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  • 1992  (15)
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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 2025-2026 
    ISSN: 0009-2940
    Keywords: Aza-nido-decaborane(12) ; (1H-Triazen-1,3-diyl)-aza-arachno-decaborane(13) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1,3-Addition of Azides to Azadecaborane: 6-Azadecaborane-4,9-diyltriazenesnido-NB9H12 (1) reacts with azides RN3 to form a coordinative B-N bond between B9 and N1 of RN3, accompanied by the α-addition of the B4-H bond of 1 to the N3 atom of RN3. The products 2a, b (R = H, CH2Ph, respectively) thus contain an azadecaborane skeleton and a five-membered unsaturated B2N3 ring with a common B-B edge. The product 2a crystallizes in the space group Pna21.
    Additional Material: 1 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 761-766 
    ISSN: 0009-2940
    Keywords: Tellurium compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Cleavage of Bulky Diaryl Ditellurides with Bromine and Iodine; Crystal Structure of Et4N+ 2,4,6-(i-C3H7)3C6H2TeI-2Bis(2,4,6-triisopropylphenyl) ditelluride (1a), obtained from 2,4,6-triisopropylphenylmagnesium bromide with tellurium followed by oxidation with oxygen, and bis(2,4,6-tri-tert-butylphenyl) ditelluride (1b) react with equimolar amounts of bromine and iodine to provide new monomeric arenetellurenyl halides 2,4,6-R3C6H2TeX (2a, b, 3a, b: R = i-C3H7, t-C4H9; X = Br, I). Both tellurenyl iodides are thermally more stable than the corresponding bromides. Green 2,4,6-(i-C3H7)3C6H2TeI (3a) reacts with Et4N+I- to give the stable, red adduct Et4N+ 2,4,6-(i-C3H7)3C6H2TeI-2 (4a). An X-ray crystal structure determination of 4a revealed a T-shaped structure of the hypervalent aryldiiodotellurate(II) anion. Iodide-ion transfer between aryldiiodotellurate(II) and arenetellurenyl iodide is a fast process (1H-NMR time scale). 125Te-NMR data of this anion and of tellurenyl halides are compared with those of the ditellurides and of lithium benzenetellurolates (LiTeR·(THF)x).
    Additional Material: 3 Ill.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 607 (1992), S. 91-95 
    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.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 16-18 
    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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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 616 (1992), S. 141-144 
    ISSN: 0044-2313
    Keywords: Crystal structure ; Synthesis ; Thermolysis, Lanthanides ; Ternary ammonium nitrates ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Structure, and Thermolysis of the (NH4)3[M2(NO3)9] (M = La—Gd)The ternary ammonium nitrates (NH4)3[M2(NO3)9] (M = La-Gd) are obtained as single crystals from a solution of the respective sesquioxides in a melt of NH4NO3 and sublimation of the excess NH4NO3. In the crystal structure of (NH4)3[Pr2(NO3)9] (cubic, P4332, Z = 4, a = 1 377.0(1) pm, R = 0.038, Rw = 0.023) Pr3+ is surrounded by six bidentate nitrate ligands of which three are bridging to neighbouring Pr3+ ions. This results in a branched folded chain, held together by the NH4+ ions which occupy cavities in the structure. (NH4)3[Pr2(NO3)9] is the first intermediate product of the thermal decomposition of (NH4)2[Pr(NO3)5(H2O)2] · 2H2O.
    Notes: Die ternären Ammoniumnitrate (NH4)3[M2(NO3)9] (M = La—Gd) erhält man in Form von Einkristallen durch Auflösen der entsprechenden Sesquioxide in einer Schmelze von NH4NO3 und Entfernen des Überschusses durch Sublimation. Die Strukturanalyse am Beispiel von (NH4)3[Pr2(NO3)9] (kubisch, P4332, Z = 4; a = 1377,0(1) pm; R = 0,038; Rw = 0,023) zeigt, daß Pr3+ von sechs zweizähnigen Nitratliganden umgeben ist, von denen drei jeweils zu einem weiteren Pr3+-Ion verbrücken. Dadurch entsteht eine verzweigte, gefaltete Kette. Sie wird durch NH4+-Ionen zusammengehalten, die sich in Hohlräumen befinden. (NH4)3[Pr2(NO3)9] stellt die erste Stufe beim thermischen Abbau von (NH4)2[Pr(NO3)9(H2O)2] · 2H2O dar.
    Additional Material: 4 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 20-22 
    ISSN: 0044-2313
    Keywords: Crystal structure ; lanthanides ; adducts ; complex nitrates ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cs4[La(NO3)6](NO3) · HNO3: The First Nitric Acid Adduct of a Ternary Alkali Lanthanide NitrateIn the crystal structure of Cs4[La(NO3)6](NO3). HNO3 (monoclinic, P21/c, Z = 2, a = 787.3(2); b = 1353.0(3); c = 1141.8(7) pm; β = 94,37(3)°) La3+ has a coordination number of twelve (six bidentate nitrate ligands). The structure may be viewed at as a layer structure: Layers of the composition [Cs(1)4La2(NO3)12]2-, and [Cs(2)4(NO3)2(HNO3)2]2+ are stacked alternatively in the [100] direction.
