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  • 11
    Electronic Resource
    Electronic Resource
    {Mo2(O2C—Ph)2[Ph—C(NSiMe3)2]2}, ein Benzoato-Amidinato-Komplex von Molybdän(II)Frau Professor Marianne Baudler zum 70. Geburtstage am 27. April 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 594 (1991), S. 106-112 
    Details
    ISSN: 0044-2313
    Keywords: Benzoato-Amidinato Complex of Molybdenum(II) ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: {Mo2(O2C-Ph)2[Ph-C(NSiMe3)2]2}, a Benzoato-Amidinato Complex of Molybdenum(II)The title compound has been prepared by the reaction of Mo2(O2C—Ph)4 with N,N,N′-Tris(trimethylsilyl)benzamidine in boiling CH2Cl2, forming yellow-orange crystals, which were characterized by an X-ray structure determination.Space group C2/m, Z = 4, 1 886 observed unique reflexions, R = 0.053. Lattice dimensions at 20°C: a = 2 011.4, b = 1 115.5, c = 1 183.0 pm, β = 114.19°. The compound forms a molecular structure, in which the Mo⍣Mo dumbbell (bond length 208.3 pm) is surrounded by the chelating 0 atoms of two benzoato ligands and the N atoms of two amidinato ligands.
    Notes: Die Titelverbindung wird in Form gelboranger Kristalle bei der Reaktion von Mo2(O2C—Ph)4 mit N,N,N′-Tris(trimethylsilyl)benzamidin in siedendem Dichlormethan erhalten und durch eine röntgenographische Strukturanalyse charakterisiert.Raumgruppe C2/m, Z = 4, 1886 beobachtete unabhängige Reflexe, R = 5,3%. Gitterabmessungen bei 20°C: a = 2 011,4; b = 1 115,5; c = 1 183,0 pm, β = 114,19°. Die Verbindung hat eine Molekülstruktur, in der die Mo⍣Mo-Hantel (Bindungslänge 208,3 pm) von den O-Atomen zweier Benzoatoliganden und von den N-Atomen zweier Amidinatoliganden chelatartig umgeben ist.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19915940112
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  • 12
    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.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19915960108
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  • 13
    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.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19916060112
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  • 14
    Electronic Resource
    Electronic Resource
    Die Kristallstrukturen von Triphenylarsin-p-toluolsulfonylimin und seines Donor-Akzeptorkomplexes [ZrCl4(Ph3AsNSO2Tol)]2Professor Heinz Dieter Lutz zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 851-855 
    Details
    ISSN: 0044-2313
    Keywords: Triphenylarsin-p-toluene sulfonylimine ; Zirconium tetrachloride complex ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structures of Triphenylarsin-p-toluene Sulfonylimine and of its Donor-Acceptor Complex [ZrCl4(Ph3AsNSO2Tol)]2The molecular structures of the title compounds are reported. In the donor-acceptor complex [ZrCl4(Ph3AsNSO2Tol)]2 the zirconium atoms are bridged by the oxygen atoms of the triphenylarsin-p-toluene sulfonylimine molecules, forming a centrosymmetric dimer with a puckered Zr2O4S2 eight-membered ring in the chair conformation.Ph3AsNSO2Tol: Space group P1, Z = 2, structure determination with 4 010 observed unique reflections, R = 0.036. Lattice dimensions at 19°C: a = 897.52(4), b = 1 071.82(6), c = 1 337,49(5) pm, α = 110.280(4)°, β = 98.814(4)°, γ = 109.872(4)°.[ZrCl4(Ph3AsNSO2Tol)]2: Space group P21/n, Z = 4, structure determination with 3 762 observed unique reflections, R = 0.078. Lattice dimensions at -60°C: a = 1 387.3(4), b = 1 434.9(2), c = 1 404.7(4) pm, β = 92.71(1)°.
