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  • 1
    ISSN: 0044-2313
    Keywords: Tetraalkyl phosphonium triiodide ; tetraalkyl arsonium triiodide ; tetraalkyl stibonium triiodide ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Crystal Structure Analyses of Tetraalkyl Phosphonium, Arsonium, and Stibonium TriiodidesThe reaction of Me4EI (E=P, As), Me3EtSbI, Me2Et2SbI, MeEt3SbI, or Et4SbI with I2 in absence of solvent gives Me4PI3 (E=P, As), Me3EtSbI3, Me2Et2SbI3, MeEt3SbI3, or Et4SbI3. Me4SbI3 is formed in a reversible reaction by addition of I2 to (Me4Sb)3I8 or by reaction of a solution of Me4SbI in ethanol with I2 in benzene. The crystal structures of Me4EI3 (E=P, Sb), and Me3EtSbI3 and the syntheses of the novel compounds are reported.
    Notes: Die Reaktion von Me4EI (E=P, As), Me3EtSbI, Me2Et2SbI, MeEt3SbI oder Et4SbI mit I2 im Substanzgemisch ohne Lösungsmittel führt zu den entsprechenden Triiodiden Me4EI3 (E=P, As), Me3EtSbI3, Me2Et2SbI3, MeEt3SbI3 oder Et4SbI3. Me4SbI3 entsteht in reversibler Reaktion durch Zugabe von I2 zu (Me4Sb)3I8 oder durch Umsetzung einer ethanolischen Lösung von Me4SbI mit einer Lösung von Iod in Benzol. Über die Kristallstrukturen von Me4EI3 (E=P, Sb) und Me3EtSbI3 und die Synthese der neuen Verbindungen wird berichtet.
    Additional Material: 4 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 446 (1978), S. 119-125 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Diphenyl(trimethylmetall)stibines and Bis(diphenylstibido)dimethyl MetalsDiphenyllithiumantimonide, which is prepared by fission of triphenylstibine with lithium, reacts with the organometal halides Me3MCl and Me2MCl2 under elimination of LiCl and yields the organometal stibines Ph2SbMMe3, M = Si 1, Ge 2, Sn 3, and (Ph2Sb)2MMe2. M = Si 5, Ge 6, Sn 7. The corresponding reaction with 2,2-dichloropropane yields (Ph2Sb)2CHe2 4. The main products of the reaction of Ph2SbNa and Me3SnCl are (Me3Sn)2 and (Ph2Sb)2. The i.r., n.m.r., and mass spectra data of the new compounds as well as some of their reactions are communicated.
    Notes: Aus Triphenylstibin und Lithium hergestelltes Lithiumdiphenylantimonid reagiert mit den Organometallhalogeniden Me3MCl und Me2MCl2 unter LiCl-Abspaltung zu den Organometallstibinen Ph2SbMMe3, M = Si 1, Ge 2, Sn 3, und (Ph2Sb)2MMe2, M = Si 5, Ge 6, Sn 7. Die entsprechende Umsetzung mit 2,2-Dichlorpropan führt zu (Ph2Sb)2CMe2 4. Die Reaktion von Ph2SbNa mit Me3SnCl in flüssigem NH3 ergibt bevorzugt (Me3Sn)2 und (Ph2Sb)2. IR-, NMR- und MS-Daten der neuen Verbindungen sowie einige ihrer Reaktionen werden mitgeteilt.
    Additional Material: 5 Tab.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 445 (1978), S. 215-218 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Binuclear Metal Carbonyl Complexes with Tetraalkyldistibane and Bis(diphenylstibino)-methane LigandsTetramethyldistibane 1, tetraethyldistibane 2 and bis(diphenylstibino)methane 3 react with photochemically generated solutions of pentacarbonyl(tetrahydrofuran)chromium and -tungsten. Thereby the binuclear complexes (Co)5MSbR2SbR2M(CO)5 (M = Cr, W; R = CH3,C2H5) and (CO)5CrSb(C6H5)2CH2Sb(C6H5)2Cr(CO)5 are formed.
