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  • 1
    Electronic Resource
    Electronic Resource
    [Rb2(H2O)2][Re3(μ-Cl)3Br7(H2O)2]2 · H2O, ein gemischtes Halogenid-Hydrat mit anionischen Dimeren {[Re3(μ-Cl)3Br7(H2O)2]2 · H2O}2-Professor Kurt Dehnicke zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 595 (1991), S. 131-137 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium ; rubidium rhenium halide hydrates ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Rb2(H2O)2][Re3(μ-Cl)3Br7(H2O)2]2 · H2O, a Mixed Halide-Hydrate with the Anionic Dimer {[Re3(μ-Cl)3Br7(H2O)2]2 · H2O}2-[Rb2(H2O)2][Re3(μ-Cl)3Br7(H2O)2]2 · H2O crystallizes as dark redbrown single crystals from an hydrobromic-acid solution of ReCl3 and RbBr at 0°C. An important feature of the crystal structure (monoclinic, C2/c; a = 1494.61(8); b = 835.71(4); c = 3079.96(19) pm; β = 97.801(4)°; Vm = 573.9(4) cm3mol-1; R = 0.060; Rw = 0.038) is the connection of two anions [Re3(μ-Cl)3Br7(H2O)2]- via a water molecule to dimers, {[Re3(μ-Cl)3Br7(H2O)2]2 · H2O}2-. These dimeric units are contained in slabs that are stacked in the [001] direction and held together by Rb+ cations and crystal water.
    Notes: [Rb2(H2O)2][Re3(μ-Cl)3Br7(H2O)2]2 · H2O kristallisiert in dunklen, rotbraunen Einkristallen aus bromwasserstoffsaurer Lösung von Rheniumtrichlorid und Rubidiumbromid bei 0°C. Ein wichtiges Merkmal der Kristallstruktur (monoklin; C2/c; a = 1494,61(8); b = 835,71(4); c = 3079,96(19) pm; β = 97,801(4)°; Vm = 573,9(4) cm3mol-1; R = 0,060; Rw = 0,038) ist die Verknüpfung zweier Anionen [Re3(μ-Cl)3Br7(H2O)2]- über ein Wassermolekül zu Dimeren {[Re3(μ-Cl)3Br7(H2O)2]2 · H2O}2-. Diese dimeren Baugruppen sind zu Schichtpaketen zusammengefaßt, die längs [001] gestapelt und über die Rb+-Ionen in Gemeinsamkeit mit Kristallwasser verbunden sind.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19915950113
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  • 2
    Electronic Resource
    Electronic Resource
    Kristallstruktur von (NMe4)2[Re3Br11(H2O)] [Re3Br9(H2O)3](H2O)2 (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1655-1660 
    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: Crystal Structure of (NMe4)2[Re3Br11(H2O)] [Re3Br9(H2O)3](H2O)2.(NMe4)2[Re3Br11(H2O)] [Re3Br9(H2O)3](H2O)2 crystallizes from hydrobromic acid solution of Re3Br9 · 2 H2O and NMe4Br at 0 - 5°C. The crystal structure (monoclinic; P21/m (Nr. 11); a = 967.9(3); b = 1 529.7(4); c = 1 710.9(4) pm; β = 91.66(2)°; Z = 2; R = 0.113; Rw = 0.068) has been determined from four-circle diffractometer data. The structure contains two different cluster units of trivalent rhenium, isolated anionic [Re3Br11(H2O)]2- units and neutral cluster units that are connected through crystal water molecules to chains∞1{[Re3Br9(H2O)3](H2O)2}.