    Notes: Es wird über die Molekülstrukturen der beiden Titelverbindungen berichtet. In dem Donor-Akzeptorkomplex [ZrCl4(Ph3AsNSO2Tol)]2 sind die Zirkoniumatome über die O-Atome der Triphenylarsin-p-toluolsulfonylimin-Moleküle zu einem zentrosymmetrischen Dimer mit einem Zr2O4S2-Achtring in der Sesselkonformation verknüpft.Ph3AsNSO2Tol: Raumgruppe P1, Z = 2, Strukturlösung mit 4 010 unabhängigen beobachteten Reflexen, R = 0,036. Gitterkonstanten bei 19°C: a = 897,52(4), b = 1 071,82(6), c = 1 337,49(5) pm, α = 110,280(4)°, β = 98,814(4)°, γ = 109,872(4)°.[ZrCl4(Ph3AsNSO2Tol)]2: Raumgruppe P21/n, Z = 4, Strukturlösung mit 3 762 unabhängigen beobachteten Reflexen, R = 0,078. Gitterkonstanten bei -60°C: a = 1 387,3(4), b = 1 434,9(2), c = 1 404,7(4) pm, β = 92,71(1)°.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200517
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  • 15
    Electronic Resource
    Electronic Resource
    Phenylethinyl-[1,3,2]dithiaphospholan. Bis(dithiaphospholanyl)-[1,4]dithian (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1714-1718 
    Details
    ISSN: 0044-2313
    Keywords: Alkinyl thiophosphinous acid ester ; alkinyl [1,3,2]dithiaphospholane ; [1,4]dithiane ; nmr, mass, i.r. spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phenylethinyl-[1,3,2]dithiaphospholane. Bis(dithiaphospholanyl)-[1,4]dithianeNucleophilic substitution of the amino group but no cycloaddition occurs in the reaction of phenyl phenylethinyl phosphinous acid diethylamide, 5, with 2-aminothiophenol forming compound 6. By analogous reaction, phenylethinyl phosphonic bis(diethylamide), 7, and ethane-1,2-dithiol form compound 8. Cycloaddition besides nucleophilic substitution is observed, however, when acetylene bis(phosphonic diethyl-amide), 9, and ethane-1,2-dithiol are reacted resulting in compound 11. All new products are characterized by their nmr, mass, and i.r. spectra. Furthermore, the results of an X-ray structure analysis of 11 are reported.
    Notes: Bei der Reaktion von Phenyl-phenylethinyl-phosphinigsäure-diethylamid, 5, mit 2-Aminothiophenol findet keine Cycloaddition statt sondern eine nukleophile Substitution der Aminogruppe, die zu Verbindung 6 führt. Analog reagiert Phenylethinyl-phosphonigsäure-bis(diethylamid), 7, mit Ethan-1,2-dithiol zu Verbindung 8. Cycloaddition und nukleophile Substitution werden jedoch bei der Umsetzung von Acetylen-bis(phosphonigsäurediethylamid), 9, und Ethan-1,2-dithiol beobachtet; es entsteht Verbindung 11. Alle neuen Reaktions-produkte sind durch ihre NMR-, Massen- und IR-Spektren charakterisiert. Von 11 wird eine Kristallstrukturanalyse mitgeteilt.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201009
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  • 16
    Electronic Resource
    Electronic Resource
    1, 2λ5-azaphosphinines and a new 1λ5, 3λ5-. DiphosphinineDedicated to Prof. Shigeru Oae on the occasion of his seventy-fifth birthday. (1995)
    New York, NY [u.a.] : Wiley-Blackwell
    Heteroatom Chemistry 6 (1995), S. 355-363 
    Details
    ISSN: 1042-7163
    Keywords: Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The 1,2-azaphosphinine, 9, and the 1,3-diphosphinine, 10, can be isolated from a mixture resulting from the reaction of 1,1,3,3-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete, 1, and ethyl isothiocyanate. The reaction of 1 with phenyl isothiocyanate yields the 1,2-azaphosphinine, 16. Mechanisms for the formation of the compounds 9, 10, and 16 are suggested. The properties, the NMR, mass, and IR spectra, and the molecular and crystal structures of 9 and 10 are described and discussed.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/hc.520060413
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  • 17
    Electronic Resource
    Electronic Resource
    Die Reaktion von Bis(η5-cyclopentadienyl)(1,2,3-triphenyltriphosphan-1,3-diyl)zirconium(IV), , mit Diazoessigsäureethylester (Cp = η5-C5H5) (1988)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 121 (1988), S. 1207-1211 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The Reaction of Bis(η5-Cyclopentadienyl)(1,2,3-triphenyltriphosphane-1,3-diyl)zirconium(IV), , with Ethyl Diazoacetate (Cp = η5-C5H5)The reaction of bis(η5-cyclopentadienyl) (1,2,3-triphenyltriphosphane-1,3-diyl)zirconium(IV), (1), with ethyl diazoacetate leads to insertion into both Zr—P bonds with formation of (2), which contains the novel 1,2,3-triphenyltriphosphane-1,3-bishydrazonido(2 -) ligand. The 31P-NMR spectrum shows that only the meso isomer of the P3Ph3 fragment is present in solution. The crystal structure analysis shows this, too, as well as the η2-bonding mode of both N,N′ units to the zirconium atom.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19881210630
