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  • 1
    Electronic Resource
    Electronic Resource
    The chlorides Na3MCl6 (M = Eu—Lu, Y, Sc): Synthesis, crystal structures, and thermal behaviourProfessor Albrecht Rabenau zum 65. Geburtstage am 17. November 1987 gewidmet (1987)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 554 (1987), S. 25-33 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Die Chloride Na3MCl6 (M = Eu—Lu, Y, Sc): Synthese, Kristallstrukturen, thermisches VerhaltenEinkristalle von Na3ErCl6 erhält man bei der metallothermischen Reduktion von ErCl3 mit Natrium. Die Kristallstruktur entspricht der des Minerals Kryolith mit a = 684,54(4); b = 725,18(4); c = 1012,39(6) pm; β = 90,768(5)°; Z = 2, Raumgruppe P21/n. Zwei Synthesewege zu reinen Pulverproben der Chloride Na3MCl6 (M = Eu—Lu, Y, Sc) werden beschrieben. Diese sind mit M = Dy—Lu, Y, Sc isotyp mit Na3ErCl6, während jene mit M = Eu, Gd, Tb in einer aufgefüllten Struktur von LiSbF6-Typ kristallisieren. Die Dimorphie von Na3GdCl6 und die Abhängigkeit der Gitterkonstanten und des molaren Volumens von der Temperatur wurden untersucht. Bei 205°C beobachtet man eine Phasenumwandlung erster Ordnung aus dem aufgefüllten LiSbF6-Typ (Na3GdCl6-I) in den Kryolith-Typ (Na3GdCl6-II), die von einem negativen Volumensprung (3,71%) begleitet ist.
    Notes: Single crystals of Na3ErCl6 were obtained via the metallothermic reduction of ErCl3 with Na. The crystal structure is that of the mineral cryolite with a = 684.54(4), b = 725.18(4), c = 1012.39(6) pm, β = 90.768(5)°, Z = 2, space group P21/n. Two applicable synthetic routes to pure powder samples of the chlorides Na3MCl6 (M = Eu—Lu, Y, Sc) are described. With M = Dy—Lu, Y, Sc, these are isotypic with Na3ErCl6 while those with M = Eu, Gd, Tb adopt a „stuffed“ LiSbF6-type structure. The dimorphism of Na3GdCl6 and dependence of the lattice constants and the molar volume upon temperature has been investigated: At 205°C, a first-order phase transition from the stuffed LiSbF6-type Na3GdCl6-I to the cryolite-type Na3GdCl6-II occurs exhibiting a 3.71% negative molar volume discontinuity.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19875541104
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  • 2
    Electronic Resource
    Electronic Resource
    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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  • 3
    Electronic Resource
    Electronic Resource
    Synthesis and crystal structure of tetraethylammonium-μ-trichloro-heptachloro-diaqua-trirhenate(III)-dihydrate, NEt4[Re3Cl10(H2O)2] · 2 H2OProfessor Robert Juza zum 85. Geburtstage am 8. Dezember 1989 gewidmet (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 579 (1989), S. 116-122 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese und Kristallstruktur von Tetraethylammonium-µ-trichloro-heptachloro-diaquatrirhenat(III)-dihydrat, NEt4[Re3Cl10(H2O)22] · 2 H2ONEt4[Re3Cl10(H2O)2] · 2 H2O (1) entsteht in Form von dunkelroten Einkristallen beim langsamen Eindunsten salzsaurer Lösungen von ReCl3 und Tetraethylammoniumchlorid, NEt4Cl. 1 gehört zum orthorhombischen Kristallsystem, Raumgruppe Pnma, Z = 4; a = 1838,7(2); b = 1455,9(1); c = 972,08(7) pm; Vm = 391,81(6) cm3 · mol-1. Die Kristallstruktur enthält anionische Baugruppen [Re3Cl10(H2O)2]-, die nach Art einer hexagonal-dichtesten Kugelpackung angeordnet sind. Die Anionen werden durch (fehlgeordnete) Kationen NEt4+ zusammengehalten und sind gemeinsam mit dem Kristallwasser in ein System von Wasserstoffbrücken-Bindungen eingebunden.
