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  • synthesis  (7)
  • syntheses  (5)
  • Nitrido ligand  (2)
  • 1
    Electronic Resource
    Electronic Resource
    Donor-Akzeptorkomplexe [SnCl4(Se4N2)2] und [TiCl4(Se4N2)] (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 606 (1991), S. 73-78 
    Details
    ISSN: 0044-2313
    Keywords: Complexes of tetraselenium-dinitride ; syntheses ; IR-spectra ; 119Sn-Mössbauer spectrum ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Donor-Acceptor Complexes [SnCl4(Se4N2)2] and [TiCl4(Se4N2)]The donor-acceptor complexes [SnCl4(Se4N2)2] and [TiCl4(Se4N2)] have been prepared by the reactions of Se4N2 with SnCl4 and TiCl4, respectively, in CH2Cl2 suspensions, forming red-brown, moisture sensitive crystal powders. The complexes are characterized by i. r. spectroscopy, the tin compound additionally by 119Sn Mössbauer spectroscopy. According to the spectra, in the tin complex both Se4N2 molecules are bonded with one of the nitrogen atoms at the tin atom in transposition (symmetry Ci), whereas in the titanium complex we assume both nitrogen atoms to be bonded in a chelating fashion at the titanium atom.
    Notes: Die Donorakzeptorkomplexe [SnCl4(Se4N2)2] und [TiCl4(Se4N2)] werden aus den Komponenten Se4N2 und SnCl4 bzw. TiCl4 in CH2Cl2-Suspensionen in Form rotbrauner, feuchtigkeitsempfindlicher Kristallpulver hergestellt. Die Komplexe werden durch ihre IR-Spektren, die Zinnverbindung zusätzlich durch das 119Sn-Mößbauer-Spektrum charakterisiert. Danach sind die Se4N2-Moleküle in der Zinnverbindung in trans-Position über je ein N-Atom an das Zinnatom koordiniert (Symmetrie Ci), während in dem Titankomplex vermutlich beide N-Atome des Se4N2-Moleküls chelatartig an das Titanatom gebunden sind.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916060107
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  • 2
    Electronic Resource
    Electronic Resource
    Osmium-Nitridtrichlorid, OsNCl3 (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1205-1208 
    Details
    ISSN: 0044-2313
    Keywords: Osmium Nitridotrichloride ; synthesis ; IR spectrum ; magnetic susceptibility ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Osmium Nitridotrichloride, OsNCl3OsNCl3 was prepared by the reaction of (NH4)2[OsNCl5] with chlorine at 300°C, forming a black, X-ray amorphous moisture sensitive, paramagnetic powder which was characterized by IR spectroscopy and measurement of the magnetic susceptibility in the range of 5-300 K.
    Notes: OsNCl3 wird als schwarzes, röntgenamorphes, feuchtigkeitsempfindliches paramagnetisches Pulver durch Reaktion von (NH4)2[OsNCl5] mit Chlor bei 330°C hergestellt und IR-spektroskopisch sowie durch magnetische Suszeptibilitätsmessungen im Bereich von 5-300 K charakterisiert.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19966220717
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  • 3
    Electronic Resource
    Electronic Resource
    Über die Kronenetherkomplexe [K(15-Krone-5)2]3[Sb3I12], [TeCl3(15-Krone-5)][TeCl5] und [TeCl3(15-Krone-5)]2[TeCl6] (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 55-61 
    Details
    ISSN: 0044-2313
    Keywords: Crown ether complexes ; tellurium ; antimony ; syntheses ; i.r. spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Crown Ether Complexes [K(15-Crown-5)2]3[Sb3I12], [TeCl3(15-Crown-5)][TeCl5], and [TeCl3(15-Crown-5)]2[TeCl6]Orange-coloured crystals of [K(15-crown-5)2]3[Sb3I12] are formed in the reaction of potassium iodide with antimony triiodide and 15-crown-5 in acetonitrile solution. An X-ray structure determination reveals severe disorder of the crown ether molecules, which coordinate to the potassium atoms in a sandwich array; so only the [Sb3I12]3- ion and the potassium positions were ascertained. The anion is a centrosymmetric trimer (symmetry C2h), which can be understood as central SbI63- ion, coordinated by two SbI3 molecules. (Space group C2/m), Z = 2, 3263 observed, independent reflections, R = 0.06, lattice dimensions at 20°C: a = 2541.1 pm, b = 1441.7 pm, c = 1588.4 pm, β = 113.33°.The tellurium complexes [TeCl3(15-crown-5)] [TeCl5] and [TeCl3(15-crown-5)]2[TeCl6] are prepared by reaction of TeCl4 with 15-crown-5 in acetonitrile solution, forming yellow-green crystals sensitive to moisture. They are characterized by their i.r. spectra.