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  • 18
    Electronic Resource
    Electronic Resource
    Ni-chloralkylierte Nitridochlorokomplexe des Molybdän(VI) [Cl5Mo≡N-R]- mit R = CCl3, C2Cl5 Die Kristallstruktur von (AsPh4)2[(MoOCl4)2CH3CN] (1980)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 460 (1980), S. 191-199 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: N-chloralkyl-nitridochloro Complexes of Molybdenum (VI). [Cl5Mo≡N-R]- with R = CCl3, C2Cl5. Crystal Structure of (AsPh4)2[(MoOCl4)2CH3CN]In the reaction of tetraphenyl arsonium chloride with the complexes Cl3PO—(Cl4)-Mo≡N—R (R=CCl3, C2Cl5) the POCl3 is displaced by chloride and yields [Cl5Mo≡N—R] -. From the i.r. spectra a structure with six-coordinated molybdenum and a Mo≡N triple bond can be deduced. By reaction with water in acetonitrile the molybdenum is reduced to Mo(V) and the nitride ligand is removed yielding (AsPh4)2[(MoOCl4)2CH3CN]. The crystal structure of this compund was determined with X-ray diffraction data. In the tetragonal structure (space group P4/n) AsPh4+ cations and two different anions were found: square pyramidal [MoOCl4]- and [MoOCl4 · NCCH3]- in which the nitrile is bonded in trans position to the oxygen. The short Mo—O distances of 165 pm indicate a strong π-bonding.
    Notes: Die mit POCl3 Solvatisierten N-chloralkylierten Nitride Cl3PO—(Cl4)-Mo≡N—R (R = CCl3 C2Cl5) reagieren mit Tetraphenylarsonuiumchlorid unter Ablösung des POCl3 zu den entsprechenden Chlorokomplexen [Cl5Mo≡N—R] - Nach den IR-Spektren ist das Molybdän sechsfach koordiniert mit einer Mo≡N. Dreifachbindung (lokale Symmetrie C4v). Mit Wasser läßt sich in Acetonitril der Nitridligand ablösen, wobei unter Reduktion zum Mo(V) die Verbindung (AsPh4)2[(MoOCl4)2CH3CN]. entsteht, deren Kristallstruktur mit Hilfe von Röntgenbeugungsdaten bestimmt wurde. Sie kristallisiert tetragonal in der Raumgruppe P4/n. In der Struktur liegen AsPh4+-Kationen und zwei verschiedene Anionen Vor: das quadratisch-pyramidale [MoOCl4]- und das [MoOCI4 · NCCH 3]-, in welchem das Nitril trans-ständig zum sauerstoff gebunden ist. Die kurzen Mo-O-Abstände von 165 pm weisen auf eine starke π-Bindung.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19804600118
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  • 19
    Electronic Resource
    Electronic Resource
    Dichloracetylen als stabiler Komplexligand Die Kristallstruktur von PPh4[WCl5(C2Cl2)] · 0,5 CCl4Professor Josef Goubeau zum 85. Geburtstage am 31. März 1986 gewidmet (1986)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 533 (1986), S. 73-82 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Dichloro Acetylene as Complex Ligand. Crystal Structure of PPh4[WCl5(C2Cl2)] · 0.5 CCl4Tungsten hexachloride and dichloro acetylenediethyletherate react in boiling CCl4 in presence of C2Cl4 as reducing agent forming [Et2O · WCl4(C2Cl2)]. In vacuo the complex looses ether giving the dichloro acetylene complex [WCl4(C2Cl2)]2 which is dimeric with chloro bridges. Both complexes react with tetraphenylphosphonium chloride to form PPh4[WCl5(C2Cl2)] which is equally prepared by ligand exchange of PPh4[WCl5(C2I2)] with silver chloride. All dichloro acetylene complexes are red to brown crystalline solids sensitive to moisture, and are thermally and mechanically very stable compared with the highly explosive dichloro acetylene. The compounds are characterized by their i.r. spectra; [Et2O · WCl4(C2Cl2)] was additionally investigated by 13C-nmr spectroscopy. PPh4[WCl5(C2Cl2)] · 0.5 CCl4 formes dark brown crystals; according to the structural investigation by X-ray diffraction methods the compound crystallizes orthorhombic in the space group Pbca with 8 formula units per unit cell (1317 observed, independent reflexions, R = 0.049). The cell dimensions are a = 1702 pm, b = 1675 pm and c = 2228 pm. The compound consists of [WCl5(C2Cl2)]⊖ anions and PPh4⊕ cations including CCl4 molecules without bonding interactions. The tungsten atoms are seven-coordinated by five chlorine atoms and two carbon atoms. The dichloro acetylene ligand is bonded symmetrically side-on and has a C—C bond length of 128 pm. The W—C distances are 201 pm, the four equatorial Cl atoms have W—Cl bond lengths of 234 pm whereas the chlorine atom in trans-position to the W—C2 group is situated in a distance of 244 pm.