    Notes: NEt4[Re3Cl10(H2O)2] · 2 H2O (1) was obtained from hydrochloric acid solutions of ReCl3 and tetraethylammonium chloride, NEt4Cl, by isothermal evaporation as dark red crystals. 1 crystallizes in the orthorhombic crystal system, space group Pnma, Z = 4, with a = 1838,7(2), b = 1456.9(1), c = 972.08(7) pm, Vm = 391.81(6) cm3 · mol-l. The crystal structure consists of [Re3Cl10(H2O)2]- anions that are arranged in the fashion of a hexagonal closest-packing of spheres. These are held together by partially disordered NEt4+ cations and are bound into a hydrogen bonding system with the crystal water.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895790113
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  • 4
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    Electronic Resource
    Synthese und Kristallstrukturen von Chlororhenaten(III) mit den zweiwertigen Kationen Ethylendiammonium und Piperazinium:(EnH2)2(Pipzh2)[Re3Cl12]2· 6H2O, und (PipzH2) [Re3Cl12]CI·H2O und (Pipzh2) [Re3Cl11(H2O)]·3H2O (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 607 (1992), S. 72-78 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium ; crystal structure ; synthesis ; ethylenediammonium ; piperazinium ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structures of Chlororhenates(III) with the Divalent Cations Ethylenediammonium and Piperazinium: (EnH2)2(PipzH2) [Re3Cl12]2·6H2O, (EnH2) (PipzH2) [Re3Cl12]Cl· H2O, and (PipzH2) [Re3Cl11(H2O)] · 3H2OThe deep red salt (EnH2)2(PipzH2)[Re3CI12] · 6 H2O (1), (EnH2)(PipzH2)[Re3Cl12]CI · H2O (2), and (PipzH2)[Re3Cl11(H2O)] · 3H2O (3) crystallize upon evaporation from hydrochloride acid solutions of ReCl3 on addition of ethylenediammonium chloride (EnH2Cl2) and/or piperazinium chloride (PipzH2Cl2). The crystal structures have been determined from four-circle diffractometer data.1:monoclinic; a = 1889.63(11), b = 1615.82(8), c = 790.28(4)pm; β = 101.354(5)°; Z = 2; P21/n; R = 0.119, Rw = 0.070.2:triclinic; a = 1330.35(4), b = 1051.14(5), c = 1165.32(6)pm; α = 122.308(4), β = 102.412(3), γ = 92.226(4)°; Z = 2, P1; R = 0.092, Rw = 0.059.3:orthorhombic; a = 971.43(4), b = 1619.51(7), c = 1478.87(6)pm; Z = 4; Pbcm; R = 0.034, Rw = 0.032.
    Notes: Aus salzsauren Lösungen von ReCl3 und Ethylendiammoniumchlorid und/oder Piperaziniumchlorid kristallisieren beim Einengen der tiefroten Salze (EnH2)2(PipzH2) [Re3Cl12]2 m6H2O(1), (EnH2) (PipzH2)[Re3Cl12]CI · H2O (2), und (PipzH2) [re3Cl11(H2)] · 3H2O (3) aus. Ihre Kristallstrukturen wurden aus Vierkreisdiffraktometer-Daten bestimmt.1:monoklin; a = 1889,63(11), b = 1615,82(8), c = 790,28(4) pm; β = 101,354(5)°; Z = 2; P21/n; R = 0,119, Rw = 0,070.2:triklin; a = 1330,35(4), b = 1015,14(5), c = 1165,32(6) pm; α = 122,308(4), β = 102,412(3), γ = 92,226(4)°; Z = 2,P1; R = 0,092, Rw = 0,059.3:orthorhombisch; a = 971,43(4), b = 1619,51(7), c = 1478,87(6) pm; Z = 4; Pbcm; R = 0,034, Rw = 0,032.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926070113
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  • 5
    Electronic Resource
    Electronic Resource
    Rhenium trichloride, ReCl3, and its 5/3-hydrate synthesis, crystal structure, and thermal expansion (1987)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 552 (1987), S. 81-89 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Rheniumtrichlorid, ReCl3, und sein 5/3-Hydrat. Synthese, Kristalstruktur und thermische AusdehnungReCl3 wurde durch Vakuumsublimaton in Form von Einkristallen erhalten und die Kristallstruktur verfeinert (trigonal, R3m, a = 1020,62(5); c = 2035,3(2) pm; Vm = 61,340(8) cm3 mol-1; R = 0,049 Rw = 0,031). Aus salzsauren Lösungen bon ReCl3, die me4NCl enthalten, läßt sich das Hydrat ReCl3 · 5/3 H2O aussalzen: exagonal, P62c, a = 944,89(3); c = 1470,07(9) pm; Vm = 114,09(1) cm3 mol-1. Die kristallstruktur (R = 0,079; Rw = 0,051) wird aus hexagonal dichtest-gepackten molekülen [Re3Cl9(H2O)3] aufgebaut, die lose durch zwei moleküle Kristallwasser zwischen den Clustern in Richtung [00.1] zusammengehalten werden. Hierdurch bilden sich „Ketten“, die gegeneinander um 1/2c verschoben sind. Die thermische Ausdehnung von ReCl3, ReCl3 · 5/3 H2O and RbReCl4 wurde gemessen und wird im Zusammenhang mit den Kristallstrukturen diskutiert.
