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  • Electronic Resource  (44)
  • Inorganic Chemistry  (44)
  • 1,4,2λ5,5λ5-Dioxadiphosphorinane  (2)
  • 1
    Electronic Resource
    Electronic Resource
    Metallorganische CO2-Speichersysteme aus Nickel(0)-1-azadieneinheiten und ihre Reaktivität bei der Carboxylierung von Acetophenon (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 281-287 
    Details
    ISSN: 0009-2940
    Keywords: Carbon dioxide fixation ; 1-Azadiene ligands ; Nickel(0) complexes ; Carboxylation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Organometallic CO2 Reservoires from Nickel(0)-1-Azadiene-Type Ligands and Their Reactivity in the Carboxylation of Acetophenone1-Azadiene-type ligands yield with nickel(0) binuclear organometallic compounds of the type [Ni(1-azadiene)n,]2 (n = 1, 2). The structures of the complexes 1 (n = 2, ligand A) and 3 (n = 1, ligand C) have been characterized by X-ray crystallography. 1 is unreactive towards CO2, 3 and similar compounds are able to react with CO2 to give metallacyclic carbamato complexes of Ni(II). In these compounds CO2 is activated and can carboxylate acetophenone to yield benzoylic acid upon protolysis. These reactions mimic biologic conversion reactions of CO2 into organic material by organometallics. - The addition of two moles of the (bpy)Ni(0)-fragment [from (bpy)Ni(COD)] to 3 gives the tetranuclear complex 6. The X-ray analysis of the monomeric model compound (bi-py)Ni(A) (11) shows that only the olefin part is coordinated. 6 and 11 can also react with CO2. Cu(I) complexes with 1-azadiene-type ligands are not reactive towards CO2.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280312
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  • 2
    Electronic Resource
    Electronic Resource
    P,P′-(2,5-Dihydroxy-3,6-dimethyl-2,5-dioxo-2λ5,5λ5-[1,4,2,5]-dioxadiphosphinan-2,5-diyl)-bis-phosphonsäure (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1799-1804 
    Details
    ISSN: 0044-2313
    Keywords: 1,4,2λ5,5λ5-Dioxadiphosphorinane ; NMR spectra ; Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: P,P′-(2,5-Dihydroxy-3,6-dimethyl-2,5-dioxo-2λ5,5λ5-[1,4,2,5]dioxadiphosphinane-2,5-diyl)-bis-phosphonic AcidThe tetrahydrate 1 of the title compound crystallizes in the monoclinic space group P21/c with a = 845.8, b = 1 098, c = 981.7 pm, β = 113.02° and Z = 2. The anions of the oxonium compound (H3O+ · H2O)2(C4H10O12P42-) are layered by hydrogen bridges. The 1H, 13C and 31P NMR spectra (4 and 5 spin systems) are discussed.
    Notes: C4H12O12P4 · 4 H2O (1), das Tetrahydrat der Titelverbindung, kristallsiert monoklin in der Raumgruppe P21/c mit a = 845,8, b = 1 098, c = 981,7 pm, β = 113,02° und Z = 2. 1 liegt als Oxoniumsalz (H3O+ · H2O)2(C4H10O12P42-) vor, in dem die Anionen über H-Brücken zu Schichten verknüpft sind. Die 4- und 5-Spinsysteme der 1H-, 13C- und 31P-NMR-Spektren werden detailliert analysiert.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946201023
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  • 3
    Electronic Resource
    Electronic Resource
    P,P′-(2,5-Dimethoxy-3,6-dimethyl-2,5-dioxo-2λ5,5λ5-[1,4,2,5]dioxadiphosphinan-2,5-diyl)-bis-phosphonsäuretetramethylesterNomenklatur nach Beilstein. Nach Chem. Abstr.: P,P′-(2,5-Dimethoxy-3,6-dimethyl-1,4,2,5-dioxadiphosphorinan-2,5-diyl)bis[phosphonic acid tetramethylester]-2,5-dioxide (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1063-1068 
    Details
    ISSN: 0044-2313
    Keywords: 1,4,2λ5,5λ5-Dioxadiphosphorinane ; NMR-Spectra ; Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: P,P′-(2,5-Dimethoxy-3,6-dimethyl-2,5-dioxo-2λ5,5λ5-[1,4,2,5]dioxadiphosphinane-2,5-diyl)-bis-phosphonic acid tetramethylesterThe title compound 1 is formed by reaction of the corresponding phosphonic acid 2 and orthoformicacidmethylester as a mixture of four stereoisomeres. The RRSS isomer was separated. It crystallizes in the triclinic space group P -1 with a = 649.2 pm, b = 976.1 pm, c = 1 571.7 pm, α = 80.9°, β = 88.1°, γ = 78.6° and Z = 2. The 31P and 13C NMR spectra (4 and 5 spin systems) are discussed.
