Synthesis and Characterization of donor‐functionalized ansa‐Cyclopentadienyl‐Indenyl and ansa‐Indenyl‐Indenyl Complexes of Yttrium, Samarium, Thulium, and Lutetium
Identifieur interne : 002539 ( Main/Exploration ); précédent : 002538; suivant : 002540Synthesis and Characterization of donor‐functionalized ansa‐Cyclopentadienyl‐Indenyl and ansa‐Indenyl‐Indenyl Complexes of Yttrium, Samarium, Thulium, and Lutetium
Auteurs : Herbert Schumann [Allemagne] ; Frank Erbstein ; Dirk F. Karasiak ; Igor L. Fedushkin ; Jörg Demtschuk ; Frank GirgsdiesSource :
- ZAAC ‐ Journal of Inorganic and General Chemistry [ 0044-2313 ] ; 1999-05.
Descripteurs français
- Wicri :
- topic : Collecte de données, Solvant.
English descriptors
- KwdEn :
- Acta crystallogr, Allg, Anorg, Calc, Chem, Crude product, Crystal structures, Crystallographic data, Cyclopentadienyl, Data collection, Deng, Diethyl ether, Dimethylamino group, Elemental analyses, Fudan xuebao, Functionalized side chain, Hexane, Indenyl, Indenyl ligand, Indenyl lithium, Lanthanide, Lanthanide complexes, Ligand, Lutetium, Mass spectra, Mmol, Molecular structures, Nitrogen atom, Organomet, Organometallic compounds, Organometallics, Ortep plot, Potassium hydride, Qian, Room temperature, Schumann, Solvent, Solvent molecules, Space group, Standard deviations, Technischen universitat, Thulium, Unit cell, Yellow crystals, Zheng, Ziran kexueban.
- Teeft :
- Acta crystallogr, Allg, Anorg, Calc, Chem, Crude product, Crystal structures, Crystallographic data, Cyclopentadienyl, Data collection, Deng, Diethyl ether, Dimethylamino group, Elemental analyses, Fudan xuebao, Functionalized side chain, Hexane, Indenyl, Indenyl ligand, Indenyl lithium, Lanthanide, Lanthanide complexes, Ligand, Lutetium, Mass spectra, Mmol, Molecular structures, Nitrogen atom, Organomet, Organometallic compounds, Organometallics, Ortep plot, Potassium hydride, Qian, Room temperature, Schumann, Solvent, Solvent molecules, Space group, Standard deviations, Technischen universitat, Thulium, Unit cell, Yellow crystals, Zheng, Ziran kexueban.
Abstract
The stepwise reaction of Me2SiCl2 with K[C5H3 tBuMe‐3] or Li[C9H7] and then with K[C9H6CH2CH2‐ NMe2‐1] followed by double deprotonation with NaH or LiBu, yields the two dimethylsilicon bridged cyclopentadienyl‐indenyl and indenyl‐indenyl donor‐functionalized ligand systems K2[(C5H2 tBu‐3‐Me‐5)SiMe2(1‐C9H5CH2CH2NMe2‐3)] (1), and Li2[(1‐C9H6)SiMe2(1‐C9H5CH2CH2NMe2‐3)] (2), respectively. Treatment of 1 with YCl3(THF)3, SmCl3(THF)1.77, TmI3(DME)3, and LuCl3(THF)3 gives the mixed ansa‐metallocenes [(C5H2 tBu‐3‐Me‐5)SiMe2(1‐C9H5CH2CH2NMe2‐3)]LnX (X = Cl, Ln = Y (3), Sm (4), Lu (5); X = I, Ln = Tm (6)), respectively. The reaction of 2 with LuCl3(THF)3 yields [(1‐C9H6)SiMe2(1‐C9H5CH2CH2NMe2‐3)]LuCl (7). Compound 4 reacts with LiMe to give the corresponding alkyl derivative [(C5H2 tBu‐3‐Me‐5)SiMe2(1‐C9H5CH2CH2NMe2‐3)]Sm(CH3) (8). The new complexes were characterized by elemental analyses, MS spectrometry, and NMR spectroscopy. The molecular structures of 5 and 6 were determined by single crystal X‐ray diffraction.
