Synthetic and structural studies on early transition metal siloxides

 

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dc.contributor.advisor Hutton, Alan T
dc.contributor.author Jones, Robert Edward
dc.date.accessioned 2017-01-25T14:27:11Z
dc.date.available 2017-01-25T14:27:11Z
dc.date.issued 1993
dc.identifier.citation Jones, R. 1993. Synthetic and structural studies on early transition metal siloxides. University of Cape Town. en_ZA
dc.identifier.uri http://hdl.handle.net/11427/23079
dc.description.abstract [Super- and subscripts in abstract] n-Bu3SiOH was prepared from both n-Bu3SiH and n-Bu3SiCI. Reactions of n-Bu3SiOH with NaH, LiBun, MC15 (M = Ta or Mo) and Cp2MCl2 (Cp = 115-C5H5, M = Ti or Zr) were investigated, in some cases using the base Et3N as a hydrogen chloride acceptor. Na+(QSiPh3r was prepared from the reaction of Ph3SiOH with NaH, but in poor yield. Ph3SiOH was reacted with TaCI5, but the product, if formed at all, was intractable. When Ph3SiOH was reacted with Cp2MC12 (M = Ti or Zr) products were isolated and characterised, viz. [Cp2 TiCl(OSiPh3)]n (n = 1 or 2) and Cp2Zr(OSiPh3)2. Single crystals Cp2Zr(OSiPh3h were studied using X-ray photographic techniques. They crystallise in the monoclinic system with a = 35. 7, b = 10.4, c = 21.1 A, f3 = 97.7 °, V= 7763 A3. A full crystal structure analysis was not possible due to failure of the diffractometer software to locate the monoclinic unit cell determined by photographic methods. Ph3 SiOH was also reacted with Cp 2ZrC12 (Cp = 115-C5Me5) and the product was tentatively assigned to be Cp 2Zr(OSiPh3h as a pure sample could not be obtained. An interesting spirocompound, Ti[OSiPh2(0SiPh2)30h, was prepared from Ph2Si(0Hh and Ti(n-Bu0)4 and the crystal structure determined by X-ray crystallography. It crystallises in the monoclinic system, space group P21/n, a = 13.805(5), b = 27.545(5), c = 23.476(9) A, f3 = 94.41(3) 0 , V= 8901(5) A3, Z = 4, R = 0.0831 for 5528 reflections with Ire/> 2a(Iref).
dc.language.iso eng
dc.subject.other Chemistry
dc.title Synthetic and structural studies on early transition metal siloxides
dc.type Thesis
dc.date.updated 2016-11-22T08:38:53Z
dc.publisher.institution University of Cape Town
dc.publisher.faculty Faculty of Science en_ZA
dc.publisher.department Department of Chemistry en_ZA
dc.identifier.apacitation Jones, R. E. (1993). <i>Synthetic and structural studies on early transition metal siloxides</i>. (). University of Cape Town ,Faculty of Science ,Department of Chemistry. Retrieved from http://hdl.handle.net/11427/23079 en_ZA
dc.identifier.chicagocitation Jones, Robert Edward. <i>"Synthetic and structural studies on early transition metal siloxides."</i> ., University of Cape Town ,Faculty of Science ,Department of Chemistry, 1993. http://hdl.handle.net/11427/23079 en_ZA
dc.identifier.vancouvercitation Jones RE. Synthetic and structural studies on early transition metal siloxides. []. University of Cape Town ,Faculty of Science ,Department of Chemistry, 1993 [cited yyyy month dd]. Available from: http://hdl.handle.net/11427/23079 en_ZA
dc.identifier.ris TY - Thesis / Dissertation AU - Jones, Robert Edward AB - [Super- and subscripts in abstract] n-Bu3SiOH was prepared from both n-Bu3SiH and n-Bu3SiCI. Reactions of n-Bu3SiOH with NaH, LiBun, MC15 (M = Ta or Mo) and Cp2MCl2 (Cp = 115-C5H5, M = Ti or Zr) were investigated, in some cases using the base Et3N as a hydrogen chloride acceptor. Na+(QSiPh3r was prepared from the reaction of Ph3SiOH with NaH, but in poor yield. Ph3SiOH was reacted with TaCI5, but the product, if formed at all, was intractable. When Ph3SiOH was reacted with Cp2MC12 (M = Ti or Zr) products were isolated and characterised, viz. [Cp2 TiCl(OSiPh3)]n (n = 1 or 2) and Cp2Zr(OSiPh3)2. Single crystals Cp2Zr(OSiPh3h were studied using X-ray photographic techniques. They crystallise in the monoclinic system with a = 35. 7, b = 10.4, c = 21.1 A, f3 = 97.7 °, V= 7763 A3. A full crystal structure analysis was not possible due to failure of the diffractometer software to locate the monoclinic unit cell determined by photographic methods. Ph3 SiOH was also reacted with Cp 2ZrC12 (Cp = 115-C5Me5) and the product was tentatively assigned to be Cp 2Zr(OSiPh3h as a pure sample could not be obtained. An interesting spirocompound, Ti[OSiPh2(0SiPh2)30h, was prepared from Ph2Si(0Hh and Ti(n-Bu0)4 and the crystal structure determined by X-ray crystallography. It crystallises in the monoclinic system, space group P21/n, a = 13.805(5), b = 27.545(5), c = 23.476(9) A, f3 = 94.41(3) 0 , V= 8901(5) A3, Z = 4, R = 0.0831 for 5528 reflections with Ire/> 2a(Iref). DA - 1993 DB - OpenUCT DP - University of Cape Town LK - https://open.uct.ac.za PB - University of Cape Town PY - 1993 T1 - Synthetic and structural studies on early transition metal siloxides TI - Synthetic and structural studies on early transition metal siloxides UR - http://hdl.handle.net/11427/23079 ER - en_ZA


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