    Notes: Die Titelverbindung 1 entsteht aus der zugrundeliegenden Phosphonsäure 2 und Orthoameisensäuremethylester als Gemisch aus vier Stereoisomeren, von denen das RRSS-Isomer präparativ abgetrennt werden konnte. Dieses kristallisiert triklin in der Raumgruppe P -1 mit a = 649,2 pm, b = 976,1 pm, c = 1 571,7 pm, α = 80,9°, β = 88,1°, γ = 78,6° und Z = 2. Die 4- und 5-Spinsysteme der 31P- und 13CNMR-Spektren werden analysiert.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956210629
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  • 4
    Electronic Resource
    Electronic Resource
    Sulfoximid und Sulfoximidium-Salze - Strukturen und H—Brückenbindungen (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1168-1174 
    Details
    ISSN: 0044-2313
    Keywords: Sulfoximide ; Sulfoximidium Salts ; Structure ; Hydrogenbonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Sulfoximide and Sulfoximidium Salts - Structures and Hydrogen BondingIn the solid state dimethylsulfoximide (1) (orthorhombic; space group Pbca; a = 577.8, b = 931.2 and c = 1645.6 pm) makes intermolecular N—H ≡ N hydrogen bonds. The hydrogen halide salts (CH3)2S(O)NH2+Hal- ((2), Hal-=Cl-; (4), Hal-=Br-) reacts with metal halides to yield (CH3)2S(O)NH2+MHalyn- with the complex anions ((5), MHalyn-=SbCl4-; (6), MHalyn-=SbCl52-; (7), MHalyn-=SbCl6-; (8), MHalyn-=SbBr52-; (9), MHalyn-=AlCl4-). 2 crystallizes from ethanol (96%) as [(CH3)2S(O)NH2+Cl-]2 · H2O (3). The structures of 3 (monoclinic; space group P21/c; a = 917.0, b = 1344.7, c = 1080.8 pm and β = 103.8°; Z = 10), 4 (orthorhombic; space group Pbcn; a = 1028.9, b = 1132.6, c = 1074.1 pm; Z = 8) and 6 (monoclinic; space group C2/c; a = 2041.1, b = 1101.4, c = 3365.6 pm and β = 153.8°; Z = 8) are determined by X-ray analysis. In 6 Sb is coordinated in a distorted octahedra by 6 Cl in three short (mean 245,5 pm; SbCl3) and three long distances (291 to 299 pm; Cl-). Two of the chloride ions connect the Sb atoms to infinite Sb … Cl … Sb chains. Except for 7 and 9 there are bridges between the NH2 groups and the halide ions. The NH valence vibrations are discussed in view of hydrogen bonding.