    Notes: Tetramethyldistiban 1, Tetraethyldistiban 2 und Bis(diphenylstibino)-methan 3 reagieren mit photochemisch erzeugten Lösungen von Pentacarbonyl(tetrahydrofuran)-chrom und -wolfram zu den Zweikernkomplexen (Co)5MSbR2SbR2M(CO)5 (M = Cr, W; R = CH3,C2H5) sowie (Co)5CrSb(C6H5)2CH2Sb(C6H5)2Cr(CO)5.
    Additional Material: 5 Tab.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 502 (1983), S. 175-177 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Formation and Mass Spectrum of Penta-tert-butyl-cyclopentastibane(t-BuSb)5 (1) is formed together with known (t-BuSb)4 by reduction of t-BuSbCl2 with Mg in tetrahydrofuran. 1 was preparatively concentrated to 60 mole-% and characterized by its 1H-nmr and mass spectrum.
    Notes: (t-BuSb)5 (1) entsteht neben dem bekannten (t-BuSb)4 bei der Reduktion von t-BuSbCl2 mit Mg in Tetrahydrofuran. 1 wurde präparativ auf etwa 60 Mol-% angereichert und durch das 1H-NMR- und das Massenspektrum charakterisiert.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 487 (1982), S. 111-118 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Vibrational Spectra of Tetramethyl-, Tetraethyl-, and TetraphenyldistibaneThe infrared spectra of liquid tetramethyldistibane from 4 000 to 20 cm-1, of liquid tetraethyldistibane and solid tetraphenyldistibane as well as the Raman spectra of liquid Me4Sb2 at 25 to 100° including the depolarisation values of the bands, of solid Me4Sb2 at 0°, of liquid Et4Sb2 and solid Ph4Sb2 are reported. Based on positions, relative intensities and polarisation values of the bands assignments are made, which include proposals for the positions of the Sb—Sb valence frequencies. In the case of Me4Sb2 it is possible to assign two frequencies, in the case of Et4Sb2 and Ph4Sb2 only one frequency to ν Sb—Sb. This corresponds to the presence of gauche and trans conformers in Me4Sb2 and of only one conformer in Et4Sb2 and Ph4Sb2.
    Notes: Die Infrarotspektren von flüssigem Tetramethyldistiban von 4 000 bis 20 cm-1, von flüssigem Tetraethyldistiban und von festem Tetraphenyldistiban von 4 000 bis 200 cm-1 sowie die Ramanspektren von flüssigem Me4Sb2 bei 25 bis 100° mit Angabe des Polarisationsgrades der Banden, von festem Me4Sb2 bei 0°, von flüssigem Et4Sb2 und festem Ph4Sb2 werden mitgeteilt. Aufgrund der Lage, der relativen Intensitäten und des Polarisationsgrades der Banden werden Zuordnungen getroffen, die Vorschläge für die Lage der Sb—Sb-Valenzschwingungen einschließen. Hierfür kommen im Fall von Me4Sb2 zwei, im Fall von Et4Sb2 und Ph4Sb2 nur eine Frequenz in Frage. Dies entspricht dem Vorliegen von gauche- und trans-Konformeren bei Me4Sb2 und nur eines Konformeren bei Et4Sb2 und Ph4Sb2.
    Additional Material: 4 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 510 (1984), S. 104-108 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Trialkylbismutines as Ligands in Carbonyl Complexes of Iron and Group VIa ElementsThe complexes (CO)4FeBiR3 (R = Et, Pr, Bu) are synthesized by reaction of Fe2(CO)9 and the corresponding bismutines. Complexes of the type Bu3BiM(CO)5 (M = Cr, Mo, W) are formed by irradiation of the hexacarbonyls of group VIa elements in tetrahydrofuran and subsequent addition of Bu3Bi. The novel compounds are obtained in 40 - 90% yield. They are stable in an inert atmosphere above 25°C. Their 1H-n. m. r., i. r., and m. s. data are discussed.
