First NMR observation of 47Ti and 49Ti in cyclopentadienyl complexes

Dormond, A.; Fauconet, Michel; Leblanc, Jean-Claude; Moı̈se, Claude

doi:10.1016/s0277-5387(00)84642-2

Cited by 24 publications

(12 citation statements)

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“…(64) Ti( 17 OPr i )4 was prepared by the repeated mixing and vacuum distillation of Ti(OPr i )4 and a 1:1 mixture of (20%) H 17 OPr i /HOPr i . pentadienyl halide, [65][66][67][68][69][70][71] carbonyl, 72 halide, 65,66,71,[73][74][75] and alkoxide 13,65,76 ligands. It appears that even slightly perturbed octahedrally bound titanium metal centers are not amenable to Ti NMR nuclei studies due to the reduced symmetry of the axial ligands.…”

Section: Resultsmentioning

confidence: 99%

Titanium(IV) Neopentoxides. X-ray Structures of Ti₃(μ₃-O)(μ₃-Cl)(μ-OCH₂CMe₃)₃(OCH₂CMe₃)₆and [Ti(μ-OCH₂CMe₃)(OCH₂CMe₃)₃]₂

et al. 1997

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Attempts to synthesize titanium(IV) neopentoxide led to two unique products which were crystallographically characterized. A metathesis reaction between TiCl(4) and NaOCH(2)CMe(3) (NaONp) yielded Ti(3)(O)(Cl)(ONp)(9).C(7)H(8), 1, which adopts a standard M(3)(&mgr;(3)-X)(2)(&mgr;-X)(3)X(6) structure. The &mgr;(3) ligands are a Cl and an O atom, with the rest of ligands represented by bridging and terminal ONp ligands. [Ti(ONp)(4)](2), 2, was isolated in high yield by an alcoholysis exchange between Ti(OPr(i))(4) and HONp. 2 adopts a typical M(2)(&mgr;-X)(2)(X)(6) fused axial-equatorial edge-shared geometry, wherein each metal center is 5 coordinated. On the basis of molecular weight solution studies and (1)H, (13)C, (17)O (natural abundance), and (47,49)Ti solution and solid-state NMR investigations, 2 was determined to be a monomer in solution.

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Section: Resultsmentioning

confidence: 99%

Titanium(IV) Neopentoxides. X-ray Structures of Ti₃(μ₃-O)(μ₃-Cl)(μ-OCH₂CMe₃)₃(OCH₂CMe₃)₆and [Ti(μ-OCH₂CMe₃)(OCH₂CMe₃)₃]₂

et al. 1997

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“…Only few reports to date have dealt with 47/49Ti NMR. [3][4][5][6] We report here our attempts to measure 47/49Ti NMR on a series of organic reagents and our failure to detect the 47/49Ti signal in several cases, in order that unfruitful work by other groups may be avoided. The results are given in Table 1.…”

Section: Introductionmentioning

confidence: 99%

^47/49Ti NMR of some titanium compounds

Berger

Bock

Marth

et al. 1990

Magnetic Reson in Chemistry

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“…The 49 Ti NMR spectrum features an intense signal at δ = –726 ppm (Δ ν 1/2 = 270 Hz), which is in the range characteristic of titanocene dichlorides 8. In addition, 1 and the complex trichlorido{η 5 ‐[dimethyl(phenylethynyl)silyl]cyclopentadienyl}titanium(IV), PhC≡CMe 2 SiC 5 H 4 TiCl 3 , [ δ ( 49 Ti) = –366 ppm]8b were identified as byproducts 14…”

Section: Resultsmentioning

confidence: 99%

Transition‐Metal Compounds Containing Alkynylsilyl Groups – Cyclopentadienyl Complexes

2012

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6018 was also successful. In contrast, the direct complexation of (alkynylsilyl)cyclopentadiene or the direct alkynylsilylation of cymantrene were not feasible. Redox reactions and the desilylation of the cyclopentadienyl ring were hampering side reactions in all routes but to varying extent. All three complexes were characterized by NMR spectroscopy. 1 and 3 were also studied by IR and UV/Vis spectroscopy. The molecular and crystal structure of compound 1 was determined by X-ray diffraction analysis.metathesis of an (alkynylsilyl)cyclopentadienide], [4] and one of manganese [prepared by the reaction of a (chlorosilyl)cyclopentadienyl complex with a lithium acetylide] [5] reported, which bear alkynylsilyl groups, whereas the corresponding oligosilyl compounds are completely unknown. However, there is a number of related (alkenyl-or allenylsilyl)cyclopentadienyl complexes. [6] Herein, we present a comparative assessment of synthetic routes leading to (alkynylsilyl)cyclopentadienyl complexes, as well as two new examples of such compounds. [7] Scheme 1. Synthesis of compounds 1 and 2.

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First NMR observation of 47Ti and 49Ti in cyclopentadienyl complexes

Cited by 24 publications

References 4 publications

Titanium(IV) Neopentoxides. X-ray Structures of Ti₃(μ₃-O)(μ₃-Cl)(μ-OCH₂CMe₃)₃(OCH₂CMe₃)₆and [Ti(μ-OCH₂CMe₃)(OCH₂CMe₃)₃]₂

Titanium(IV) Neopentoxides. X-ray Structures of Ti₃(μ₃-O)(μ₃-Cl)(μ-OCH₂CMe₃)₃(OCH₂CMe₃)₆and [Ti(μ-OCH₂CMe₃)(OCH₂CMe₃)₃]₂

^47/49Ti NMR of some titanium compounds

Transition‐Metal Compounds Containing Alkynylsilyl Groups – Cyclopentadienyl Complexes

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First NMR observation of 47Ti and 49Ti in cyclopentadienyl complexes

Cited by 24 publications

References 4 publications

Titanium(IV) Neopentoxides. X-ray Structures of Ti3(μ3-O)(μ3-Cl)(μ-OCH2CMe3)3(OCH2CMe3)6and [Ti(μ-OCH2CMe3)(OCH2CMe3)3]2

Titanium(IV) Neopentoxides. X-ray Structures of Ti3(μ3-O)(μ3-Cl)(μ-OCH2CMe3)3(OCH2CMe3)6and [Ti(μ-OCH2CMe3)(OCH2CMe3)3]2

47/49Ti NMR of some titanium compounds

Transition‐Metal Compounds Containing Alkynylsilyl Groups – Cyclopentadienyl Complexes

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Titanium(IV) Neopentoxides. X-ray Structures of Ti₃(μ₃-O)(μ₃-Cl)(μ-OCH₂CMe₃)₃(OCH₂CMe₃)₆and [Ti(μ-OCH₂CMe₃)(OCH₂CMe₃)₃]₂

Titanium(IV) Neopentoxides. X-ray Structures of Ti₃(μ₃-O)(μ₃-Cl)(μ-OCH₂CMe₃)₃(OCH₂CMe₃)₆and [Ti(μ-OCH₂CMe₃)(OCH₂CMe₃)₃]₂

^47/49Ti NMR of some titanium compounds