    Notes: Im festen Dimethylsulfoximid (1) (orthorhombisch; Raumgruppe Pbca; a = 577,8, b = 931,2 und c = 1645,6 pm) sind zwischen den Imidgruppen N—H … N-Brückenbindungen ausgebildet. Die mit HHal darstellbaren Salze (CH3)2S(O)NH2+Hal- ((2), Hal-=Cl-; (4), Hal-=Br-) reagieren mit MHalx zu (CH3)2S(O)NH2+MHalyn- ((5), MHalyn-=SbCl4-; (6), MHalyn-=SbCl52-; (7), MHalyn-=SbCl6-; (8), MHalyn-=SbBr52-; (9), MHalyn-=AlCl4-). 2 kristallisiert aus 96% Ethanol als [(CH3)2S(O)NH2+Cl-]2 · H2O (3). Die Strukturen von 3 (monoklin; Raumgruppe P21/c; a = 917,0, b = 1344,7, c = 1080,8 pm und β = 103,8°; Z = 10), 4 (orthorhombisch; Raumgruppe Pbcn; a = 1028,9, b = 1132,6, c = 1074,1 pm; Z = 8) und 6 (monoklin; Raumgruppe C2/c; a = 2041,1, b = 1101,4, c = 3365.6 pm und β = 153,8°; Z = 8) wurden bestimmt. In 6 ist Sb verzerrt oktaedrisch von 6 Cl in drei kurzen (im Mittel 245,5 pm; SbCl3) und drei langen Abständen (291 bis 299 pm; Cl-) umgeben. Zwei der lang gebundenen Cl-Ionen verknüpfen die Sb-Atome zu unendlichen Sb … Cl … Sb-Ketten. Die NH2-Gruppen der Kationen bilden außer in 7 und in 9 H—Brückenbindungen zu den Halogenidionen. Die NH-Valenzschwingungen werden im Hinblick auf die Wasserstoffbrückenbindungen diskutiert.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230727
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  • 5
    Electronic Resource
    Electronic Resource
    Dimethylammonium-chloroantimonate. Struktur und Schwingungsspektren (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 557 (1988), S. 208-218 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Dimethylammonium Chloroantimonates. Structure and Vibrational SpectraTetrakis(dimethylammonium)-chloride-hexachloroantimonate(III) (3) and the N-deuterated compound 4 were prepared. The structure of 3 was determined by X-Ray analysis. There are discrete chloride and distorted octahedral hexachloroantimonate(III) ions hydrogen bonded to the cations. The vibrational spectra of 3 and 4 are compared with those of the related nonachlorodiantimonate(III) (1), the pentachloroantimonate(III) (2), and two other hexachloroantimonates(III), and the spectral range of the NH and SbCl vibrations is discussed.
    Notes: Das Tetrakis(dimethylammonium)-chlorid-hexachloroantimonat(III) (3) sowie das N-deuterierte Analoga (4) wurden dargestellt. Die Struktur von 3, die durch Röntgenstrukturanalyse ermittelt wurde, besteht aus diskreten Chlorid- und verzerrt oktaedrischen Hexachloroantimonat(III)-Anionen, die über H-Brückenbindungen mit den Kationen verknüpft sind. Die Schwingungsspektren von 3 und 4 werden mit denen des entsprechenden Nonachlorodiantimonats(III) (1), des Pentachloroantimonats(III) (2) sowie zweier weiterer Hexachloroantimonate(III) verglichen, und im Bereich der NH- und SbCl-Valenzschwingungen diskutiert.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885570122
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  • 6
    Electronic Resource
    Electronic Resource
    Dimethyldithiocarbamatoarsane und -stibane (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 539-544 
    Details
    ISSN: 0044-2313
    Keywords: Ionic arsen- and antimony(III)-dithiocarbamates ; synthesis ; vibrational and mass spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Dimethyldithiocarbamatoarsanes and -stibanesThe Halogeno-bis(dimethyldithiocarbamato)-compounds (dtc)2AsCl 1, (dtc)2AsBr 2, (dtc)2AsI 3 and (dtc)2SbI 4 are prepared from (dtc)3As and (dtc)3Sb resp. Reaction of 1 to 4 with CF3SO3Sime3 yields the ionic compounds (dtc)2As+CF3SO3- 5 and [(dtc)2El+]2Hal-(CF3SO3-) · CH2Cl2 6 (El = As; Hal = I), 7 (El = Sb; Hal = I) and 8 (El = As; Hal = Br) resp. by elimination of me3SiHal. The mass spectra and the main fragmentation from 1 to 8 are reported. The vibrational spectra of these compounds, of As(dtc)3, Sb(dtc)3 and of the antimony compounds which are corresponding to 6 and 8 are discussed.