    Notes: Die Komplexe (CO)4FeBiR3 (R = Et, Pr, Bu) werden durch Umsetzung von Fe2(CO)9 mit den entsprechenden Bismutinen synthetisiert. Komplexe des Typs Bu3BiM(CO)5 (M = Cr, Mo, W) entstehen durch Bestrahlung der Hexacarbonyle der VIa-Elemente in Tetrahydrofuran und nachfolgende Umsetzung mit Bu3Bi. Die neuen Verbindungen werden in 40 - 90% Ausbeute erhalten. Sie sind bei Luftausschluß auch oberhalb von 25°C stabil. Ihre 1H-NMR-, IR- und EI-MS-Daten werden diskutiert.
    Additional Material: 2 Tab.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 454 (1979), S. 167-174 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Spectroscopic Investigations of Mono- and Binuclear Metalcarbonyl Complexes of Tetraalkyldistibane and Tetraphenyldistibane LigandsThe reactions of photochemically generated solutions of pentacarbonyl (tetrahydrofurane)chromium and -tungsten with tetramethyldistibane 1, tetraethyldistibane 2, tetra-tert-butyldistibane 3, and tetraphenyldistibane 4 yield mononuclear complexes (OC)5M—SbR2SbR2 (5; M = Cr, W; R = CH3, C2H5, C6H5) and binuclear complexes (OC)5M—SbR2SbR2—M(CO)5 (6; M = Cr, W; R = t-C4H9, C6H5). The chemical and spectroscopic properties of these compounds are discussed.
    Notes: Aus photochemisch erzeugten Lösungen von Pentacarbonyl(tetrahydrofuran)-chrom und -wolfram bilden sich mit Tetramethyldistiban 1, Tetraethyldistiban 2, Tetra-tertbutyldistiban 3 und Tetraphenyldistiban 4 einkernige Komplexe des Typs (OC)5M—SbR2SbR2 (5; M = Cr, W; R = CH3, C2H5, C6H5) sowie zweikernige Komplexe (OC)5M—SbR2SbR2—M(CO)5 (6; M = Cr, W; R = t-C4H9, C6H5). Die chemischen und spektroskopischen Eigenschaften dieser Verbindungen werden diskutiert.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 477 (1981), S. 119-125 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Reactions of μ-Distibane- and Di-μ-antimonido-bridged Metalcarbonyl Complexes of Chromium, Molybdenum, and TungstenBy irradiation of hexacarbonylmolybdenum in tetrahydrofuran solutions are produced, which react with tetramethyl-, -ethyl-, and -phenyldistibane to yield the complexes (CO)5MoSbR2SbR2Mo(CO)5, R = Me, Ph and (CO)4Mo(SbR2)2Mo(CO)4, R = Me, Et, Ph.(CO)4W(SbPh2)2W(CO)4 is a product of the thermal reaction of hexacarbonyltungsten and tetraphenyldistibane. Cleavage of (CO)5CrSbMe2SbMe2Cr(CO)5 with bromine yields (CO)5CrSbMe2Br.
    Notes: Durch Bestrahlen von Hexacarbonylmolybdän in Tetrahydrofuran erzeugte Lösungen reagieren mit Tetramethyl-, -ethyl- und -phenyldistiban zu den Komplexen (CO)5MoSbR2SbR2Mo(CO)5, R = Me, Ph und (CO)4Mo(SbR2)2Mo(CO)4, R = Me, Et, Ph.(CO)4W(SbPh2)2W(CO)4 entsteht thermisch aus Hexacarbonylwolfram und Tetraphenyldistiban. Die Spaltung von (CO)5CrSbMe2SbMe2Cr(CO)5 mit Brom ergibt (CO)5CrSbMe2Br.
