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  • Inorganic Chemistry  (28)
  • ACM25/26; ACM25/26_Northwest_2; DATE/TIME; DEPTH, water; MOOR; Mooring; Temperature, water; Temperature recorder, Brancker; WOCE; World Ocean Circulation Experiment
  • Air-sea interaction
  • Marine meteorology
  • 1990-1994  (28)
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  • 11
    Electronic Resource
    Electronic Resource
    Template-Reaktion von Bis(acetylacetonato)-dioxo-molybdän(VI) mit Benzoylhydrazin (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 357-360 
    Details
    ISSN: 0044-2313
    Keywords: Template Reaction ; Benzolhydrazido(2-)-acetylacetonebenzoylhydrazonato(2-)-oxomolybdenum(VI) ; Acetylacetonebenzoylhydrazone ; Mass Spectra ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Template Reaction of Bis(acetylacetonato)-dioxo-molybdenum(VI) with BenzoylhydrazoneBy reaction of bis(acetylacetonato)-dioxo-molybdenum(VI) with benzoylhydrazine benzoylhydrazido(2-)-acetylacetonebenzoylhydrazonato(2-)-oxo-molybdenum(VI) was formed beside another species. The compound was characterized by mass spectrometry and X-ray structural analysis. Crystallographic data see „Inhaltsübersicht“.
    Notes: Als Reaktionsprodukt der Umsetzung von Bis(acetylacetonato)-dioxo-molybdän(VI) mit Benzoylhydrazin in Gegenwart von Triphenylphosphan wurde Benzoylhydrazido-(2-)-acetylacetonbenzoylhydrazonato(2-)-oxo-molybdän(VI) neben einem weiteren Molybdänkomplex erhalten und massenspektrometrisch sowie röntgenkristallstrukturanalytisch charakterisiert. (Raumgruppe Cc, Z = 4, 2 020 beobachtete Reflexe, R = 3,7%. Gitterabmessungen bei 19°C: a = 1 188,5(2) pm, b = 2 110,2(2) pm, c = 813,2(2) pm, β = 105,77(2)°).
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200226
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  • 12
    Electronic Resource
    Electronic Resource
    [W(NPPh3)4]Cl2  -  Ein Phosphaniminato-Komplex mit einem Wolfram-DikationProfessor Heinrich Nöth zum 65. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 999-1003 
    Details
    ISSN: 0044-2313
    Keywords: Phosphoraneiminato 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: [W(NPPh3)4]Cl2  -  a Phosphoraneiminato Complex with a Dication of TungstenThe title compound has been prepared by the reaction of Me3SiNPPh3 with WNCl3 and WO2Cl2, respectively, in acetonitrile, forming colourless crystals, which were characterized by IR spectroscopy and by an X-ray structure determination. Space group P21/n, Z = 4, 4 424 observed unique reflections, R = 0.045. Lattice dimensions at 20°C: a = 1 206.5(2), b = 2 225.3(2), c = 2 421.0(3) pm, β = 101.09(1)°. In the dication [W(NPPh3)4]2+ the tungsten atom is surrounded in a tetrahedral fashion by the four nitrogen atoms of the phosphoraneiminato ligands. The bond lengths WN and PN correspond with double bonds.
