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'NMR Spectra' in keywords Facet   Publication Year 1994  [X]
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1994[X]
1Author    Jörn Müller, PetraEscarpa Gaede, Ke QiaoRequires cookie*
 Title    ^-Olefin-Iridium-Komplexe, XXII [1] C -H -Aktivierung von aromatischen und aliphatischen Solvensmolekülen RH bei der Reaktion von [Cp*IrCI2 ] 2 mit Butadienmagnesium unter Bildung von [Cp*Ir(773-C4H 7)R] sowie Kristallstruktur von [Cp*Ir(i/3-C4H 7)C6H 5] jr-Olefin Iridium Complexes, XXII [1] C -H Activation of Aromatic and Aliphatic Solvent Molecules RH in the Reaction of [Cp*IrCl2 ] 2 with Butadienemagnesium with Formation of [Cp*Ir(?;3 -C4 H 7 )R], and Crystal Structure of [Cp*Ir(773 -C4 H 7 )C6 H 5] Activation of C -H , (l-Methylallyl)(pentamethylcyclopentadienyl)iridium-a-organyl Com­ plexes  
 Abstract    Reactions of [Cp*IrCl2]2 (Cp* = ^3-C5M e5) with [MgC4H6 -2 THF]" at low temperature give [Cp*Ir(^4-C4H6)] together with [Cp*Ir(/73-C4H 7)R] compounds, the latter being formed via C -H activation of solvent molecules RH (RH = benzene, toluene, anisole, thiophene, furane, N-methylpyrrole, pentane, cyclohexane. THF). In the case of pyrrole, C -N -activation occurs. The ratio of syn and anti isomers of the 1-methylallyl com plexes as well as the sites o f C -H activation of RH were investigated by NM R spectrometry. An enantiomorphous crystal of [Cp*Ir(773-C4H7)C6Hs] was characterized by X-ray diffraction analysis which reveals trigonal planar coordination at the Ir atom and an exo, syn conformation o f the 1-methylallyl ligand. A mechanism of the reaction which involves 16-electron intermediates is discussed. The corresponding system [Cp*RhCl2]2/butadienemagnesium/RH gives only [Cp*Rh(>/4-C4H6)], and no C -H activation is observed. 
  Reference    Z. Naturforsch. 49b, 1645—1653 (1994) 
  Published    1994 
  Keywords    Synthesis, NMR Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1645.pdf 
 Identifier    ZNB-1994-49b-1645 
 Volume    49 
2Author    Anne-Kathrin Duhme, Henry StrasdeitRequires cookie*
 Title    Ligandenmangelkomplexe des Cadmiums. Synthese und spektroskopische Charakterisierung molekularer (Pentafluorphenyl)cadmium-Thiolate und die Struktur des Cubankomplexes [{Cd(C6F5)(SBur)}4] Ligand-Deficient Complexes of Cadmium. Synthesis and Spectroscopic Characterization o f Molecular Pentafluorophenyl Cadmium Thiolates and the Structure o f the Cubane Complex [{Cd(C6F5)(SBuf)}4]  
 Abstract    In toluene, bis(pentafluorophenyl)cadmium(II) and thiols RSH (R = Bu', 2,4,6-Pr'3C6H2, 2,4,6-Bu'3C6H2) react to give soluble pentafluorophenyl cadmium thiolates [(Cd(C6F5)(SR)} J. The compounds [{Cd(C6F 5)(SBu')}4] (1)0 .5 C6H5CH3, [ {Cd(C6F5)(SC6H2Pr'3-2,4,6)} J (2)-ca. 0.25n C6H 5CH3, and [{Cd(C6F5)(SC6H2Bu'3-2,4,6)} J (3) ca. 0.25« C6H5CH3 have been prepared in 65, 59 and 78% yield, respectively. 1-0.5 C6H5CH3 crystallizes in the triclinic space group PI with a = 11,635(1)Ä, b = 11.583(1)Ä, c = 21.480(2)Ä, a = 82.12(1)°, ß = 76.26(1)°, y — 89.35(1)°, and Z = 2. 1 is a cubane-type complex with a {Cd4(/z3-SBur)4}4+ core. Each Cd atom is coordinated by three bridging thiolato ligands and one terminal C6F5 group (C d -S 2.62 A, C d -C 2.15Ä (mean values)). The central C atoms of the Bu'S" ligands of 1 show a remarkable low-field shift o f their 13C N M R resonance (12.3 ppm relative to the value of the free thiol). A characteristic spectral feature of (Cd(C6F5) } + complexes is the large value of the coupling constant 2/ (19F ,13C) o f the ipso-C atom (1, 2: 68 Hz; 3: 67 Hz). The complexes [Cd(C6F5)(SR) + H]+, [Cd(SR)2 + H]+, and [Cd2(SR)3]+ were identified in the Cl mass spectra (/50-butane) of 2 and 3. 