    Notes: In der Kristallstruktur von Cs4[La(NO3)6](NO3) · HNO3 (monoklin, P21/c, Z = 2, a = 787,3(2); b = 1353,0(3); c = 1141,8(7)pm; β = 94,37(3)°) hat La3+ die Koordinationszahl zwölf (sechs zweizähnige Nitratliganden). Sie kann als Schichtstruktur aufgefaßt werden: Zwischen Schichten der Zusammensetzung [Cs(1)4La2(NO3)12]2-, die längs [100] gestapelt sind, liegen Cs(2)+- und NO3--Ionen sowie HNO3-Moleküle, die ihrerseits Schichtpakete [Cs(2)4(NO3)2(HNO3)2]2+ bilden.
    Additional Material: 2 Ill.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 15-19 
    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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  • 8
    ISSN: 0044-2313
    Keywords: Heterodinuclear Cyclooctatetraene Complexes ; Synthesis ; Crystal Structure ; ESR Spectrum ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kooperative Wirkung in π-Ligand-verbrückten Zweikernkomplexen. XII. Gemischtkernige elektronenarme μ-Cyclooctatetraen-Zweikernkomplexe mit CrFe-und CrCo-KombinationenDie synfacialen gemischtkernigen μ-Cot-Zweikernkomplexe [(CpCr)(CpM)]μ-Cot (M = Fe, 3; M = Co, 4) (Cp = Cyclopentadienyl; Cot = Cyclooctatetraen) werden in thermischen Reaktionen aus der einkernigen Sandwichverbindung CpCr(n6-Cot) und CpMLn [M = Fe, Ln = Benzol (Bz); M = Co, Ln = (C2H4)2] gebildet. 3 besitzt zwei ungepaarte Elektronen, während 4 mit nur einem ungepaarten Elektron SSR-ak-tiv ist. Aufgrund der Molekülstruktur von 3 und den ESR-Daten von 4 kann gefolgert werden, daß die ungepaarten Elektronen dieser Produkte hauptsächlich auf den Cr-Zentren lokalisiert sind. Daraus ergibt sich eine enge elektronische Verwandtschaft zwischen den hetero-dinuklearen Verbindungen 3 und 4 und den einkernigen Sandwichverbindungen Chromocen beziehungsweise CpCrBz.
    Notes: The synfacial heterodinuclear μ-Cot complexes (Cot = cyclooctatetraene) [(CpCr) (CpM)]μ-Cot (Cp = cyclopentadienyl; M = Fe, 3; M = Co, 4) are formed in a thermal reaction of the mononuclear mixed sandwich compound CpCr(n6-Cot) and CpMLn [M = Fe, Ln = benzene (Bz); M = Co, Ln = (C2H4)2]. 3 possesses two unpaired electrons whereas 4 has only one unpaired electron and is ESR active. From the molecular structure of 3 and from the ESR data of 4 it can be deduced that the unpaired electrons are localized at the Cr centers predominantly forcing a close electronical relation between the heterodinuclear compounds 3 and 4 and the mononuclear sandwich complexes chromocene and CpCrBz, respectively.
    Additional Material: 7 Ill.
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 618 (1992), S. 26-29 
    ISSN: 0044-2313
    Keywords: Rhenium complexes ; synthesis ; crystal structure ; thermal behaviour ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Structure and Thermolysis of NH4[Re3Br10]NH4[Re3Br10] crystallizes as dark brown single crystals upon slow cooling of a hot, saturated hydrobromic-acid solution of [Re3Br9(H2O)2] after the addition of NH4Br. The crystal structure (monoclinic, C2/m (Nr. 12); Z = 4; a = 1461.6(7), b = 1 085.6(4), c = 1030.3(7) pm, β = 92.63(4)°, Vm = 245.9(4)cm3/mol; R = 0.097, Rw = 0.043) contains [Re3Br12]- units that share two common edges. These chains run along [010] and are held together by NH4+ ions. Each NH4+ is surrounded by eight Br- from four different chains. The first step of the thermal decomposition at 290°C is the disproportionation to ReBr3 (ReCl3 type), rhenium metal and (NH4)2[ReBr6]. Secondly, the internal reduction of (NH4)2[ReBr6] at 390°C to rhenium metal takes place.
    Notes: Aus heißer, gesättigter, bromwasserstoffsaurer Lösung von [Re3Br9(H2O)2] erhält man nach Zugabe von NH4Br beim langsamen Abkühlen dunkelbraune Einkristalle von NH4[Re3Br10]. In der Kristallstruktur (monoklin, C2/m (Nr. 12); Z = 4; a = 1 461,6(7); b = 1 085,6(4); c = 1030,3(7) pm, β = 92,63(4)°, Vm = 245,9(4) cm3/mol; R = 0,097, Rw = 0,043) erstrecken sich entlang [010] doppelt kantenverknüpfte [Re3Br12]--Baueinheiten. Diese Stränge werden durch NH4+-Ionen zusammengehalten, wobei jedes NH4+ von acht Br- aus vier unterschiedlichen Strängen umgeben ist. Der thermische Abbau erfolgt im wesentlichen in zwei Schritten: Bei 290°C entsteht durch Disproportionierung ReBr3 im ReCl3-Typ bzw. Rhenium-Metall neben (NH4)2[ReBr6], das bei 390°C durch “innere Reduktion” zu Rhenium-Metall abgebaut wird.
    Additional Material: 1 Ill.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 613 (1992), S. 149-149 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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