    Notes: Orange Kristalle [K(15-Krone-5)2]3[Sb3I12] entstehen durch Einwirkung von Kaliumiodid auf Antimontriiodid bei Anwesenheit von 15-Krone-5 in Acetonitrillösung. Wegen Fehlordnung der die Kaliumionen sandwichartig koordinierenden Kronenethermoleküle konnten röntgenogrpahisch in der Struktur nur das [Sb3I12]3--Ion sicher aufgeklärt werden. Es bildet ein zentrosymmetrisches Trimer (Symmetrie C2h), das sich als zentrales SbI63--Ion mit zwei koordinierten SbI3-Molekülen auffassen läßt. Raumgruppe C2/m, Z = 2, 3263 unabhängige beobachtete Reflexe, R = 6,2%. Gitterabmessungen bei 20 °C: a = 2541,1; b = 1441,7; c = 1588,4 pm, β = 113,33°.Die Tellurokomplexe [TeCl3(15-Krone-5)] [TeCl5] und [TeCl3(15-Krone-5)]2[TeCl6] entstehen aus TeCl4 und 15-Krone-5 in Acetonitrillösung als gelbgrüne, feuchtigkeitsempfindliche Kristalle, die durch ihre IR-Spektren charakterisiert werden.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915960108
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  • 4
    Electronic Resource
    Electronic Resource
    Benzamidinium-Hexachlorostannat Synthese und Kristallstruktur (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 133-138 
    Details
    ISSN: 0044-2313
    Keywords: Benzamidinium hexachlorostannate ; synthesis ; crystal structure ; i.r. spectrum ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Benzamidinium Hexachlorostannate: Synthesis and Crystal Structure[Ph—C(NH2)2SnCl6] has been prepared by the reaction of hydrogen chloride with the amidinato complex [Ph—C(NSiMe3)2SnCl3] in CH2Cl2 solution, forming colourless crystals. which were characterized by IR spectroscopy as well as by an X-ray structure determination. Space group P21/c, Z = 4, 3070 observed unique reflexions, R = 0.029. Lattice dimensions at -50°C: a = 892.5, b = 1076.7, c = 1175.6 pm, β = 109.3°. The compound consists of benzamidinium ions C6H5—C(NH2)2+ and anions SnCl62-, which are connected by a network of N—H…Cl hydrogen bridges.
    Notes: [Ph—C(NH2)2]2SnCl6 entsteht in Form farbloser Einkristalle durch Einwirkung von Chlorwasserstoff auf eine Lösung des Amidinatokomplexes [Ph—C(NSiMe3)2SnCl3] in Dichlormethan. Die Verbindung wird durch das IR-Spektrum und durch eine röntgenographische Strukturanalyse charakterisiert. Raumgruppe P21/c, Z = 4, 3070 beobachtete unabhängige Reflexe, R = 2,9%. Gitterabmessungen bei -50°C: a = 892,5; b = 1076,7; c = 1175,6 pm; β = 109,3°. Die Verbindung besteht aus Benzamidinium-Kationen C6H5—C(NH2)2+ und SnCl62--Ionen, in denen ein Netz von N—H…Cl-Wasserstoffbrücken besteht.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915960118
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  • 5
    Electronic Resource
    Electronic Resource
    Chalkogeno-Fluoro-Wolframate. Die Kristallstrukturen von [Na-15-Krone-5]2[WO2F3]2 · 2 2 CH3CN und [Na-15-Krone-5]2[WOSF3]2 · 2 CH3CNHerrn Professor Hanskarl Müller-Buschbaum zum 60. Geburtstage am 24. Mai 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 121-132 
    Details
    ISSN: 0044-2313