    Notes: Die Titelverbindung entsteht durch Reaktion von Me3SiNPPh3 mit WNCl3 bzw. mit WO2Cl2 in Acetonitril in Form farbloser Kristalle, die wir durch das IR-Spektrum und eine röntgenographische Strukturanalyse charakterisiert haben. [W(NPPh3)4]Cl2 kristallisiert monoklin in der Raumgruppe P21/n mit Z = 4 (4 424 beobachtete unabhängige Reflexe, R = 4,5%). Gitterabmessungen bei 20°C: a = 1 206,5(2); b = 2 225,3(2); c = 2 421,0(3) pm; β = 101,09(1)°. In dem Dikation [W(NPPh3)4]2+ ist das Wolframatom tetraedrisch von den vier N-Atomen der Phosphaniminatoliganden umgeben mit WN- und PN-Abständen, die Doppelbindungen entsprechen.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190607
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  • 13
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstruktur von [ReNCl(NPPh2C6H4)]2 · [Ph3PNH2]Cl · CH3CN, einem rheniumorganischen Nitrido-Phosphaniminato-KomplexProfessor Friedrich Hensel zum 60. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1121-1126 
    Details
    ISSN: 0044-2313
    Keywords: Organometallic Nitrido Phosphoraneiminato Complex of Rhenium(VI) ; Synthesis ; X-ray structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of [ReNCl(NPPh2C6H4)]2 · [Ph3PNH2]Cl · CH3CN, a Rhenium Organic Nitrido Phosphoraneiminato ComplexThe title compound is synthesized by the reaction of ReNCl4 with Me3SiNPPh3 in boiling acetonitrile, forming colourless crystals, which are characterized by an X-ray structure determination. Space group P1, Z = 2, 4 037 observed unique reflections, R = 0.043. Lattice dimensions at 19°C: a = 1 005.5; b = 1 695.2; c = 1 744.7 pm, α = 105.86°; β = 101.49°; γ = 104.45°. The structure consists of dimeric molecules [ReNCl(NPPh2C6H4)]2, triphenylphosphorane ammoniumchloride and included acetonitrile molecules. In the nitrido phosphoraneiminato complex the rhenium atoms are μ2-bridged via the N-Atoms of the phosphoraneiminato ligands. Because of this bridging and a Re—Re bond, one terminal nitrido ligand, one terminal chloro ligand, and a Re—C bond of an -C-atom of one phenylene group of Re-atoms attain co-ordination number six.
    Notes: Die Titelverbindung entsteht bei der Reaktion von ReNCl4 mit Me3SiNPPh3 in siedendem Acetonitril in Form farbloser Kristalle, die durch eine röntgenographische Strukturanalyse charakterisiert wurden. Raumgruppe P1, Z = 2, 4 037 beobachtete unabhängige Reflexe, R = 0,043. Gitterabmessungen bei 19°C: a = 1 005,5; b = 1 695,2; c = 1 744,7 pm, α = 105,86°; β = 101,49°; γ = 104,45°. Die Struktur besteht aus dimeren Molekülen [ReNCl(NPPh2C6H4)]2, Triphenylphosphanammoniumchlorid und eingelagerten Acetonitrilmolekülen. In dem Nitrido-Phosphaniminatokomplex sind die Rheniumatome über die N-Atome der Phosphaniminatoliganden μ2-verbrückt. Die Re-Atome erreichen dadurch sowie durch eine Re—Re-Bindung, durch je einen terminalen Nitrido- und Chloroliganden und durch eine Re—C-Bindung eines -C-Atoms einer Phenylengruppe die Koordinationszahl sechs.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190626
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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
    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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  • 16
    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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  • 17
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstrukturen der Nitridodiolato-Osmate(VI) PPh4[OsNCl2(O2C2H4)] und PPh4[OsNCl2(O2C2Me4)] · 2 THF (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 853-858 
    Details
    ISSN: 0044-2313
    Keywords: Nitrido Diolato Osmates(VI) ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Crystal Structures of the Nitridodiolato Osmates(VI) PPh4[OsNCl2(O2C2H4)] and PPh4[OsNCl2(O2C2Me4)] · 2 THFThe title compounds were prepared by the reaction of PPh4[OsNCl4] with glycole and pinacole, respectively, in CH2Cl2 and THF, respectively, in the presence of triethylamine, forming orange-red single crystals. According to the crystal structure determinations the compounds have ionic structures. In the anions the nitrido ligand occupies the apical position of the distorted tetragonal pyramid, and the two chlorine atoms and the two oxygen atoms of the diolato ligands are in equatorial positions.PPh4[OsNCl2(O2C2H4)]: Space group P21/n, Z = 4, 3 331 observed unique reflections, R = 0.031. Lattice dimensions at 19°C: a = 1 750.3, b = 816.8, c = 1 816.5 pm, β = 95.16°.PPh4[OsNCl2(O2C2Me4)] · 2 THF: Space group P1, Z = 2, 5 238 observed unique reflections, R = 0.051. Lattice dimensions at -80°C: a = 898.9, b = 1 405.1, c = 1 518.6 pm, α = 93.66°, β = 92.89°, γ = 92.51°.