    Notes: Single crystals of ReCl3 were grown by vacuum sublimation and the crystal structure (trigonal, R3m, a = 1020.62(5), c = 2035.3(2) pm, Vm = 61.430(8) cm3mol-1) was refined to R = 0.049, Rw = 0.031. From hydrochloric acid solutions of ReCl3 containing me4NCl, the hydrete ReCl3 · 5/3 H2O is salted out: hexagonal, P62c, a = 944.89(3), c = 1470.07(9) pm, Vm = 114.09(1) cm3 mol-1. The crystal structure (R = 0.079, Rw = 0.051) contains hexagonally closest-packed [Re3Cl9(H2O)3] molecules held loosely together by two molecules of crystal water positioned between the clusters in the [00.1] direction thereby forming chains that are shifted against each other by 1/2c. Thermal expansion of ReCl3, ReCl3. 5/3 H2O and RbReCl4 has been recorded and is discussed in connection with the crystal structures.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19875520908
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  • 6
    Electronic Resource
    Electronic Resource
    NH4[Re3Cl10(OH2)2] · 2 H2O: Synthese und Struktur Ein Beispiel für starke N—H … O- und O—H … Cl-Bindungen (1986)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 534 (1986), S. 115-120 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: NH4[Re3Cl10(OH2)2] · 2 H2O: Synthesis and Structure. An Example for “Strong” N—H … O and O—H … Cl Hydrogen BondingThe red NH4[Re3Cl10(OH2)2] · 2 H2O crystallizes from hydrochloric-acid solutions of ReCl3 with NH4Cl. It is tetragonal, P41212, No. 92, a = 1157.6, c = 1614.5 pm, Z = 4. The crystal structure contains “isolated” clusters [Re3Cl10(OH2)2]-. These contain Cl…H—O—H…Cl units with “very strong” hydrogen bonds: distances Cl—O are only 286 pm. NH4+ has seven Cl- as nearest neighbours and, additionally, one H2O which belongs to a cluster [d(N—O1) = 271 pm] and one crystal water [d(N—O2) = 286 pm].
    Notes: Aus der salzsauren Lösung von ReCl3 kristallisiert mit NH4Cl rotes NH4[Re3Cl10(OH2)2] · 2 H2O aus; tetragonal, P41212 (Nr. 92), a = 1157,6; c = 1614,5 pm, Z = 4. Es treten „isolierte“ Cluster [Re3Cl10(OH2)2]- auf. Sie enthalten die Gruppierung Cl…H—O—H…;Cl mit „sehr starken“ Wasserstoff-Brücken-Bindungen, d(Cl—O) = 286 pm. NH4+ hat 7 Cl- als nächste Nachbarn, zusätzlich 2 H2O, von denen eines einem Cluster angehört [d(N—O1) = 271 pm], das andere ist „Kristallwasser“ [d(N—O2) = 286 pm].
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19865340315
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  • 7
    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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  • 8
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    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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  • 9
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    Electronic Resource
    Synthesis, Molecular and Crystal Structure of a Second Rhenium Trichloride Hydrate: [Re3Cl9(H2O)3] · 10 H2OProfessor Hans-Uwe Schuster zum 60. Geburtstage am 20. Februar 1990 gewidmet (1990)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 581 (1990), S. 104-110 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese, Molekül- und Kristallstruktur eines zweiten Hydrates des Rheniumtrichlorids: [Re3Cl9(H2O)3] · 10 H2ODas Dekahydrat von [Re3Cl9(H2O)3] erhält man aus der wäßrigen Lösung von ReCl3 bei Temperaturen von 0 bis -5°C. Die Kristallstruktur (orthorhombisch, Pnma, Z = 4; a = 1 125,16(3), b = 1 630,30(5), c = 1 378,84(5) pm) wurde aus Einkristall-Diffraktometer-Daten bestimmt. Die Moleküle [Re3Cl9(H2O)3] werden in Richtung [0 1 0] gestapelt und durch Kristallwasser voneinander getrennt. Gemeinsam mit dem „Koordinationswasser“ in den Molekülen bilden sie ein System starker Wasserstoffbrücken-Bindungen, wenn dies aus den kurzen Abständen d (O—O) = 277 pm alleine geschlossen werden darf.