    Keywords: Chalcogeno-fluorotungstates ; syntheses ; i.r. spectra ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chalcogeno-Fluoro-Tungstates. The crystal Structures of [Na-15-Crown-5]2[WO2F3]2 ·2 CH3CN and [Na-15-Crown-5]2[WOSF3]2 · 2 CH3CNThe reaction of sodium fluoride with WSCL4 in acetonitrile solution successively leads in the presence of 15-crown-5 to the complexes [Na-15-crown-5][WSCl4F], [Na-15-crown-5]2[WSCl2F3], and [Na-15-crown-5][WSF5]. These complexes are characterized by their i.r. spectra. In acetonitrile partial hydrolysis of [Na-15-crown-5][WSF5] leads to [Na-15-crown-5]2[WSOF3]2 · 2 CH3CN; likewise one obtains [Na-15-crown-5]2[WO2[WO2F3]2] · 2 CH3CN from [Na-15-crown-5]2[WSOF7] by partial hydrolysis. X-ray structural analyses were carried out for both these chalcogeno complexes. [Na-15-crown-5]2[WO2F3]2 · 2 CH3CN: space group P1, Z = 1, 2316 unique observed reflexions, R = 0.036. Lattice dimensions at -65°C: a = 851.0, b = 1064.6, c = 1130.2 pm, α = 105.18°, β = 95.12°, γ = 102.48°.[Na-15-crown-5]2[WOSF3]2 · 2 CH3CN: space group P1, Z = 1,2472 unique observed reflexions, R = 0.030. Lattice dimensions at -80°C: a = 856.3, b = 1062.8, c = 1181.1 pm, α = 107.68°, β = 95.52°, γ = 102.65°.Both compounds are isotypical with each other; they form ion triples which originate from two short Na…F-contacts of 232 pm each with the four axially arranged fluorine ligands of the dimeric anions [WO2F3]22- and [WSOF3]22-, respectively. The dimerization takes place via angular fluoro bridges with W—F-bondings which are only slightly differing in length. The chalcogeno ligands are in the trans-positions to the bridging fluorine atoms.
    Notes: Die Reaktion von Natriumfluorid mit WSCl4 in Acetonitrillösung führt in Gegenwart von 15-Krone-5 schrittweise zu den Komplexen [Na-15-Krone-5][WSCl4F], [Na-15-Krone-5][WSCl2F3] und [Na-15-Krone-5][WSF5], die durch ihre IR-Spektren charakterisiert werden. Partielle Hydrolyse von [Na-15-Krone-5][WSF5] führt in Acetonitril zu [Na-15-Krone-5]2[WSOF3]2 · 2 CH3CN, ebenso erhält man aus [Na-15-Krone-5][WF7] durch partielle Hydrolyse [Na-15-Krone-5]2[WO2F3]2 · 2 CH3CN. Von beiden Chalkogenokomplexen wurden röntgenographische Strukturanalysen ausgeführt.[Na-15-Krone-5]2[WO2F3]2 · 2 CH3CN: Raumgruppe P1, Z = 1, 2316 unabhängige beobachtete Reflexe, R = 3,6%. Gitterkonstanten bei -65°C: a = 851,0; b = 1064,6; c = 1130,2 pm; α = 105,18°; β = 95,12°; γ = 102,48°. [Na-15-Krone-5]2[WOSF3]2 · 2 CH3CN: Raumgruppe P1, Z = 1, 2472 unabhängige beobachtete Reflexe, R = 3,0%. Gitterkonstanten bei -0°C: a = 856,3; b = 1062,8; c = 1181,1 pm; α = 107,68°; β = 95,52°; γ = 102,65°.Beide Verbindungen sind miteinander isotyp; sie bilden Ionentripel, die durch je zwei kurze Na…F-Kontakte von 232 pm mit den vier axial angeordneten Fluorliganden der dimeren Anionen [WO2F3]22- bzw. [WSOF3]22- zustandekommen. Die Dimerisierung erfolgt über gewinkelte Fluorobrücken mit nur wenig verschieden langen W—F-Bindungen. Die Chalkogenoliganden befinden sich in den trans-Positionen zu den Brücken-F-Atomen.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19915960117
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  • 6
    Electronic Resource
    Electronic Resource