    Notes: Wolframhexachlorid reagiert mit Dichloracetylendiethyletherat bei Anwesenheit von C2Cl4 als Reduktionsmittel in siedendem CCl4 unter Bildung von [Et2O · WCl4(C2Cl2)]. Im Vakuum verliert der Komplex Ether, wobei der über eine Chlorobrücke dimerisierte Dichloracetylenkomplex [WCl4(C2Cl2)]2 entsteht. Mit Tetraphenylphosphoniumchlorid setzen sich beide Verbindungen zu PPh4[WCl5(C2Cl2)] um, zu dem auch Zugang über Ligandenaustausch von PPh4[WCl5(C2I2)] mit Silberchlorid besteht. Alle Dichloracetylenkomplexe sind rote bis braune, feuchtigkeitsempfindliche, kristalline Festkörper, die im Gegensatz zu dem hochexplosiven Dichloracetylen thermisch und mechanisch sehr stabil sind. Die Verbindungen werden durch ihre IR-Spektren charakterisiert; von [Et2O · WCl4(C2Cl2)] wird auch das 13C-Kernresonanzspektrum mitgeteilt. PPh4[WCl5(C2Cl2)] · 0,5 CCl4 kristallisiert mit eingelagertem Tetrachlorkohlenstoff in Form brauner Kristalle. Nach der röntgenographischen Strukturbestimmung kristallisiert die Verbindung in der orthorhombischen Raumgruppe Pbca mit 8 Formeleinheiten pro Elementarzelle (1317 unabhängige, beobachtete Reflexe, R = 4,9%) und mit den Gitterabmessungen a = 1702, b = 1675 und c = 2228 pm. Die Verbindung besteht aus PPh4⊕-Ionen, eingelagerten CCl4-Molekülen ohne bindende Wechselwirkungen und Anionen [WCl5(C2Cl2)]⊖. In ihnen sind die W-Atome siebenfach von fünf Chloratomen und von den beiden C-Atomen des seitwärts symmetrisch gebundenen Dichloracetylenliganden mit einem CC-Abstand von 128 pm koordiniert. Die W--C-Abstände betragen 201 pm, die vier äquatorialen Cl-Atome haben W—Cl-Abstände von 234 pm, während das trans zur WC2-Gruppe gebundene Cl-Atom einen W—Cl-Abstand von 244 pm aufweist.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19865330210
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  • 20
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    Electronic Resource
    Darstellung. IR-Spektrum und Kristallstruktur von AsPh4[WSCI5] (1980)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 467 (1980), S. 89-94 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation, I.R. Spectrum, and Crystal Structure of AsPh4[WSCl5]The title compound is prepared by the reaction WSCl4 with AsPh4Cl in dichloromethane solution. It forms dark green, hygroscopic crystals. The crystal structure determination was solved by X-ray diffraction methods. (R = 3.13%, 826 independent observed reflexions). AsPh4[WSCL5] crystallizes in the tetragonalic space group P4/n with two formula units per unit cell. The structure consists of AsPh4⊕ ions and octahedral [WSCl5]⊖ anions with symmetry C4v; the trans effect of the S ligand is very small. The i.r. spectrum is recorded and discussed with respect to the spectrum of WSCl4; the latter is recorded again.
    Notes: Die Titelverbindung entsteht aus WSCl4 und Tetraphenylarsoniumchlorid in Dichlormethanlösung in Form dunkelgrüner, hygroskopischer Kristalle. Die Kristallstruktur wurde mittels Röntgenbeugung ermittelt und bei 826 unabhängigen, beobachteten Reflexen bis R = 3,13% verfeinert. AsPh4[WSCl5] kristallisiert tetragonal in der Raumgruppe P4/n mit zwei Formeleinheiten pro Elementarzelle. Die Struktur besteht aus AsPh4⊕-Ionen und oktaedrischen [WSCl5]⊖-Anionen der Symmetrie C4v; der trans-Effekt des Thioliganden ist sehr gering. Das IR-Spektrum wird mitgeteilt und im Vergleich zu dem des WSCl5 diskutiert. Das IR-Spektrum von WSCl4 wird neu vermessen.
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    URL: http://dx.doi.org/10.1002/zaac.19804670111
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