    Notes: (NMe4)2[Re3Br11(H2O)] [Re3Br9(H2O)3](H2O)2 kristallisiert aus einer bromwasserstoffsauren Lösung von Re3Br9 · 2 H2O und NMe4Br als dunkel-rotbraune Einkristalle bei 0 - 5°C aus. Die Kristallstruktur wurde aus Vierkreis-Diffraktometerdaten bestimmt: monoklin; P21/m (Nr. 11); a = 967,9(3); b = 1 529,7(4); c = 1 710,9(4) pm; β = 91,66(2)°; Z = 2; R = 0,113; Rw = 0,068. In der Struktur liegen zwei unterschiedliche Clustereinheiten vor: Eine anionische, isolierte Baueinheit, [Re3Br11(H2O)]2-, sowie eine neutrale über Kristallwasser zu Strängen gemäß ∞1{[Re3Br9(H2O)3](H2O)2} verknüpfte Einheit.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936191003
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  • 3
    Electronic Resource
    Electronic Resource
    (NH4)3[Re3Cl12]: Synthese, Kristallstruktur und Thermolyse (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 604 (1991), S. 7-15 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium ; crystal structure ; thermolysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: (NH4)3[Re3Cl12]: Synthesis, Crystal Structure, and Thermolysis(NH4)3[Re3Cl12] may be obtained by reaction of ReCl3 with liquid ammonia and subsequent reaction of the solid product with hydrochloric acid solution or, less pure, directly from ReCl3 and NH4Cl in hydrochloric acid. The crystal structure (monoclinic, P21/m, Z = 2, a = 946.82(6), b = 1138.37(6), c = 912.30(4)pm, β = 93.840(5)°) contains the isolated building units [Re3Cl12]3-. The anions are connected via the NH4+ cations (symbolized by N1 and N2) that have coordination numbers of 10(N1) and 9(N2). Thermal decomposition was investigated by simultaneous DSC/TG-MS measurements. It leads, finally, to metallic rhenium and the gases HCL and N2, but consists of three steps at 320, 420 and 480°C, respectively, with (NH4)2[ReCl6] and ReCl3 as intermediate products.
    Notes: Bisher unbekanntes (NH4)3[Re3Cl12] erhält man durch Behandeln von ReCl3 mit fl. NH3 und anschließender Umsetzung des Reaktionsproduktes mit Salzsäure oder, weniger rein, direkt aus ReCl3 und NH4Cl in Salzsäure. In der Kristallstruktur (monoklin, P21/m, Z = 2; a = 946,82(6); b = 1138,37(6); c = 912,30(4) pm; β = 93,840(5)°) liegen isolierte Baueinheiten [Re3Cl12]3- vor. Die Anionen werden durch die Kationen NH4+ (repräsentiert durch N1 und N2) miteinander verknüpft, sie weisen Koordinationszahlen von 10 (N1) bzw. 9 (N2) auf. Der thermische Abbau wurde mittels simultaner DSC/TG-MS untersucht. Er führt letztlich zu metallischem Rhenium und den Gasen HCl und N2 und erfolgt in drei Stufen bei 320, 420 und 480°C, wobei als Zwischenprodukte (NH4)2[ReCl6] und ReCl3 auftreten.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19916040102
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  • 4
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstrukturen der methylsubstituierten Ammonium-μ-trichlorononachloro-trirhenate(III), (NH4-xMex)3 [Re3Cl12] (1 ≤ X ≤ 3) (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 604 (1991), S. 17-26 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium ; crystal structure ; syntheses ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structures of Methyl-Substituted Ammonium-μ-trichloro-nonachloro-trirhenates(III), (NH4-xMex)3[Re3Cl12] (1 ≤ x ≤ 3)The chlorides (NH3Me)3[Re3Cl12] (1), (NH2Me2)3[Re3Cl12] (2) and (NHMe3)3[Re3Cl12] (3) are obtained from the binary components, for example (NH3Me)Cl and ReCl3, by slow evaporation of the hydrochloric-acid solutions as brick red single crystals. The crystal structures were determined from four-circle diffractometer data.1:orthorhombic, Pnma, Z = 4; a = 1667.93(9); b = 1197.01(5); c = 1110.44(5) pm; R = 0,115; Rw = 0,062.2:monoklin, P21/n, Z = 4; a = 1563,03(12); b = 1648,73(10); c = 984,34(7) pm; β = 93,422(8)°; R = 0,054; Rw = 0,035.3:monoklin, P21/n, Z = 4; a = 1651,7; b = 1679,5; c = 1014,2pm; β = 90,3°; R = 0,107; Rw = 0,075.
