Metallocen-chemie hochfluorierter ligand-systeme XI. Synthese und charakterisierung von Cp2Ti(SbF6)2 und Cp2Ti(Sb2F11)2; struktur von Cp2Ti(SbF6)2 und Cp2V(SbF6)2

Gowik, Petra; Klapötke, Thomas M.; Thewalt, Ulf

doi:10.1016/0022-328x(90)85005-j

Cited by 16 publications

(8 citation statements)

References 9 publications

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“…77,78 Compounds 33 and 34 are isostructural. 79 The increase in Ti-F bond distance for 33 is reflected in a lowering of the ν Ti-F vibration by ∼30 cm -1 . Compounds 33 and 34 appear to be thermodynamically unstable with respect to decomposition processes involving formation of transition metal- In this case the Cp 2 Ti 2+ fragment attains an 18-electron configuration by coordinating three acetonitriles.…”

Section: Titanium(iv) Metallocenesmentioning

confidence: 98%

See 1 more Smart Citation

Organometallic Fluorides: Compounds Containing Carbon−Metal−Fluorine Fragments of d-Block Metals

1997

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Section: Titanium(iv) Metallocenesmentioning

confidence: 98%

“…On the basis of conductivity measurements they may be associated in dichloromethane solution , Compounds 33 and 34 are isostructural . The increase in Ti−F bond distance for 33 is reflected in a lowering of the ν Ti - F vibration by ∼30 cm -1 .…”

Section: A Titanium(iv)1 Titanium(iv) Metallocenesmentioning

confidence: 99%

Organometallic Fluorides: Compounds Containing Carbon−Metal−Fluorine Fragments of d-Block Metals

1997

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“…The V1-F1 distance of 2.008(2)Å is slightly shorter than the V-F distances in V( (1) and 2.04(1)Å, resp.) [9,10], which likely reflects the high Lewis acidities of AsF 5 and SbF 5 .…”

Section: Resultsmentioning

confidence: 99%

“…For vanadium, the dichloride [1], dibromide [2], and diiodide [3] are all known and the dibromide [4], the dichloride, and some alkyl-substituted analogues [5][6][7][8] have been crystallographically characterized. No structures have been reported for any mixed species, nor for fluoride complexes, with the exception of species having two AsF 5 or SbF 5 fragments linked to the fluorides [9,10]. Herein a reaction product isolated from an attempt to generate a mixed V(C 5 H 5 ) 2 BrF complex is reported.…”

Section: Introductionmentioning

confidence: 99%

Solid State Structure of Bis[(bromo)(dicyclopentadienyl)vanadium(μ₂-fluoro)][(bromo)(cyclopentadienyl)vanadium][tetrafluoroborate]

Chan

Arif

Ernst

2015

Journal of Crystallography

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− has been isolated from the reaction of vanadocene monobromide with the ferrocenium cation. The complex is a mixed valence compound composed of two V(IV) and one V(III) centers. The V(III) center has one cyclopentadienyl ligand in its coordination sphere, as well as a bromide and two fluoride ligands. Each fluoride ligand is also attached to one of the V(IV) centers, which additionally is coordinated by a bromide and two cyclopentadienyl ligands. The complex crystallizes in the monoclinic space group 2 1 / , with = 7.66490(10)Å, = 15.2457(2)Å, = 13.3185(2)Å, and = 101.2721(8) ∘ at 150(1) K.

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“…Extensive investigations by Thewalt and co-workers of complexes of the type Cp 2 Ti(CF 3 SO 3 ) 2 and Cp 2 Ti(NO 3 ) 2 showed that the bonding in these complexes is predominantly covalent. Using more weakly coordinating anions, Cp 2 Ti(PF 6 ) 2 was synthesized and characterized in solution, and notably, Cp 2 Ti(AsF 6 ) 2 and Cp 2 Ti(SbF 6 ) 2 were synthesized and structurally characterized by Klapötke, Thewalt, and co-workers, which opened up this area of chemistry. Whereas salts containing the AsF 6 - or SbF 6 - counteranions were prepared on a gram scale by the straightforward reaction of Cp 2 TiCl 2 with AgEF 6 (E = As, Sb) in SO 2 solution (eq 1), , attempts to isolate Cp 2 Ti(PF 6 ) 2 and Cp 2 Ti(BF 4 ) 2 derived from the weaker Lewis acids BF 3 and PF 5 in the solid state were unsuccessful …”