    Notes: Die Synthese der Halogeno-bis(dimethyldi-thiocarbamato)-Verbindungen (dtc)2AsCl 1, (dtc)2AsBr 2, (dtc)2AsI 3 und (dtc)2SbI 4 aus (dtc)3As bzw. (dtc)3Sb wird beschrieben. Umsetzungen von 1 bis 4 mit CF3SO3Sime3 führen unter me3SiHal-Abspaltung zu den salzartigen Verbindungen (dtc)2As1CF3SO3 5 bzw. [(dtc)2El1]2Hal (CF3SO3) · CH2Cl2 6 (El = As; Hal = I), 7 (El = Sb; Hal = I) und 8 (El = As; Hal = Br). Die Massenspektren und die Hauptzerfallswege von 1 bis 8 werden mitgeteilt. Die Schwingungsspektren von 1 bis 8, As(dtc)3, Sb(dtc)3 sowie den 6 und 8 entsprechenden Antimonverbindungen werden diskutiert.
    Additional Material: 7 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200326
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  • 7
    Electronic Resource
    Electronic Resource
    Zum chemischen Transport von Cobaltmonophosphid mit Iod. Experimente und Modellrechnungen (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1693-1702 
    Details
    ISSN: 0044-2313
    Keywords: Cobalt monophosphide ; chemical transport ; thermochemical calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Chemical Vapour Transport of Cobalt Monophosphide using Iodine. Experiments and Thermochemical Model CalculationsCoP can be crystallized by chemical vapour transport using iodine as transport agent. Over a wide temperature range (650°C ≤ T̄ ≤ 1000°C; T̄ = (T1 + T2)/2; ΔT = 100 K) the migration from the higher to the lower temperature is based on the heterogeneous equilibrium \documentclass{article}\pagestyle{empty}\begin{document}$$ {\rm CoP}_{\rm s} + 5/2{\rm I}_{2,{\rm g}} = {\rm CoI}_{2,{\rm g}} + {\rm PI}_{3,{\rm g}}. $$\end{document} CoI2,l is observed as second condensed equilibrium phase besides CoPs in experiments carried out at lower mean temperatures (T̄ ≤ 800°C) and with sufficiently high amounts of iodine. Thermochemical model calculations, based on modified data for CoI2,l, CoI2,g and Co2I4,g, reproduce the observed deposition rates as well as the compositions of the condensed equilibrium phases. These calculations allow a detailed description of the equilibrium gas phase in the system Co/P/I under variable experimental conditions. The influence of traces of moisture on the transport behavior will be discussed.
    Notes: CoP ist bei hinreichender Zugabe von Iod als Transportmittel über einen großen Temperaturbereich (650°C ≤ T̄ ≤ 1000°C; T̄ (T1 + T2)/2, ΔT = 100 K) aufgrund endothermer Reaktionen transportierbar. Zentrale Bedeutung für die Wanderung des Cobaltmonophosphids hat das heterogene Gleichgewicht \documentclass{article}\pagestyle{empty}\begin{document}$$ {\rm CoP}_{\rm s} + 5/2{\rm I}_{2,{\rm g}} = {\rm CoI}_{2,{\rm g}} + {\rm PI}_{3,{\rm g}}. $$\end{document} Bei niedrigen Transporttemperaturen (T̄ ≤ 800°C) und genügend hohen Transportmitteldichten (D ≥ 7,5 mg · cm-3) liegt CoI2,l neben CoP in der Senke vor. Thermodynamische Modellrechnungen zum chemischen Transport von CoP mit Iod unter Verwendung überarbeiteter thermodynamischer Daten für CoI2,l, CoI2,g und Co2I4,g geben die beobachteten Phasenverhältnisse im Bodenkörper sowie die Transportraten für CoP gut wieder. Detaillierte Aussagen zur Zusammensetzung der Gleichgewichtsgasphase sind möglich. Der Einfluß von Feuchtigkeitsspuren auf das Transportverhalten wird erörtert.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956211014
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  • 8
    Electronic Resource
    Electronic Resource
    (CH3)2SBr2 - einige Reaktionen und Strukturen (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1633-1638 
    Details
    ISSN: 0044-2313
    Keywords: (CH3)2S derivatives ; Structure ; Spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: (CH3)2SBr2 - Reactions and Structures(CH3)2SBr2 (1) is a donor acceptor complex (8-S-3 + 10-Br-2) which reacts with (CH3)2S(=O)NSi(CH3)3 to yield [(CH3)2S(O)=N—S(CH3)2]+Br- (2). With SbBr3 (CH3)2SBr+SbBr4- (3) can be isolated. 1 crystallizes monoclinic in the space group P21/c with a = 733.8, b = 734.2, c = 1132.7 pm, β = 92.8° and Z = 4. 2 crystallizes in the orthorhombic space group Pnma with a = 967.2, b = 793.3, c = 1168.3 pm and Z = 4. The SBr and BrBr force constants of 1 are compared with those of S2Br2, 3 and Br2 resp. The nmr and mass spectra of 1 and 2 are communicated.
