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  • synthesis  (7)
  • syntheses  (5)
  • Nitrido ligand  (2)
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 606 (1991), S. 73-78 
    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.
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  • 2
    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.
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  • 3
    ISSN: 0044-2313
    Keywords: Polytellurido complexes of copper and silver ; synthesis ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Crystal Structures of the Polytellurido Complexes (PPh4)4[M2Te12] of Copper(I) and Silver(I)The title compounds have been prepared as black crystal needles by reactions of Na2Te3 with CuCl and AgNO3, respectively, in dimethylformamide in the presence of PPh4Br. With regard to the large cell dimensions the crystal structure determinations were done by an imaging plate instrument.(PPh4)4[Cu2Te12]: Space group P21/n, Z = 6, 51 338 detected reflections, structure determination with 14 177 unique reflections with I 〉 4σ(I), R = 0.081. Lattice dimensions at - 50°C: a = 1 704.5, b = 1 694.5, c = 5 044 pm, β = 94.20°.(PPh4)4[Ag2Te12]: Space group P21/n, Z = 6, 80 811 detected reflections, structure determination with 16 092 unique reflections with I 〉 3σ(I), R = 0.052. Lattice dimensions at - 50°C: a = 1 703.8, b = 1 722.9, c = 5 123 pm, β = 94.65°.The structures of the isotypic compounds consist of six symmetry independent PPh4+ ions and two symmetry independent anions [M2Te12]4-, in which the metal atoms of two (MTe4)--fivering fragments are linked by a Te42- chain.
    Notes: Die Titelverbindungen entstehen als schwarze Kristallnadeln aus Na2Te3 und CuCl bzw. AgNO3 in Dimethylformamid in Gegenwart von PPh4Br. Wegen der großen Zellabmessungen wurden die Kristallstrukturen mit Hilfe des Flächendetektors der Firma Stoe vermessen.(PPh4)4[Cu2Te12]: Raumgruppe P21/n, Z = 6, 51 338 gemessene Reflexe, Strukturlösung mit 14 177 unabhängigen Reflexen mit I 〉 4σ(I), R = 0,081. Gitterabmessungen bei - 50°C: a = 1 704,5; b = 1 694,5; c = 5 044 pm; β = 94,20°.(PPh4)4[Ag2Te12]: Raumgruppe P21/n, Z = 6, 80 811 gemessene Reflexe, Strukturlösung mit 16 092 unabhängigen Reflexen, mit I 〉 3σ(I), R = 0,052. Gitterabmessungen bei - 50°C: a = 1 703,8; b = 1 722,9; c = 5 123 pm; β = 94,65°.Die beiden miteinander isotypen Strukturen enthalten sechs symmetrieunabhängige PPh4+-Ionen und zwei symmetrieunabhängige Anionen [M2Te12]4-. In diesen sind die Metallatome zweier (MTe4)--Fünfringfragmente über eine Te42--Kette miteinander verknüpft.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 775-778 
    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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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Angewandte Chemie International Edition in English 20 (1981), S. 413-426 
    ISSN: 0570-0833
    Keywords: Multiple bonds ; Bond theory ; Nitrido ligand ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Numerous nitrido complexes of transition metals show very short metal-nitrogen bond lengths, suggesting M≡N-triple bonds. At present, compounds of this type are being intensively investigated. In particular the molybdenum complexes are considered as model substances for the study of at least an intermediate step of N2-assimilation. This article contains a review of the structure and bonding, as well as syntheses and reactions of these complexes.
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  • 6
    ISSN: 0044-2313
    Keywords: Crown ether complexes of Sb3+ and Bi3+ ; synthesis ; IR spectra ; 121Sb Mössbauer spectrum ; X-ray structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Sb(12-Crown-4)2(CH3CN)][SbCl6]3 and [Bi(12-Crown-4)2(CH3CN)][SbCl6]3, first Trications of Antimony(III) and Bismuth(III)The crown ether complexes [M(12-crown-4)2(CH3CN)][SbCl6]3 with M = Sb and Bi are formed by the reaction of antimony trichloride and bismuth trichloride, respectively, with antimony pentachloride in acetonitrile solution in the presence of 12-crown-4. They form colourless, moisture sensitive crystals, which were characterized by X-ray structure determinations and by IR spectroscopy. The complex with M = Sb was also characterized by 121Sb Mössbauer spectroscopy.Both complexes crystallize isotypically in the orthorhombic space group Pbcn with four formula units per unit cell.M = Sb: 3 483 observed unique reflections, R = 0.038. M = Bi: 2 958 observed unique reflections, R = 0.036. The compounds consist of SbCl6- ions and trications [M(12-crown-4)2(CH3CN)]3+, in which the M3+ ions are ninefold coordinated by the eight oxygen atoms of the crown ether molecules and by the nitrogen atom of the acetonitrile molecule. The lone pair of the M3+ ions has no steric effect.
    Notes: Die Kronenetherkomplexe [M(12-Krone-4)2(CH3CN)][SbCl6]3 mit M = Sb und Bi entstehen durch Reaktion von Antimontrichlorid bzw. Bismuttrichlorid mit Antimonpentachlorid in Acetonitrillösung in Gegenwart von 12-Krone-4. Sie bilden farblose, feuchtigkeitsempfindliche Kristalle, die wir durch kristallographische Strukturanalysen und durch die IR-Spektren charakterisiert haben. Von dem Komplex mit M = Sb wurde ein 121Sb-Mößbauer-Spektrum aufgenommen.Beide Komplexe kristallisieren isotyp in der orthorhombischen Raumgruppe Pbcn mit vier Formeleinheiten pro Elementarzelle. M = Sb: 3 483 beobachtete unabhängige Reflexe, R = 0,038. M = Bi: 2 958 beobachtete unabhängige Reflexe, R = 0,036. Die Verbindungen enthalten neben den SbCl6--Ionen Trikationen [M(12-Krone-4)2(CH3CN)]3+, in denen die M3+-Ionen durch die acht O-Atome der beiden Kronenethermoleküle und durch das N-Atom des Acetonitrilmoleküls neunfach koordiniert sind. Das freie Elektronenpaar an den M3+-Ionen bleibt ohne sterische Wirksamkeit.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 618 (1992), S. 93-97 
    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.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 606 (1991), S. 109-117 
    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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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1205-1208 
    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.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 55-61 
    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.
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