    Trimethylsilyl-substituierte Amidinatokomplexe von Thallium(III). Die Kristallstruktur von [Ph—C(NHSiMe3)2] [Ph—C(NSiMe3)2 TICI3]Herrn Professor Eberhard Hoyer zum 60. Geburtstage am 26. Mai 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 600 (1991), S. 7-14 
    Details
    ISSN: 0044-2313
    Keywords: Amidinato complexes of thallium(III) ; syntheses ; i.r. spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Trimethylsilyl Substituted Amidinato Complexes of Thallium(III). The Crystal Structure of [Ph—C(NHSiMe3)2] [Ph—C(NSiMe3)2TlCl3]The amidinato complexes [Ph—C(NSiMe3)2TlCl3] and [Ph—C(NHSiMe3)2] [Ph—C(NSiMe3)2TlCl3] have been prepared by the reaction of TlCl3 with N,N,N′-tris(trimethylsilyl)benzamidine in THF solution. They were characterized by IR spectroscopy, [Ph—C(NHSiMe3)2] [Ph—C(NSiMe3)2TlCl3] additionally by an X-ray structure determination. Space group P21/c, Z = 4, 4300 observed unique reflexions, R = 0.053. Lattice dimensions at -43°C: a = 1157.2, b = 2346.3, c = 1536.9 pm, β = 105.98°. The structure consists of amidinium cations, and of anions [Ph—C(NSiMe3)2TlCl3]-, in which the thallium atom is fivefold surrounded by three chlorine atoms and by two nitrogen atoms of the amidinato chelate.
    Notes: Die Amidinatokomplexe [Ph—C(NHSiMe3)2TlCl2] und [Ph—C(NHSiMe3)2TlCl2] [Ph—C(NSiMe3)2TlCl3] entstehen bei der Einwirkung von Thallium(III)-chlorid auf N,N,N′-Tris(trimethylsilyl)benzamidin in Tetrahydrofuranlösung. Sie werden durch ihre IR-Spektren, und [Ph—C(NHSiMe3)2] [Ph—C(NSiMe3)2TlCl3] zusätzlich durch eine Kristallstrukturanalyse charakterisiert. Raumgruppe P21/c, Z = 4, 4300 unabhängige beobachtete Reflexe, R = 5,3%. Die Gitterkonstanten betragen bei -43°C: a = 1157,2; b = 2346,3; c = 1536,9 pm; β = 105,98°. Die Verbindung besteht aus einem Amidiniumkation und einem [Ph—C(NSiMe3)2TlCl3]--Anion, in dem das Thalliumatom verzerrt trigonal-bipyramidal von drei Cl-Atomen und chelatartig von den beiden N-Atomen des Amidinatoliganden umgeben ist.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916000102
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  • 7
    Electronic Resource
    Electronic Resource
    Synthese, Kristallstruktur und 121Sb-Mößbauer-Spektrum von [SbCl2(18-Krone-6)]+SbCl6- (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 618 (1992), S. 93-97 
    Details
    ISSN: 0044-2313
    Keywords: Crown ether complex of antimony ; synthesis ; 121Sb-Mössbauer spectrum ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Crystal Structure, and 12Sb-Mössbauer Spectrum of [SbCl2(18-Crown-6)]+SbCl6-The title compound, which has been prepared by the reaction of antimony trichloride and antimony pentachloride in the presence of 18-crown-6 in acetonitrile solution, is characterized by its 121Sb-Mössbauer spectrum and by an X-ray structure determination. Space group P21, Z = 2, 2439 observed unique reflections, R = 0.045, wR = 0.043. Lattice dimensions at -80°C: a = 780.6(7), b = 1297.5(9), c = 1 278.5(10) pm, β = 100.56(7)°. The structure of [SbCl2(18-crown-6)]+SbCl6- contains cations in which the antimony atom in the first coordination sphere is surrounded in a φ-trigonal-bipyramidal fashion by two oxygen atoms of the crown ether in axial position as well as in the equatorial position by the two chlorine atoms and the lone electron pair.
