Co-Atom quadratisch planar von den vier N-Atomen des TMTAA-Liganden koordiniert (Raumgruppe C2/c (Nr. 15), Z = 4, a = 1945,1(4) pm, b = 1165,6(2) pm, c = 1144,7(2) pm, β = 116,38(1)°).
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926150916
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    Cadmium iodide complexes with dimethylsulphoxide, and their crystal structures (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 143-148 
    Details
    ISSN: 0044-2313
    Keywords: Cadmium iodide dimethylsulfoxide complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cadmiumiodid-Komplexe mit Dimethylsulfoxid und ihre KristallstrukturenEinkristalldaten der Verbindungen [{CdI2(dmso)}n] (1,) und [Cd2I4(dmso)4] (2,) zeigen, daß mit steigendem Anteil von dmso Übergang zu ionischen Species wie [Cd(dmso)6]2+ [Cd(dmso)I3]2- · EtOH (3,) und [Cd(dmso)6]2+ [CdI4]2- (4,) erfolgt. Bei (1,) liegen polymere Ketten mit Cd2+ der CN 4 bzw. 6 vor, wobei I- überbrückt. Die Ketten von (2,) weisen ein bi-nukleares Segment auf und sind als Vorläufer der typisch ionischen Stoffe (3,) bzw. (4,) aufzufassen. Wegen der lockeren Packung der konstituierenden Ionen in (3,) ist Ethanol eingebaut.
    Notes: The crystalline compounds [{CdI2(dmso)}n] (1,) and [Cd2I4(dmso)4] (2,) provide a structural sequence illustrating the conversion of CdI2 into the ionic derivatives [Cd(dmso)6]2+ [Cd(dmso)I3]2- · EtOH (3,) and [Cd(dmso)6]2+ CdI42- (4,), with increasing proportions of dmso. (1,) comprises polymeric chains with Cd centres linked by bridging iodide atoms, and alternately in four- and six-coordination. (2,) is a binuclear segment of the chains and can be seen as the structural forerunner of the ionic compounds (3,) and (4,). The ion packing in (3,) is loose, with lattice ethanol.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926150929
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    Untersuchungen über Zinn(IV)-alkoxide. II. Isolierung und Charakterisierung der Verbindung Sn3O(OiBu)10 · 2i-BuOH. Das erste Beispiel für ein partielles Hydrolyseprodukt eines Zinn(IV)-alkoxids (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 137-142 
    Details
    ISSN: 0044-2313
    Keywords: Tin(IV) alkoxides ; partially hydrolized tin(IV) alkoxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Investigations into Tin(IV) Alkoxides. II. Isolation and Characterization of the Compound Sn3O(OiBu)1010 · 2i-BuOH. The First Example of a Partially Hydrolized Tin(IV) AlkoxideThe partial hydrolysis product Sn3O(OiBu)10 · 2i-BuOH was obtained by slow hydrolysis of the reaction product of tin tetrachloride with sodium isobutoxide. The compound forms colourless, moisture sensitive crystals, which easily release the coordinated solvent molecules in dry air. Its crystal and molecular structure has been determinated by single crystal X-ray diffraction. The compound crystallizes in the triclinic space group P1 with a = 1363.5(7), b = 1462.7(10), c = 1637.7(7) pm, α = 95.40(5)°, β = 96.79(4)°, γ = 102.12(5)° and Z = 2. The crystal structure consists of discrete, trimeric molecules with octahedrally coordinated tin atoms which are connected to each other corresponding to the formulation Sn3(μ3-O)(μ2-OiBu)3(O1Bu)7 · (i-BuOH)2 by three isobutoxide groups bridging two metal atoms and a single threefold bridging oxygen atom
    Notes: Das partielle Hydrolyseprodukt Sn3O(OiBu)10 · 2i-BuOH des Zinn(IV)-isobutanolats wurde bei der schonenden Hydrolyse des Reaktionsproduktes von Zinntetrachlorid mit Natriumisobutanolat erhalten. Die Verbindung bildet farblose, feuchtigkeitsempfindliche Kristalle, die in trockener Luft unter Abspaltung der Lösungsmittelmoleküle rasch verwittern. Die Kristall- und Molekülstruktur wurde durch Röntgenstrahlbeugung an einem Einkristall bestimmt. Die Verbindung kristallisiert in der triklinen Raumgruppe P1 mit den Gitterkonstanten a = 1363,5(7), b = 1462,7(10), c = 1637,7(7) pm, α = 95,40(5)°, β = 96,79(4)°, γ = 102,12(5)° und Z = 2. Die Kristallstruktur besteht aus diskreten, trimeren Molekülen, in denen die oktaedrisch koordinierten Zinnatome entsprechend der Formulierung Sn3(μ3-O)(μ2-OiBu)3(OiBu)7(i-BuOH)2 über drei, je zwei Metallatome verbrückende Isobutanolat-Gruppen und ein einzelnes dreifach verbrückendes Sauerstoffatom miteinander verbunden sind.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926150928
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    Darstellung, Struktur und magnetische Eigenschaften der Natriumeisenchalkogenide Na6FeS4 und Na6FeSe4Professor Rudolf Hoppe zum 70. Geburtstage gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 616 (1992), S. 14-18 
    Details
    ISSN: 0044-2313
    Keywords: Sodium iron chalcogenides, Na6FeS4, Na6FeSe4 ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Structure, and Magnetic Properties of the Sodium Iron Chalcogenides Na6FeS4 and Na6FeSe4The compounds Na6FeS4 and Na6FeSe4 have been synthesized by fusion reactions of sodium carbonate with iron and chalcogen in a stream of hydrogen.Structural investigations on single crystals show that both compounds crystallize in an atomic arrangement isotypic with Na6ZnO4 (space group P63mc). The structure is characterized by isolated [FeX4]-tetrahedra.The magnetic susceptibilities show Curie-Weiss behaviour. The deviations at low temperatures are obviously caused by antiferromagnetic interactions.
    Notes: Durch Schmelzreaktionen von Natriumcarbonat mit Eisen und Chalkogen im Wasserstoffstrom gelang die Darstellung von Na6FeS4 und Na6FeSe4.Röntgenstrukturuntersuchungen an Einkristallen ergaben daß die beiden Verbindungen isotyp kristallisieren. Die Atomanordnung entspricht der des Na6ZnO4 (Raumgruppe P63mc). Als charakteristische Baueinheit treten isolierte [FeX4]6--Tetraeder auf.Die Temperaturabhängigkeiten der magnetischen Suszeptibilitäten lassen sich mit einem Curie-Weiss-Verhalten beschreiben. Bei tiefen Temperaturen treten Abweichungen von diesem Verhalten auf, die offensichtlich auf antiferromagnetische Wechselwirkungen zurückzuführen sind.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926161003
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