An Improved Synthesis of Sodium and Potassium Cyclopentadienide

Panda, Tarun K.; Gamer, and Michael T.; Roesky, Peter W.

doi:10.1021/om0207865

Cited by 116 publications

(103 citation statements)

References 6 publications

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“…NaCp was prepared according to the literature. [31] B(C 6 F 5 ) 3 was purchased from Sigma-Aldrich. The NMR spectra were recorded in [D 6 ]benzene with a Bruker AV 300 spectrometer ( 1 H 300.…”

Section: Methodsmentioning

confidence: 99%

A Convenient Synthesis of Cyclopentadienylgallium – The Awakening of a Sleeping Beauty in Organometallic Chemistry

et al. 2011

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Solid “GaI” reacts with NaCp to yield (η5‐cyclopentadienyl)gallium (GaCp) (1). During the synthesis the side product, CpGa→GaCp2I (2), with a rare gallium–gallium donor–acceptor bond could be isolated. The reaction of 1 with B(C6F5)3 affords CpGa→B(C6F5)3 (4). The molecular structures of 2 and 4, which contain the first GaCp moieties, are presented. The convenient synthesis of 1 needs only standard laboratory equipment and certainly opens the door for 1 to become a versatile reagent in organometallic chemistry; awakening the sleeping beauty GaCp nearly twenty years after its initial discovery.

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Section: Methodsmentioning

confidence: 99%

A Convenient Synthesis of Cyclopentadienylgallium – The Awakening of a Sleeping Beauty in Organometallic Chemistry

et al. 2011

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“…[56] NaCp was prepared according to a novel literature method. [58] [LnCp3] compounds (Ln = Nd, Sm, Eu, Gd, Dy, Ho, Er, Yb) were prepared according to well-known procedures [59] and before use were sublimed twice under vacuum (10 À3 mbar) at temperatures of between 150 and 250 8C. The syntheses of complexes 1-Ln and 2-Ln are based mainly on a procedure reported earlier, in particular for the Yb compounds.…”

Section: Methodsmentioning

confidence: 99%

Nanocrystalline Lanthanide Nitride Materials Synthesised by Thermal Treatment of Amido and Ammine Metallocenes: X‐ray Studies and DFT Calculations

Baisch

Pagano

Zeuner

et al. 2006

Chemistry A European J

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The decomposition process of ammine lanthanide metallocenes was studied by X-ray diffractometry, spectroscopy and theoretical investigations. A series of ammine-tris(eta(5)-cyclopentadienyl)lanthanide(III) complexes 1-Ln (Lanthanide (Ln)=Sm, Gd, Dy, Ho, Er, Yb) was synthesised by the reaction of [Cp(3)Ln] complexes (Cp=cyclopentadienyl) with liquid ammonia at -78 degrees C and structurally characterised by X-ray diffraction methods, mass spectrometry and vibrational (IR, Raman) spectroscopy. Furthermore, amido-bis(eta(5)-cyclopentadienyl)lanthanide(III) complexes 2-Ln (Ln=Dy, Ho, Er, Yb) were synthesised by heating the respective ammine adduct 1-Ln in an inert gas atmosphere at temperatures of between 240 and 290 degrees C. X-ray diffraction studies, mass spectrometry and vibrational (IR, Raman) spectroscopy were carried out for several 2-Ln species and proved the formation of dimeric mu(2)-bridged compounds. Species 1-Ln are highly reactive coordination compounds and showed different behaviour regarding the decomposition to 2-Ln. The reaction of 1-Ln and 2-Ln with inorganic bases yielded lanthanide nitride LnN powders with an estimated crystallite size of between 40 and 90 nm at unprecedented low temperatures of 240 to 300 degrees C. Temperature-dependent X-ray powder diffraction and transmission electron microscopy (TEM) investigations were performed and showed that the decomposition reaction yielded nanocrystalline material. Structural optimisations were carried out for 1-Ln and 2-Ln by employing density functional (DFT) calculations. A good agreement was found between the observed and calculated structural parameters. Also, Gibbs free energies were calculated for 1-Ln, 2-Ln and the pyrolysis reaction to the nitride material, and were found to fit well with the expected ranges.

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“…, [14] MA C H T U N G T R E N N U N G [C 29 H 37 ] (M= Li, K), [15] K[BA C H T U N G T R E N N U N G (C 6 F 5 ) 4 ], [16] (Me 2 N)B 2 A C H T U N G T R E N N U N G (h 1 -C 5 H 5 )(Br), [11] (Me 2 NBBr) 2 [17] and NaCp [18] were obtained according to literature procedures. HfCl 4 , nBuLi and MeLi were obtained commercially and used without further purification.…”

Section: A C H T U N G T R E N N U N G [Zrcl 4 a C H T U N G T R E N mentioning

confidence: 99%

Sterically Demanding Hetero‐Substituted [2]Borametallocenophanes of Group IV Metals: Synthesis, Structure and Reactivity

Braunschweig

Dörfler

Mies

et al. 2011

Chemistry A European J

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We report the synthesis and characterisation of unprecedented unstrained [2]diborametallocenophanes of zirconium and hafnium that bear the bulky octamethylfluorenyl (η(5)-C(29)H(36)) system, the proligands of which were pre-constructed by a two-step synthesis. The compounds were fully characterised by NMR spectroscopy, MALDI-TOF mass spectrometry and X-ray diffraction analysis. Typical reactivities relevant to olefin polymerisation such as methylation and chloride abstraction were also investigated. Finally, a sterically demanding bis(octamethylfluorenyl) metallocene was prepared.

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An Improved Synthesis of Sodium and Potassium Cyclopentadienide

Cited by 116 publications

References 6 publications

A Convenient Synthesis of Cyclopentadienylgallium – The Awakening of a Sleeping Beauty in Organometallic Chemistry

A Convenient Synthesis of Cyclopentadienylgallium – The Awakening of a Sleeping Beauty in Organometallic Chemistry

Nanocrystalline Lanthanide Nitride Materials Synthesised by Thermal Treatment of Amido and Ammine Metallocenes: X‐ray Studies and DFT Calculations

Sterically Demanding Hetero‐Substituted [2]Borametallocenophanes of Group IV Metals: Synthesis, Structure and Reactivity

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