Low-frequency infrared and Raman spectra of .pi.-cyclopentadienyl compounds of titanium, zirconium, and hafnium

Samuel, Edmond; Ferner, R.; Bigorgne, M.

doi:10.1021/ic50122a035

Cited by 47 publications

(13 citation statements)

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“…Methods for the preparation of Cp/titanium alkoxide complexes. enyl titanium trichloride (CpTiCl 3 ), 11 and pentamethylcyclopentadienyl titanium trichloride (Cp*TiCl 3 ) 11 were prepared according to the literature.…”

Section: Methodsmentioning

confidence: 99%

Novel catalyst compositions for the syndiospecific polymerization of styrene prepared by the combination of cyclopentadenyl complexes of group IIA or group IIIA elements with titanium alkoxides

Tsai

Kuo

Chen

2005

J. Polym. Sci. A Polym. Chem.

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A highly reactive catalyst system, which induces the syndiospecific polymerization of styrene with high activity, has been found by the combination of cyclopentadienyl (Cp) complexes of group IIA or group IIIA elements with titanium alkoxides. The 1 H NMR monitoring of these reactions reveals the occurrence of a novel Cp-transfer reaction that leads to the generation of Cp-containing titanium complexes as catalysts for promoting the syndiospecific polymerization of styrene. Detailed in situ 1 H NMR studies reveal that the rate of the Cp-transfer reaction is highly dependent on the steric bulkiness of the titanium alkoxide complexes, the structures of the Cp complexes of group IIA or group IIIA elements, and the polymerization temperature. Styrene polymerization studies also reveal that a more effective Cp-transfer reaction can typically lead to the generation of a more highly reactive catalyst for sPS polymerization. This study provides a convenient method for the in situ generation of variable structures of Cp/titanium alkoxide complexes, which are difficult to synthesize by other methods. Most importantly, the mixture of a catalyst precursor can be directly used as an sPS polymerization catalyst without isolation and purification of Cp/titanium complexes. # 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym

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Section: Methodsmentioning

confidence: 99%

Novel catalyst compositions for the syndiospecific polymerization of styrene prepared by the combination of cyclopentadenyl complexes of group IIA or group IIIA elements with titanium alkoxides

Tsai

Kuo

Chen

2005

J. Polym. Sci. A Polym. Chem.

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“…Two equivalents of compound L CN ( n -Bu) 2 SnF or L CN Ph 2 SnF, or one equivalent of (L CN ) 2 SnF 2 , respectively, were mixed with one equivalent of titanocene dichloride, Brought to you by | University of Bath Authenticated Download Date | 6/17/15 12:18 AM and stirred in dichloromethane at 35 ° C, in the air. Within 3 h the color changed from orange to yellow and the desired compound (Cp 2 TiF 2 ) (Druce et al , 1969 ;Nesmeyanov et al , 1972Nesmeyanov et al , , 1975Samuel et al , 1973 ;Cauzzi et al , 2002 ) was isolated essentially quantitatively by easy washing the product with cold pentane, no trace of starting material was observed.…”

Section: Fluorination Of Complexes Of Ti Sb and Bimentioning

confidence: 99%

Use of C,N-chelated triorganotin(IV) fluoride for fluorination of organic compounds, coordination compounds, phosphines, silanes and stannanes

Růžička¹

2011

Main Group Metal Chemistry

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C,N-chelated triorganotin(IV) compounds containing the L CN ligand, where L CN is {2-[(CH 3 ) 2 NCH 2 ]C 6 H 4 } -, reveal the monomeric structure in solution as well as in the solid state with pentacoordinated tin atom in trigonal bipyramidal coordination polyhedra. These compounds were used as mild and very effi cient metathetical fl uorinating agents in fl uorinations of various organic, inorganic substrates and organometallic species containing E-Cl (E = C, Si, P, S and metal) bond(s) (metal halides, phosphines, silanes, etc.) as well as the F ion selective carriers with low detection limits.

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“…Die IR-Spektren von 2,6-Bis(methylencyclopentadienyl)pyridin-zirconiumdichlorid (13) und der analogen Hafniumverbindung (14) sowie des 2,6-Bis(methylenindenyl)pyridin-zirconiumdichlorids (3) und Picolyl-inden-1-yl-zirconiumtrichlorids (12) [16]. Im Gasphasenspektrum wurden diesen Schwingungen die Banden bei 351 und 341 cm ±1 zugeordnet [17].…”

Section: Ir-spektrenunclassified

“…Es sind daher die Schultern bei 330, 317 und 298 cm ±1 , die fu È r die Hf±Cl-Schwingungen in Betracht kommen. Diese Schwingungen wurden im Festko È rperspektrum des Cp 2 HfCl 2 den Banden bei 325 und 312 cm ±1 [16] und im Gasphasenspektrum denjenigen bei 332 und 324 cm ±1 zugeordnet. Die Hf±N-Valenzschwingungen sollen aus den bei 13 geschilderten Gru È nden wiederum nicht zugeordnet werden.…”

Section: Ir-spektrenunclassified

Synthese und Eigenschaften von Metallocen- und Halbsandwich-Komplexen mit pyridinhaltigen Brücken bzw. Seitenketten

Schließburg

Thiele

Lindner

et al. 2000

Z. anorg. allg. Chem.

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Aus 2,6‐Bis(chlormethyl)pyridin (1) und Indenyllithium (Molverhältnis 1 : 4) entsteht 2,6‐Bis(methylenindenyl)pyridin‐dilithium (2), das bei Reaktionen mit MCl4 · 2 THF (M = Zr, Hf) in die entsprechenden Metallocendichloride 3 und 4 übergeht. Bei Einwirkung von 2 Äquivalenten C5H5Na auf 1 wird nur ein Cl‐Atom gegen eine metallierte C5H5‐Gruppe ausgetauscht. Aus dem Reaktionsprodukt 5 läßt sich mittels Indenyllithium und ZrCl4 · 2 THF der unsymmetrische Komplex [C5H3N‐2,6‐CH2‐(2‐C5H4)–(6C9H6)ZrCl2] (7) herstellen. – Aus 2‐Chlormethylpyridiniumchlorid und C5H5Na bzw. Indenyllithium werden Picolylcyclopentadien (8) und 1‐(Picolyl)‐inden (9) synthetisiert, die metalliert und mittels MCl4 · 2 THF (M = Ti, Zr) in die Halbsandwichkomplexe (C5H4N–CH2C5H4)MCl3 (M = Ti 10, Zr 11) und (C5H4N–CH2C9H6)ZrCl3 (12) überführt werden. Die Verbindungen wurden elementaranalytisch, sowie durch ihre 1H‐NMR‐, MS‐, IR‐ und Ramanspektren charakterisiert. Das Auftreten von N → M‐Wechselwirkungen wird diskutiert bzw. für einige Verbindungen nachgewiesen.

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Low-frequency infrared and Raman spectra of .pi.-cyclopentadienyl compounds of titanium, zirconium, and hafnium

Cited by 47 publications

References 0 publications

Novel catalyst compositions for the syndiospecific polymerization of styrene prepared by the combination of cyclopentadenyl complexes of group IIA or group IIIA elements with titanium alkoxides

Novel catalyst compositions for the syndiospecific polymerization of styrene prepared by the combination of cyclopentadenyl complexes of group IIA or group IIIA elements with titanium alkoxides

Use of C,N-chelated triorganotin(IV) fluoride for fluorination of organic compounds, coordination compounds, phosphines, silanes and stannanes

Synthese und Eigenschaften von Metallocen- und Halbsandwich-Komplexen mit pyridinhaltigen Brücken bzw. Seitenketten

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