    Notes: The decahydrate of [Re3Cl9(H2O)3] is obtained from aqueous solutions of ReCl3 at zero to -5°C. The crystal structure (orthorhombic, Pnma, Z = 4; a = 1125.16(3), b = 1 630.30(5), c = 1 378.84(5) pm) has been determined from single-crystal X-ray diffractometer data. The [Re3Cl9(H2O)3] molecules are stacked in the [0 1 0] direction and the rows of such molecules are separated by the crystal water molecules. Together with the water ligands, these form a rather strong hydrogen bonding system judging from O—O distances (d = 277 pm) alone.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19905810114
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  • 10
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    Sulfat, Phosphat und Arsenat als dreizähnige Liganden. Synthese und Kristallstrukturen von (NMe4)2[Re3Cl9O3SO], (NMe4)2(H7O3)[Re3Cl9O3PO] und (NMe4)2(H5O2)[Re3Cl9O3AsO] (1990)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 587 (1990), S. 197-207 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Sulfate, Phosphate, and Arsenate as Tridentate Ligands. Synthesis and Crystal Structures of (NMe4)2[Re3Cl9O3SO], (NMe4)2(H7O3)[Re3Cl9O3PO] and (NMe4)2(H5O2)[Re3Cl9ODark red (NMe4)2[Re3Cl9O3SO] (1) (monoclinic, P21/c, a = 1129.77(6) pm, b = 1890.46(7) pm, c = 1290.09(9) pm, β = 97.29(1)°, Vm = 411.49(4) cm3/mol) is obtained by direct reaction of rhenium trichloride with NMe4Cl in hydrochloric acid solution in the presence of sulfuric acid. Dark red crystals of (NMe4)2(H7O3)[Re3Cl9O3PO] (2) (monoclinic, P21/c, a = 1249.3(1) pm, b = 1760.5(2) pm, c = 1335.1(1) pm, β = 91.71(1)°, Vm = 441.91(7) cm3/mol) and (NMe4)2(H5O2)[Re3Cl9O 3AsO] (3) (monoclinic, P21/c, a = 975.23(6) pm, b = 1838.6(1) pm, c = 1572.31(7) pm, β = 92.39(1)°, Vm = 424.10(4) cm3/mol) grow from the hydrochloric acid solution of NMe4Cl of the violet precipitate that is obtained previously by the reaction of ReCl3 and Ag3[MO4] (M = P, As) in acetone solution. Important features of the crystal structures of (1), (2), and (3) are anionic building units [Re3Cl9O3MO]n- (M = S, n = 2; M = P, As, n = 3), where the tetrahedral anions [MO4]n- act as tridentate ligands. In the structures of (2) and (3) the anions form a hydrogen bonding system together with the cations H7O3+ (2) and “H5O2+” (3).
    Notes: Tiefrotes (NMe4)2[Re3Cl9O3SO] (1) (monoklin; P21/c: a = 1129,77(6) pm; b = 1890,46(7) pm; c = 1290,09(9) pm; β = 97,29(1)°; Vm = 411,49(4) cm3/mol) ist durch direkte Umsetzung von Rheniumtrichlorid mit NMe4Cl in salzsaurer Lösung in Gegenwart von Schwefelsäure zugänglich. Tiefrote Kristalle von (NMe4)2(H7O3)[Re3Cl9O3PO] (2) (monoklin; P21/c; a = 1249,3(1) pm; b = 1760,5(2) pm; c = 1335,1(1) pm; β = 91,71(1)°; Vm = 441, 91(7) cm3/mol) und (NMe4)2(H5O2)[Re3Cl9O 3AsO] (3) (monoklin; P21/c; a = 975,23(6) pm; b = 1838,6(1) pm; c = 1572,31(7) pm; β = 92,39(1)°; Vm = 424,10(4) cm3/mol) erhält man durch Umsetzung von ReCl3 mit Ag3[MO4] (M = P, As) in Aceton und anschließende Umsetzung des gebildeten violetten Niederschlags beim Eindunsten salzsaurer Lösungen in Gegenwart von NMe4Cl. Hervorstechende Strukturmerkmale von (1), (2) und (3) sind anionische Baugruppen [Re3Cl9O3MO]n- (M = S, n = 2; M = P, As, n = 3), in denen die tetraedrischen Anionen [MO4]n- als dreizähnige Liganden fungieren. In (2) und (3) sind die Anionen mit den Kationen H7O3+ (2) bzw. „H5O2+“ (3) in ein ausgedehntes System von Wasserstoffbrücken-Bindungen eingebunden. 3AsO].
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19905870121
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