    Notes: Die Titelverbindungen entstehen als orangefarbene Einkristalle bei Reaktionen von PPh4[OsNCl4] mit Glykol bzw. mit Pinakol in Dichlormethan bzw. in Tetrahydrofuran in Gegenwart von Triethylamin. Nach den Ergebnissen der Kristallstrukturanalysen haben die Verbindungen ionischen Aufbau. In den Anionen sind die Osmiumatome verzerrt tetragonal von dem Nitridoliganden in der Apicalposition und von zwei Chloratomen und von den zwei Sauerstoffatomen der chelatisierenden Diolatoliganden in den Äquatorialpositionen umgeben.PPh4[OsNCl2(O2C2H4)]: Raumgruppe P21/n, Z = 4, 3 331 beobachtete unabhängige Reflexe, R = 3,1%. Gitterkonstanten bei 19°C: a = 1 750,3; b = 816,8; c = 1 816,5 pm; β = 95,16°.PPh4[OsNCl2(O2C2Me4)] · 2 THF: Raumgruppe P1, Z = 2, 5 238 beobachtete unabhängige Reflexe, R = 5,1%. Gitterkonstanten bei -80°C: a = 898,9; b = 1 405,1; c = 1 518,6 pm; α = 93,66°; β = 92,89°; γ = 92,51°.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190508
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  • 18
    Electronic Resource
    Electronic Resource
    Template-Reaktion von Bis(acetylacetonato)-dioxo-molybdän(VI) mit Benzoylhydrazin und Triphenylphosphan (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 955-958 
    Details
    ISSN: 0044-2313
    Keywords: Template Reactions ; Benzoylhydrazine ; Hydrazide Ligands ; Molybdenum Complexes ; Crystal Structure ; Triphenylphosphane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Template Reactions of Bis(acetylacetonato)-dioxo-molybdenum(VI) with Benzoylhydrazine and TriphenylphosphaneBy reaction of MoO2(acac)2 with C6H5—CO—NH—NH2 in the presence of P(C6H5)3 Mo(NNCOC6H5)((CH3)2CNNCOC6H5)(P(C6H5)) was obtained besides MoO(acac-NNHCOC6H5)(NNHCOC6H5). The earlier compound was characterized by X-ray structural analysis. Crystallographic data see „Inhaltsübersicht“.