Url:
DOI: 10.1002/(SICI)1521-3749(199905)625:5<781::AID-ZAAC781>3.0.CO;2-L
Affiliations:
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Le document en format XML
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<term>Calc</term>
<term>Chem</term>
<term>Crude product</term>
<term>Crystal structures</term>
<term>Crystallographic data</term>
<term>Cyclopentadienyl</term>
<term>Data collection</term>
<term>Deng</term>
<term>Diethyl ether</term>
<term>Dimethylamino group</term>
<term>Elemental analyses</term>
<term>Fudan xuebao</term>
<term>Functionalized side chain</term>
<term>Hexane</term>
<term>Indenyl</term>
<term>Indenyl ligand</term>
<term>Indenyl lithium</term>
<term>Lanthanide</term>
<term>Lanthanide complexes</term>
<term>Ligand</term>
<term>Lutetium</term>
<term>Mass spectra</term>
<term>Mmol</term>
<term>Molecular structures</term>
<term>Nitrogen atom</term>
<term>Organomet</term>
<term>Organometallic compounds</term>
<term>Organometallics</term>
<term>Ortep plot</term>
<term>Potassium hydride</term>
<term>Qian</term>
<term>Room temperature</term>
<term>Schumann</term>
<term>Solvent</term>
<term>Solvent molecules</term>
<term>Space group</term>
<term>Standard deviations</term>
<term>Technischen universitat</term>
<term>Thulium</term>
<term>Unit cell</term>
<term>Yellow crystals</term>
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<term>Elemental analyses</term>
<term>Fudan xuebao</term>
<term>Functionalized side chain</term>
<term>Hexane</term>
<term>Indenyl</term>
<term>Indenyl ligand</term>
<term>Indenyl lithium</term>
<term>Lanthanide</term>
<term>Lanthanide complexes</term>
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<term>Molecular structures</term>
<term>Nitrogen atom</term>
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<term>Organometallic compounds</term>
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<front><div type="abstract">The stepwise reaction of Me2SiCl2 with K[C5H3 tBuMe‐3] or Li[C9H7] and then with K[C9H6CH2CH2‐ NMe2‐1] followed by double deprotonation with NaH or LiBu, yields the two dimethylsilicon bridged cyclopentadienyl‐indenyl and indenyl‐indenyl donor‐functionalized ligand systems K2[(C5H2 tBu‐3‐Me‐5)SiMe2(1‐C9H5CH2CH2NMe2‐3)] (1), and Li2[(1‐C9H6)SiMe2(1‐C9H5CH2CH2NMe2‐3)] (2), respectively. Treatment of 1 with YCl3(THF)3, SmCl3(THF)1.77, TmI3(DME)3, and LuCl3(THF)3 gives the mixed ansa‐metallocenes [(C5H2 tBu‐3‐Me‐5)SiMe2(1‐C9H5CH2CH2NMe2‐3)]LnX (X = Cl, Ln = Y (3), Sm (4), Lu (5); X = I, Ln = Tm (6)), respectively. The reaction of 2 with LuCl3(THF)3 yields [(1‐C9H6)SiMe2(1‐C9H5CH2CH2NMe2‐3)]LuCl (7). Compound 4 reacts with LiMe to give the corresponding alkyl derivative [(C5H2 tBu‐3‐Me‐5)SiMe2(1‐C9H5CH2CH2NMe2‐3)]Sm(CH3) (8). The new complexes were characterized by elemental analyses, MS spectrometry, and NMR spectroscopy. The molecular structures of 5 and 6 were determined by single crystal X‐ray diffraction.</div>
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