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 486 (1982), S. 70-89 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Element-Element Bonds. I. Syntheses and Structure of Tetra(tert-butyl)tetrarsetane and of Tetra(tert-butyl)tetrastibetaneDilithium (tert-butyl)arsenide reacts with (tert-butyl)dichloroarsine to give tetra-(tert-butyl)tetrarsetane 1; homologous tetra(tert-butyl)tetrastibetane 2 is formed by reduction of (tert-butyl)dichlorostibane with magnesium. The isotypic compounds 1/2 crystallize in the monoclinic space group P21/c with Z = 4. The dimensions of the unit cells determined at -45 ± 5°C are: a = 957.4(8)/1 000.2(3); b = 1 399.1(14)/1 423.9(4); c = 1 697.4(9)/1 749.8(7) pm; β = 96.02(6)/96.77(3)°. As shown by low temperature X-ray structure determinations (3 531/3 232 symmetry independent reflections; Rg = 4.0/4.6%) the four membered rings E4 (E = As or Sb) are folded; in all-trans configuration the bulky organic substituents occupy pseudo-equatorial positions. Characteristic averaged bond distances and angles are: E—E 244/282; E—C 202/221 pm; ∢ E—E—E 86/85° ∢ E—E—C 101/99°. The dihedral angels of the bisphenoides built up by the atoms of the rings are found to be 139/133°.
    Notes: Dilithium-(tert-butyl)arsenid reagiert mit (tert-Butyl)dichlorarsan zum Tetra(tert-butyl)tetrarsetan 1; das homologe Tetrastibetan 2 bildet sich bei der Reduktion von (tert-Butyl)dichlorstiban mit Magnesium. Die isotypen Verbindungen kristallisieren monoklin in der Raumgruppe P21/c mit Z = 4. Die bei der Meßtemperatur von -45 ± 5°C bestimmten Gitterkonstanten von 1/2 sind: a = 957,4(8)/1 000,2(3); b = 1 399,1(14)/1 423,9(4); c = 1 697,4(9)/1 749,8(7) pm; β = 96,02(6)/96,77(3)°. Nach den Ergebnissen der Röntgenstrukturanalysen (3 531/3 232 symmetrieunabhängige Reflexe, Rg = 4,0/4,6%) sind die E4-Ringe (E = As, Sb) gefaltet; die voluminösen organischen Substituenten stehen pseudo-äquatorial in der all-trans-Konfiguration. Charakteristische mittlere Bindungslängen und -winkel sind: E—E 244/282; E—C 202/221 pm; ∢ E—E—E 86/85° ∢ E—E—C 101/99°. Die Diederwinkel der von den Ringatomen aufgespannten Bisphenoide betragen 139/133°.
    Additional Material: 5 Ill.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 477 (1981), S. 126-132 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Iron and Nickel Carbonyl Complexes with Substituted Distibane and Antimonido LigandsThe reactions of enneacarbonyldiiron with substituted distibanes yield mononuclear complexes [Fe(CO)4SbR2SbR2] (R = C2H5, t-C4H9), a dinuclear complex [(CO)4FeSbPh2SbPh2Fe(CO)4] and antimonido-bridged compounds [(CO)3Fe(SbR2)2-Fe(CO)3] (R = C2H5, C6H5). Product of the reaction of tetramethyldistibane with tetracarbonylnickel is the binuclear complex [(CO)3NiSbMe2SbMe2Ni(CO)3]. The 1H-n.m.r., i.r., and mass spectra of the new compounds are reported.
    Notes: Bei Reaktionen von Enneacarbonyldieisen mit substituierten Distibanen entstehen die Einkernkomplexe [Fe(CO)4SbR2SbR2] (R = C2H5, t-C4H9), der Zweikernkomplex [(CO)4FeSbPh2SbPh2Fe(CO)4] sowie die antimonido-verbrückten Verbindungen [(CO)3Fe(SbR2)2-Fe(CO)3] (R = C2H5, C6H5). Produkt der Umsetzung von Tetramethyldistiban mit Tetracarbonylnickel ist der Zweikernkomplex [(CO)3NiSbMe2SbMe2Ni(CO)3].Die 1H-NMR-, IR- und Massenspektren der dargestellten Verbindungen werden mitgeteilt.
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