Pentamethylcyclopentadienyl halo- and alkyl-alkoxo tantalum(V) complexes. Crystal structure of TaCp*(CH2SiMe3) 2{η2-O(2-CH2-6-MeC6H3)}
Authors
Castro Gausinet, Irene de; Galakhov, Mikhail V.; Gómez Rubio, ManuelIdentifiers
Permanent link (URI): http://hdl.handle.net/10017/4554DOI: 10.1016/0022-328X(95)06004-G
ISSN: 0022-328X
Publisher
Elsevier
Date
1996Bibliographic citation
Journal of Organometallic Chemistry, 1996, v. 514, n. 1-2, p. 51-58
Keywords
Tantalum
Pentamethylcyclopentadienyl derivatives
Halo alkoxides
Alkyl phenoxides
Alkyl alkylidene imino acyl
Project
PB-92-0178-C (Ministerio de Educación y Cultura)
Document type
info:eu-repo/semantics/article
Version
info:eu-repo/semantics/publishedVersion
Publisher's version
http://dx.doi.org/10.1016/0022-328X(95)06004-GRights
(c) Elsevier, 1996
Access rights
info:eu-repo/semantics/openAccess
Abstract
Reaction of TaCp" C! 4 with MOR (M - Li, Na) in different molar ratios gives halo alkoxides TaCp" CI,(OR)4_,, (n - 3: R -tBu 1;
$iPh 3 2; 2,6-Me2C6H 3 3; n -- 2: R -~Bu 4; SiPh 3 5; 2,6-Me2C6H3 6; a - !: R - SiMe 3 7) in good yields. The alkylidene complex
TaCp'(CH2SiMe,02(CHSiMe ~) is hydrolyzed in the presence of traces of water to give the oxo dialkyl derivative
[TaCp'(CH2SiM¢3)~O],, 8, and reacts with I equivalent of 2,6-MezC6H~NC affording a new 'q2-iminoacyi compound
TaCp" (CH 2$iMe3XCHSiMe3){~ 2"C(CH 2SiMe3 ) = N(2,6"MeaC6 H 3)} 9. Reactions of TaCp "(CH 2SiMe3)a(CHSiMe3 ) with I equivalent
of C6HsOH and 4-MeC6H3(OH) 2 result in the formation of the alkyl phenoxo TaCp'(CH2SiMe3)3(OC6Hs) 10 and 4-methyl
pyrocatecholate TaCp'(CH2SiMe~)2(O2C6H3Me) 11, whereas the related re,",,:don with 2,6-Me2C6H 3OH leads to the cyclic alkyi-aikoxo
compound TaCp (CH2SiMej)2(~2-O(2-CH2-6-MeC6H3)) 12. All the complexes were characterized by IR and NMR (tH and
13C) spectroscopy. The crystal and molecular structure of 12 has been determine~i. C~ystals of 12 are triclinic, space group P'[ with Z - 2
in a unit cell of dimensions a- 9.151(5) ~, b- 11.835(5) ~,, c- 14.045(4) A, a- 89.35(3) °, /3- 72.34(3) 0 and 'y-88.51(4) °,
V- 1449(I) ~s. Final values of R -0.025 and Rw -0.0655 were obtained from 554'7 reflections measured (50'70, > 2o'(i)).
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