    Notes: Die Titelverbindung entsteht aus Antimontrichlorid und Antimonpentachlorid in Gegenwart von 18-Krone-6 in Acetonitrillösung. Sie wird durch ihr 121Sb-Mößbauer-Spektrum und durch eine röntgenographische Strukturanalyse charakterisiert. Raumgruppe P21, Z = 2, 2439 beobachtete unabhängige Reflexe, R = 4,50%, wR = 4,25%. Die Gitterkonstanten betragen bei -80°C: a = 780,6(7); b = 1 297,5(9); c = 1 278,5(10) pm, β = 100,56(7)°. [SbCl2(18-Krone-6)]+SbCl6- enthält Kationen, in denen das Antimonatom in erster Koordinationssphäre φ-trigonal-bipyramidal von zwei O-Atomen des Kronenethers in Axialposition und von den beiden Cl-Atomen sowie dem freien Elektronenpaar äquatorial umgeben ist.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926180117
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  • 8
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstruktur von [Li(12-Krone-4)2][ReCl5(CH3CN)] · CH3CNHerrn Professor Joseph Grobe zum 60. Geburtstage am 2. November 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 606 (1991), S. 109-117 
    Details
    ISSN: 0044-2313
    Keywords: Pentachlorohenate(IV)-acetonitrile solvate ; 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 [Li(12-Crown-4)2][ReCl5(CH3CN)] · CH3CNThe title compound has been prepared by the reaction of lithium chloride with rhenium pentachloride in the presence of 12-crown-4 in acetonitrile solution.[Li(12-crown-4)2][ReCl5(CH3CN)] · CH3CN has been characterized by IR spectroscopy as well as by an X-ray structure determination. Space group P1, Z = 2, 4 450 observed unique reflections, R = 0.047, Lattice dimensions at 20°C: a = 1 445.8, b = 1 463.2, c = 1 580.2 pm, α = 89.28°, β = 114.19°, γ = 89.40°. The compound is ionic, the cation being formed by a lithium ion coordinated by the eight oxygen atoms of two crown ether molecules 12-crown-4 in sandwich fashion. In the anions [ReCl5(CH3CN)]- the rhenium atoms are in a distorted octahedral shape by the five chlorine atoms and by the N atom of the acetonitrile molecule. The two crystallographically independent cations and anions, respectively, are only slightly different.
    Notes: Die Titelverbindung wurde durch Reaktion von Lithiumchlorid mit Rheniumpentachlorid in Gegenwart von 12-Krone-4 in Acetonitrillösung hergestellt und durch ihr IR-Spektrum und durch eine röntgenographische Strukturanalyse charakterisiert.[Li(12-Krone-4)2][ReCl5(CH3CN)] · CH3CN kristallisiert triklin in der Raumgruppe P1 mit zwei Formeleinheiten pro Elementarzelle, 4 450 beobachtete unabhängige Reflexe, R = 4,7%. Gitterabmessungen bei 20°C: a = 1 445,8; b = 1 463,2; c = 1 580,2 pm; α = 89,28°; β = 114,19°; γ = 89,40°. Die Verbindung hat einen ionischen Aufbau, in dem die Lithiumionen sandwichartig von den acht Sauerstoffatomen zweier Kronenethermoleküle 12-Krone-4 koordiniert sind. In den Anionen [ReCl5(CH3CN)]- sind die Rheniumatome verzerrt oktaedrisch von den fünf Chloratomen und von dem N-Atom des Acetonitrilmoleküls umgeben. Die beiden kristallographisch unabhängigen Kationen bzw. Anionen unterscheiden sich nur wenig voneinander.
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    URL: http://dx.doi.org/10.1002/zaac.19916060112
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  • 9
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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.