Section: Introductionmentioning

confidence: 99%

Facile Synthesis and Structural Characterization of [Cp₂Ti^IV(NCX)₂][AsF₆]₂ Complexes: Adducts of Cp₂Ti(AsF₆)₂ with Halogen Cyanides (X = Cl, Br, I)

et al. 2005

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A series of adducts between the highly reactive dicationic Cp 2 Ti IV 2+ center and the weak Lewis base halogen cyanides (ClCN, BrCN, ICN) have been prepared in a facile synthesis and in quantitative yields from the reaction of Cp 2 Ti(AsF 6 ) 2 with ClCN, BrCN, or ICN in liquid SO 2 . The extremely air-sensitive Cp 2 Ti(NCX) 2 (AsF 6 ) 2 (X ) Cl (1), Br (2), I (3)) complexes were characterized using IR and 1 H, 14 N, 19 F, and 75 As NMR spectroscopy, as well as X-ray diffraction. The structures of 1-3 were determined using X-ray diffraction techniques. The synthetic route employed should generally be applicable for the synthesis of a range of new cationic Cp 2 Ti IV L 2 2+ (L ) neutral ligand) species using anhydrous conditions and demonstrates the usefulness of liquid SO 2 as a solvent for such systems. Compounds 1-3 are the first structurally characterized Cp 2 Ti IV L 2 (EF 6 ) 2 (L ) neutral ligand; E ) As, Sb) complexes with the weakly coordinating AsF 6 -anion and are also the first adducts between cationic Cp 2 M x+ (M ) transition metal) centers and the halogen cyanides, which are weak Lewis bases in comparison with other nitriles such as CH 3 CN.

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Metallocen-chemie hochfluorierter ligand-systeme XI. Synthese und charakterisierung von Cp2Ti(SbF6)2 und Cp2Ti(Sb2F11)2; struktur von Cp2Ti(SbF6)2 und Cp2V(SbF6)2

Cited by 16 publications

References 9 publications

Organometallic Fluorides: Compounds Containing Carbon−Metal−Fluorine Fragments of d-Block Metals

Organometallic Fluorides: Compounds Containing Carbon−Metal−Fluorine Fragments of d-Block Metals

Solid State Structure of Bis[(bromo)(dicyclopentadienyl)vanadium(μ₂-fluoro)][(bromo)(cyclopentadienyl)vanadium][tetrafluoroborate]

Facile Synthesis and Structural Characterization of [Cp₂Ti^IV(NCX)₂][AsF₆]₂ Complexes: Adducts of Cp₂Ti(AsF₆)₂ with Halogen Cyanides (X = Cl, Br, I)

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Metallocen-chemie hochfluorierter ligand-systeme XI. Synthese und charakterisierung von Cp2Ti(SbF6)2 und Cp2Ti(Sb2F11)2; struktur von Cp2Ti(SbF6)2 und Cp2V(SbF6)2

Cited by 16 publications

References 9 publications

Organometallic Fluorides: Compounds Containing Carbon−Metal−Fluorine Fragments of d-Block Metals

Organometallic Fluorides: Compounds Containing Carbon−Metal−Fluorine Fragments of d-Block Metals

Solid State Structure of Bis[(bromo)(dicyclopentadienyl)vanadium(μ2-fluoro)][(bromo)(cyclopentadienyl)vanadium][tetrafluoroborate]

Facile Synthesis and Structural Characterization of [Cp2TiIV(NCX)2][AsF6]2 Complexes: Adducts of Cp2Ti(AsF6)2 with Halogen Cyanides (X = Cl, Br, I)

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Solid State Structure of Bis[(bromo)(dicyclopentadienyl)vanadium(μ₂-fluoro)][(bromo)(cyclopentadienyl)vanadium][tetrafluoroborate]

Facile Synthesis and Structural Characterization of [Cp₂Ti^IV(NCX)₂][AsF₆]₂ Complexes: Adducts of Cp₂Ti(AsF₆)₂ with Halogen Cyanides (X = Cl, Br, I)