    Notes: Die Chloride (NH3Me)3[Re3Cl12] (1), (NH2Me2)3[Re3Cl12] (2) und (NHMe3)3 [Re3Cl12] (3) erhält man aus den binären Komponenten, z. B. (NH3Me)Cl und ReCl3, beim langsamen Eindunsten der salzsauren Lösungen als ziegelrote Einkristalle. Die Kristallstrukturen wurden aus Vierkreis-Diffraktometer-Daten bestimmt.1:orthorhombisch, Pnma, Z = 4; a = 1667,93(9); b = 1197,01(5); c = 1110,44(5)pm; R = 0,115; Rw = 0,062.2:monoklin, P21/n, Z = 4; a = 1563,03(12); b = 1648,73(10); c = 984,34(7)pm; β = 93,422(8)°; R = 0,054; Rw = 0,035.3:monoklin, P21/n, Z = 4; a = 1651,7; b = 1679,5; c = 1014,2pm; β = 90,3°; R = 0,107; Rw = 0,075.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19916040103
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  • 5
    Electronic Resource
    Electronic Resource
    (NMe4)[Re3Cl10(H2O)2] · 2H2)  -  Kein 5/3-Hydrat gemäß [Re3Cl9(H2O)3] · 2H2O (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 604 (1991), S. 27-33 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium ; crystal structure ; ir, nmr spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: (NMe4)[Re3Cl10(H2O)2] · 2H2O  -  not a 5/3-Hydrate according to [Re3Cl9(H2O)3] · 2H2ONew investigations of the so-called 5/3-hydrate, “[Re3Cl9(H2O)3] · 2H2O”, revealed that it is in fact (NMe4)[Re3Cl10(H2O)2] · 2HO. Low temperature (173 K) single crystal diffractometry confirms the main features of the previously determined crystal structure (hexagonal, P62c, No. 190; a = 937.3(2), c = 1461.2(3) pm; z = 2; Vm = 334.8 cm3/mol; R = 0.030, Rw = 0.022). There are, however, two important differences. First, the channels in the [00.1] direction contain cations NMe4+.These are disordered in a way that their orientation is “up and down” parallel to [00.1]. Infrared and solid-state 13C-NMR spectra confirm the appearance of the NMe4+ cation. Secondly, the in plane, terminal (i, t) positions at the Re3 triangle are not occupied by H2O ligands alone. Rather, the anion [Re3Cl10(H2O)2]- occurs, with statistical distribution of two water molecules (dRe—o = 224(2) pm) and one chloride ion (dRe—cl = 248(1) pm) over the three i,t positions.
    Notes: Neue Untersuchungen an dem als 5/3-Hydrat beschriebenen „[Re3Cl9(H2O)3] · 2H2O“ ergaben, daß es sich hierbei um (NMe4) [Re3Cl10(H2O)2] · 2H2O handelt. Tieftemperaturmessungen (173 K) am Einkristall bestätigen weitgehend die früher bestimmte Kristallstruktur (hexagonal. P62c, Nr. 190; a = 937,3(2), c = 1461,2(3) pm; Z = 2; Vm = 334,8 cm3/mol; R = 0,030; Rw = 0,022). Es bestehen jedoch zwei wichtige Unterschiede: In den Kanälen längs [00.1] befinden sich die Kationen NMe4+; sie sind derart fehlgeordnet, daß die Spitzen der Tetraeder in und gegen Richtung [00.1] orientiert sind. IR- und Festkörper-13C-NMR-Spektrum sind im Einklang mit der Erwartung für das Kation NMe4+. Die in plane, terminal-(i,t)-Positionen am Re3-Ring sind nicht mit drei Wassermolekülen besetzt: Es liegt vielmehr die Baugruppe [Re3Cl10(H2O)2]- vor, mit statistischer Verteilung von zwei Koordinationswasser (dRe—o = 224(2)pm) und einem Chlorid-Ion (dRe—cl = 248(1) pm) auf den drei i,t-Positionen.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19916040104
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  • 6
    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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