Synthesis and Characterization of Dibromo-Containing Ruthenium(IV) η3-Allyl and Ruthenium(IV) η4-Diene Complexes. Formation of [Ru(η5-C5Me5)Br3]- and [Ru(η5-C5Me5)Br3]2

Gemel, Christian; Mereiter, Kurt; Schmid, Roland; Kirchner, Karl

doi:10.1021/om950662a

Cited by 42 publications

(25 citation statements)

References 30 publications

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“…The structural parameters of the cation in (I) are similar to those reported for other [(arene)RuCp*] + complexes (Gemel et al, 1996;Navarro Clemente et al, 2002;Loughrey et al, 2008) with Ru-C distances of 2.177 (4)-2.196 (3) Å (Cp*) and 2.193 (3)-2.240 (3) Å (Ph). The average value of 1.41 (1) Å for the C-C bond lengths in the benzene ring is 0.02Å longer than the average of 1.39 (1) Å observed for the parent sulfonamide (Zerbe et al, 2005), while the bond lengths in the SO 2 NH 2 groups do not differ significantly.…”

supporting

confidence: 79%

(η⁵-Pentamethylcyclopentadienyl)(η⁶-p-toluenesulfonamide)ruthenium(II) tetraphenylborate

et al. 2008

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The crystal structure of the title compound, [Ru(C10H15)(C7H9NO2S)]C24H20B, has been determined as part of our investigation into the structural and biological properties of organometallic RuII–arene–Cp* complex salts of the type [R-PhRuCp*]+·X − (where Cp* is pentamethylcyclopentadiene). Tethering the RuCp* group to the benzene ring of p-toluenesulfonamide results in only minor changes to the molecular geometry of the sulfonamide, but, together with crystallization as the [BPh4]− salt, effectively blocks involvement of the sulfonamide group in N—H⋯O hydrogen-bonding networks.

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supporting

confidence: 79%

(η⁵-Pentamethylcyclopentadienyl)(η⁶-p-toluenesulfonamide)ruthenium(II) tetraphenylborate

et al. 2008

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“…The five mem bered rings Cp and C 3 B 2 are in the staggered conforma tion. The Ru···C 6 distance (1.705 Å) is similar to analo gous distances in the [Cp*Ru(C 6 H 6 )] + cation (1.710 Å) 9 and triple decker complex CpCo(C 2 B 3 Et 2 H 3 )Ru(p cymene) (1.698 Å). 10 The analysis of the unit cell packing of the [2b]PF 6 molecules shows that cations 2b and anions PF 6 -form mutually alternating layers (Fig.…”

Section: Resultssupporting

confidence: 53%

Synthesis of μ-diborolyl triple-decker complexes [CpCo(1,3-C3B2Me5)Ru(arene)]+

et al. 2009

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Cationic triple decker complexes [CpCo(1,3 C 3 B 2 Me 5 )Ru(arene)]PF 6 (arene is benzene (2a), p cymene (2b)) with a bridging diborolyl ligand were synthesized by the reaction of the sand wich anion [CpCo(1,3 C 3 B 2 Me 5 )] -(1) with [(arene)RuCl 2 ] 2 . The structure of [2b]PF 6 was confirmed by X ray diffraction analysis.The main method for the preparation of cationic triple decker complexes is the electrophilic stacking of sand wich compounds with the cationic fragments [(ring)M] n+ (n = 1, 2). 1-5 We have previously studied the reaction of the sandwich anion [CpCo(1,3 C 3 B 2 Me 5 )] -(1) with the monocationic half sandwich fragments [(C 5 R 5 )Ru] + (R = H, Me), resulting in the formation of the neutral triple decker complexes CpCo(1,3 C 3 B 2 Me 5 )Ru(C 5 R 5 ). 6 We have recently shown 7 that the similar reaction of an ion 1 with the dicationic fragments [(C 5 R 5 )M] 2+ (R = H, Me; M = Rh, Ir) affords the cationic triple decker complexes [CpCo(1,3 C 3 B 2 Me 5 )M(C 5 R 5 )] + . In the present work, we describe the reactions of sandwich anion 1 with the species [(arene)Ru] 2+ . Results and DiscussionThe reaction of the thallium derivative of anion 1 with the chloride complexes [(arene)RuCl 2 ] 2 (acting as equiva lents of the species [(arene)Ru] 2+ ) in acetonitrile afforded cationic triple decker complexes 2a,b in 60-75% yields (Scheme 1).* The behavior of anion 1 in this reaction resembles that of the cyclopentadienide anion reacting with [(C 6 H 6 )RuCl 2 ] 2 with the formation of [CpRu(C 6 H 6 )] + . 8 Hexafluorophosphates and tetraphenylborates of cat ions 2a,b are brightly colored solid substances stable in air. These salts are well soluble in polar organic solvents, such as CH 2 Cl 2 and acetone. Their structures were con Scheme 1 R 1 = R 2 = H (2a); R 1 = Me, R 2 = Pr i (2b).