    Notes: (CH3)2SBr2 (1) ist ein (8-S-3 + 10-Br-2) Donor-Akzeptor-Komplex(8-S-3 + 10-Br-2) bedeutet: acht Valenzelektronen am S-Atom, das von drei Bindungspartnern umgeben ist, und zehn Valenzelektronen am Br-Atom, das zwei Bindungspartner hat; s.: S. W. Perkins, J. C. Martin, A. J. Arduengeo III, W. Lau, A. Alegria, J. K. Kochi, J. Am. Chem. Soc. 1980, 102, 7753. und reagiert mit (CH3)2S(=O)NSi(CH3)3 zu [(CH3)2S(O)=N—S(CH3)2]+Br- (2), mit SbBr3 zu (CH3)2SBr+SbBr4- (3). 1 kristallisiert monoklin (P21/c) mit a = 733,8, b = 734,2, c = 1132,7 pm, β = 92,8° und Z = 4. 2 kristallisiert orthorhombisch in der Raumgruppe Pnma mit a = 967,2, b = 793,3, c = 1168,3 pm und Z = 4. Die SBr- und BrBr-Kraftkonstanten von 1 werden mit denen von S2Br2 und 3 bzw. Br2 verglichen. Die NMR- und Massenspektren von 1 und 2 werden kurz diskutiert.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976231025
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  • 9
    Electronic Resource
    Electronic Resource
    Antimon(III)-butoxo-Verbindungen (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 35-38 
    Details
    ISSN: 0044-2313
    Keywords: Antimony(III)-butoxo compounds ; syntheses ; vibrational spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Antimony(III)-butoxo CompoundsTri(tert.-butoxo)stiban 1 reacts with antimony(III) chloride dependent from the molar ratio to yield Sb(OtBu)2Cl 2 and Sb4Cl7O(OtBu)3 3 resp ‥ 3 are discrete molecules with a cage structure. 2 is associated by oxygen bridges. The vibrational spectra of 1-3 are assigned.
    Notes: Tri(tert.-butoxo)stiban 1 reagiert mit Antimon(III)-chlorid in Abhängigkeit von der Stöchiometrie unter Bildung von Sb(OtBu)2Cl 2 bzw. Sb4Cl7O(OtBu)3 3. 3 besteht aus diskreten Molekülen mit Käfigstruktur. 2. ist über O-Brückenbindungen hochassoziiert. Die Schwingungsspektren von 1-3 werden zugeordnet.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926090306
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  • 10
    Electronic Resource
    Electronic Resource
    Trichloroantimon(V)-methylphosphonat (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 2029-2033 
    Details
    ISSN: 0044-2313
    Keywords: Tetranuclear antimony(V) complex ; structure ; NMR, IR, Raman, mass spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Trichloroantimony(V) MethylphosphonateThe tetrameric trichloroantimony(V) methylphosphonate (1) is synthezised by reaction of antimony(V) chloride and methanephosphonic acid. It crystallizes monoclinic in the space group P21/a with a = 1 813.6 pm, b = 1 024.0 pm, c = 1 831.1 pm, β = 100.5° and Z = 4. In the unit cell there are chiral molecules which lose their chirality in solution. In solution they are dynamical and have an other conformation as in the solid state. The NMR, vibrational and mass spectra are discussed.
    Notes: Tetrameres Trichloroantimon(V)-methylphosphonat (1) entsteht aus Antimon(V)chlorid und Methanphosphonsäure. Es kristallisiert monoklin in der Raumgruppe P21/a mit a = 1 813,6 pm, b = 1 024,0 pm, c = 1 831,1 pm, β = 100,5° und Z = 4. In der Einheitszelle liegt 1 in Form spiegelbildlicher Moleküle vor, die in Lösung ihre Chiralität verlieren und eine andere Konformation als im Feststoff haben. Die NMR-, Schwingungs- und Massenspektren werden diskutiert.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956211209
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