    Notes: Bei der Umsetzung von MoO2(acac)2 mit C6H5—CONH—NH2 in Gegenwart von P(C6H5)3 wurde neben MoO(acac-NNHCOC6H5)(NNHCOC6H5) als weitere Substanz Mo(NNCOC6H5)(NNHCOC6H5)((CH3)2CNNCOC6H5) · (P(C6H5)3) erhalten, welche Benzoylhydrazidoliganden in verschiedenen Bindungsformen aufweist. Die Verbindung wurde durch Röntgenkristallstrukturanalyse charakterisiert.Raumgruppe P 21/c, Z = 4, 2 632 beobachtete unabhängige Reflexe, R = 5,9%, Gitterabmessungen bei 19°C: a = 1 583,6(2) pm, b = 1 485,0(2) pm, c = 1 656,1(2) pm, β = 100,79(1)°C.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200535
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  • 19
    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.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946201009
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  • 20
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    Electronic Resource
    Sterisch abgeschirmte Nitridokomplexe von Molybdän und Wolfram Die Kristallstrukturen von [MoN(NPh2)3] und [W4N4(NPh2)6(OnC4H9)2]Professor Josef Goubeau in memoriam (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 593 (1991), S. 99-110 
    Details
    ISSN: 0044-2313
    Keywords: Molybdenum ; Tungsten ; Nitrido Complexes ; Syntheses ; 1H, 13C NMR ; IR Spectra ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Stericly Shielded Nitrido Complexes of Molybdenum and Tungsten. The Crystal Structures of [MoN(NPh2)3] and [W4N4(NPh2)6(OnC4H9)2]The reactions of MoNCl3 and WNCl3, respectively, with lithium diphenylamide in tetrahydrofurane produce the monomeric nitrido complexes MN(NPh2)3 with CN = 4 at the metal atoms. In the presence of lithium-n-butyl LiNPh2 and WNCl3 also form the tetrameric nitrido complex [W4N4(NPh2)6(OnC4H9)2] which contains WV and WVI. The compounds are characterized by their i.r. spectra, by X-ray structural analysis, and, partially, by 1H and 13C n.m.r. spectroscopy.MoN(NPh2)3: Space group P1, Z = 2, 4060 observed independent reflexions, R = 0.031. Lattice dimensions at 20°C: a = 956.2(4) pm, b = 1 015.9(2) pm, c = 1 598.1(3) pm; α = 79.06(2)°, β = 85.67(3)°, γ = 82.57(3)°. The compound forms monomeric molecules with Mo≡N bond lengths of 163.4 pm and mean Mo—NPh2 distances of 199.2 pm.[W4N4(NPh2)6(OnC4H9)2]: Space group P21/n, Z = 2, 1903 observed independent reflexions, R=0.039. Lattice parameters at 19°C: a = 1582.2(3) pm, b = 1182.4(2) pm, c = 2053.3(4) pm; β = 103.77(2)°. The compound forms centrosymmetric molecules, in which the central W-W dumb-bell (bond length 253.5 pm) is linked by the nitrido ligands of two WN2(NPh2)2=units in a T shaped order of the N-atoms.
    Notes: Die Umsetzungen von MoNCl3 bzw. WNCl3 mit Lithium-Diphenylamid in Tetrahydrofuran führen zu den monomeren Nitridokomplexen MN(NPh2)3 mit KZ = 4 an den Metallatomen. Bei Anwesenheit von Lithium-n-butyl reagiert LiNPh2 mit WNCl3 auch zu dem tetrameren, Wolfram(V) und Wolfram(VI) enthaltenden Nitridokomplex [W4N4(NPh2)6(OnC4H9)2]. Die Verbindungen werden durch ihre IR-Spektren, zum Teil durch die 1H- und 13C-Kernresonanzspektren sowie durch Röntgenstrukturanalysen charakterisiert.MoN(NPh2)3: Raumgruppe P1, Z = 2, 4060 unabhängige beobachtete Reflexe, R = 3,1%. Gitterabmessungen bei 20°C: a = 956,2(4); b = 1015,9(2); c = 1598,1(3) pm; α = 79,06(2)°; β = 85,67(3)°; γ = 82,57(3)°. Die Verbindung bildet monomere Moleküle mit Bindungslängen Mo≡N 163,4 pm und Mo—NPh2 von im Mittel 199,2 pm.[W4N4(NPh2)6(OnC4H9)2]: Raumgruppe P21/n, Z = 2, 1903 beobachtete unabhängige Reflexe, R = 3,9%. Gitterabmessungen bei 19°C: a = 1 582,2(3); b = 1 182,4(2); c = 2 053,3(4) pm; β = 103,77(2)°. Die Verbindung bildet zentrosymmetrische Moleküle, deren zentrale W - W-Hantel (Bindungslänge 253,5 pm) über die Nitridoliganden zweier WN2(NPh2)2-Einheiten mit T-förmiger Anordnung der N-Atome verknüpft ist.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19915930110
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