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    URL: http://dx.doi.org/10.1002/zaac.19936190423
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  • 10
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    Kronenetherkomplexe von Blei(II). Die Kristallstrukturen von [PbCl(18-Krone-6)][SbCl6], [Pb(18-Krone-6)(CH3CN)3][SbCl6]2, and [Pb(15-Krone-5)2][SbCl6]2 (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1704-1712 
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    ISSN: 0044-2313
    Keywords: Crown ether complexes of lead ; syntheses ; ir. spectra ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crown Ether Complexes of Lead(II). The Crystal Structures of [PbCl(18-Krone-6)][SbCl6], [Pb(18-Krone-6)(CH3CN)3][SbCl6]2 und [Pb(15-Krone-5)2][SbCl6]2.[PbCl(18-crown-6)][SbCl6] has been prepared in low yield besides [Pb(CH3)2(18-crown-6)][SbCl6]2 by the reaction of Pb(CH3)2Cl2 with antimony pentachloride in acetonitrile solution in the presence of 18-crown-6, forming pale-yellow crystals. The other two title compounds are formed as colourless crystals by the reaction of PbCl2 with antimony pentachloride in acetonitrile solutions in the presence of 18-crown-6 and 15-crown-5, respectively. The complexes were characterized by IR spectroscopy and by crystal structure determinations.[PbCl(18-crown-6)][SbCl6]: Space group P21/c, Z = 8, 5 003 observed unique reflections, R = 0.046. Lattice dimensions at - 80°C: a = 1 386.9; b = 1 642.7; c = 2 172.1 pm, β = 92.95°. The lead atom in the cation [PbCl(18-crown-6)]+ is surrounded in an almost hexagonal-planar construction by the six oxygen atoms of the crown ether and an axially oriented Cl atom.[Pb(18-crown-6)(CH3CN)3][SbCl6]2: Space group P1, Z = 2, 6 128 observed unique reflections, R = 0.076. Lattice dimensions at - 70°C: a = 1 228.0; b = 1 422.9; c = 1 463.2 pm, α = 69.08°; β = 65.71°; γ = 64.51°. In the cation [Pb(18-crown-6)(CH3CN)3]2+ the lead atom is coordinated by the six oxygen atoms of the crown ether and by the three nitrogen atoms of the acetonitrile molecules. The structure determination is restricted by disorder.[Pb( 15-crown-5)2][SbCI6]2: Space group P63/m, Z = 6, 5 857 observed unique reflections, R = 0.059. Lattice dimensions at -70°C: a = b = 2 198.5; c = 1499.4 pm, α = β = 90°, γ = 120°. In the cation [Pb(l5-crown-5)2]2 the lead atom is sandwich-like coordinated by the ten oxygen atoms of the two crown ether molecules. The structure determination is restricted by disorder.
    Notes: [PbCl(18-Krone-6)][SbCl6] entsteht in geringer Menge neben [Pb(CH3)2(18-Krone-6)][SbCl6]2 in Form blaßgelber Kristalle bei der Einwirkung von Antimonpentachlorid auf Pb(CH3)2Cl2 in Acetonitrillösung in Gegenwart von 18-Krone-6. Die beiden übrigen Titelverbindungen werden aus PbCl2 und 18-Krone-6 bzw. 15-Krone-5 durch Reaktion mit Antimonpentachlorid in Acetonitril als farblose Kristalle erhalten. Die Komplexe wurden durch ihre IR-Spektren und durch Kristallstrukturanalysen charakterisiert.[PbCl(18-Krone-6)][SbCl6]: Raumgruppe P21/c, Z = 8, 5 003 beobachtete unabhängige Reflexe, R = 0,046. Gitterkonstanten bei - 80°C: a = 1 386,9; b = 1 642,7; c = 2 172,1 pm, β = 92,95°. In dem Kation [PbCl(18-Krone-6)]+ ist das Pb-Atom nahezu coplanar mit den sechs O-Atomen des Kronenethers angeordnet, während das Chloratom kovalent und axial mit dem Pb-Atom verbunden ist.[Pb(18-Krone-6)(CH3CN)3][SbCl6]2: Raumgruppe P1, Z = 2, 6 128 beobachtete unabhängige Reflexe, R = 0,076. Gitterkonstanten bei - 70°C: a = 1 228,0; b = 1 422,9; c = 1 463,2 pm, α = 69,08°; β = 65,71°; γ = 64,51°. In dem Kation [Pb(18-Krone-6)(CH3CN)3]2+ ist das Bleiatom neunfach durch die sechs O-Atome des Kronenethers und durch drei N-Atome der Acetonitrilmoleküle koordiniert. Die Genauigkeit der Strukturbestimmung ist durch Fehlordnung beeinträchtigt.[Pb(15-Krone-5)2][SbCl6]2: Raumgruppe P63/m, Z = 6, 5 857 beobachtete unabhängige Reflexe, R = 0,059. Gitterkonstanten bei - 70°C: a = b = 2 198,5; c = 1 499,4 pm, α = β = 90°, γ = 120°. In dem Kation [Pb(15-Krone-5)2]2+ ist das Bleiatom zehnfach sandwichartig durch die O-Atome der beiden Kronenethermoleküle koordiniert. Die Genauigkeit der Strukturbestimmung ist durch Fehlordnung beeinträchtigt.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936191013
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