  Reference    (Z. Naturforsch. 49b, 119—127 [1994]; eingegangen am 17. August 1993) 
  Published    1994 
  Keywords    Cadmium Complexes, Thiolates, Crystal Structure, NMR Spectra, Mass Spectra 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0119.pdf 
 Identifier    ZNB-1994-49b-0119 
 Volume    49 
3Author    JensR. Goerlich, Axel Fischer, PeterG. Jones, Reinhard Schmutzler+Requires cookie*
 Title    Organophosphorverbindungen mit tertiären Alkylsubstituenten. III*: Synthese und Reaktionen Di-l-adamantylsubstituierter Phosphorverbindungen; Kristallstruktur von Di-l-Adamantylphosphinsäurechlorid Organophosphorus Compounds with Tertiary Alkyl Substituents. Ill: Synthesis and Reactions of D i-l-adam antyl-Substituted Phosphorus Compounds; Crystal Structure of Di-l-adam antylphosphinic Chloride  
 Abstract    The reaction of adamantane with PC13/A1C13, followed by hydrolysis, gave (l-Ad)2P(: 0)C1 1, which was converted to (l-Ad)2P(:Ö)F 2 and (l-Ad)2P(:S)Cl 3 by standard procedures. The structure of 1 was confirmed by a single crystal X-ray structure determination; despite the bulky substituents the P-C bond lengths are normal (184.0(3), 185.0(3) pm). Whereas chlorine-fluorine exchange in 3 with AsF3 furnished (l-Ad)2P(: S)F 4, desulfuration of 3 with Ph3P to give (l-Ad)2PCl 5 failed. The secondary phosphine oxides R 'R 2P(:0)H (R1, R2 = 1-Ad: 6; R1 = 1-Ad, R2 = 'Bu: 7; R1, R2 = 'Bu: 8) were synthesized by reaction of 1, l-AdP(:0)Cl2 and 'BuP(:0)Cl2 with 'BuLi. 6 and 8 reacted readily with chloral to give the adducts R2P(:0)CH(0H)CC13 (R = 1-Ad: 9; R = 'Bu: 10). Silylation of 6 with Me2NSiMe3 in the presence of dry air led to (l-Ad)2P(:0)0SiM e3 11, which was hydrolyzed to give (l-Ad)2P (:0)0H 12. (l-Ad)2POSiMe3 13 was obtained by the reaction of 6 with /z-BuLi, followed by Me3SiCl. No reaction took place upon heating 6 with Mo(CO)6. (l-Ad)2PCl 5 was synthesized in low yield by the reaction of 6 with PC13. The action of tetrachloro-o-benzoquinone (TOB) upon 6 furnished (l-Ad)2P(: 0)(o-OH)C6Cl4 15, whereas the 'butyl analogue of 15, 16, was synthesized by hydrolysis of the TOB-adduct of di-'butylfluorophos-phine. Analogous 1-adamantyl-and 'butyl-phosphorus compounds are compared with regard to their 31P NMR data. 
  Reference    Z. Naturforsch. 49b, 801—811 (1994); eingegangen am 17. Dezember 1993 
  Published    1994 
  Keywords    Di-l-adamantyl Phosphorus Compounds, Secondary Phosphine Oxides, Di-l-adamantyl Phosphinic Acid, NMR Spectra, X-Ray 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0801.pdf 
 Identifier    ZNB-1994-49b-0801 
 Volume    49