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“…The formation of the η 3 complex was unexpected for the synthetic route employed, but its formulation was supported by the complete characterization of the analogous oxopentadienyl Ru(IV) complex [Cp*Ru(Cl) 2 ( syn -η 3 -CH 2 CMeCHCMeO)], formed through formal oxidative addition of chlorine atoms (from CHCl 3 ) to Cp*Ru(η 5 -2,4-dimethyloxopentadienyl) . Similar complexes have also been prepared, such as Cp*Ru(Cl) 2 (η 3 -2,4-dimethylpentadienyl), Cp*Ru(Br) 2 ( syn -η 3 -CH 2 CHCHCHCHMe), and Cp*Ru(Br) 2 ( anti -η 3 -CH 2 CHCHCHO) …”

Section: Resultsmentioning

confidence: 93%

Reactions of Enimines with [Cp*RuCl]₄: Half-Open Ruthenocene and Related Species Incorporating Heteroatoms

Gutiérrez¹,

Clemente²,

Paz-Sandoval³

et al. 1999

Organometallics

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The reactions of enimines and various silicon, germanium, and tin derivatives with [Cp*RuCl]4 have been investigated and found to lead to a variety of products, depending on the nature of the enimine and the reaction conditions. In general, mixtures of products were obtained comprised of Cp*Ru(η5-azadienyl), Cp*Ru(η3-azadienyl)Cl2, and Cp*Ru(η4-amino-1,3-diene)Cl complexes. Significant differences in both product preferences and overall yields were observed between the silicon, germanium, and tin reagents, the last typically favoring the η5 complexes. The choice of solvent also played a major role, the η5 complex being slightly to somewhat disfavored in THF relative to benzene. An attempt to convert an η4-aminodiene complex, Cp*Ru[η4-CH3CHCHC(CH3)CHNH(t-Bu)], to an η5-azadienyl complex through reaction with Ag+ in the presence of K2CO3 led to a mixture of species, which included the desired η5 complex as well as an unusual Cp*Ru(η3-dienimine)Cl species, which arose from a formal two-electron oxidation followed by two deprotonations, from the nitrogen center and the internal methyl group. Coordination in this species occurs through the nitrogen center and the distal olefin. Structural confirmation for this species, as well as for one η4 and three η5 complexes, has been obtained.

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Synthesis and Characterization of Dibromo-Containing Ruthenium(IV) η³-Allyl and Ruthenium(IV) η⁴-Diene Complexes. Formation of [Ru(η⁵-C₅Me₅)Br₃]^- and [Ru(η⁵-C₅Me₅)Br₃]₂

Cited by 42 publications

References 30 publications

(η⁵-Pentamethylcyclopentadienyl)(η⁶-p-toluenesulfonamide)ruthenium(II) tetraphenylborate

(η⁵-Pentamethylcyclopentadienyl)(η⁶-p-toluenesulfonamide)ruthenium(II) tetraphenylborate

Synthesis of μ-diborolyl triple-decker complexes [CpCo(1,3-C3B2Me5)Ru(arene)]+

Reactions of Enimines with [Cp*RuCl]₄: Half-Open Ruthenocene and Related Species Incorporating Heteroatoms

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Synthesis and Characterization of Dibromo-Containing Ruthenium(IV) η3-Allyl and Ruthenium(IV) η4-Diene Complexes. Formation of [Ru(η5-C5Me5)Br3]- and [Ru(η5-C5Me5)Br3]2

Cited by 42 publications

References 30 publications

(η5-Pentamethylcyclopentadienyl)(η6-p-toluenesulfonamide)ruthenium(II) tetraphenylborate

(η5-Pentamethylcyclopentadienyl)(η6-p-toluenesulfonamide)ruthenium(II) tetraphenylborate

Synthesis of μ-diborolyl triple-decker complexes [CpCo(1,3-C3B2Me5)Ru(arene)]+

Reactions of Enimines with [Cp*RuCl]4: Half-Open Ruthenocene and Related Species Incorporating Heteroatoms

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Synthesis and Characterization of Dibromo-Containing Ruthenium(IV) η³-Allyl and Ruthenium(IV) η⁴-Diene Complexes. Formation of [Ru(η⁵-C₅Me₅)Br₃]^- and [Ru(η⁵-C₅Me₅)Br₃]₂

(η⁵-Pentamethylcyclopentadienyl)(η⁶-p-toluenesulfonamide)ruthenium(II) tetraphenylborate

(η⁵-Pentamethylcyclopentadienyl)(η⁶-p-toluenesulfonamide)ruthenium(II) tetraphenylborate

Reactions of Enimines with [Cp*RuCl]₄: Half-Open Ruthenocene and Related Species Incorporating Heteroatoms