Crystallographic report: A synthetic precursor for hetero‐binuclear metal complexes, [Ru(bpy)(dppy)2(CO)2](PF6)2 (bpy = 2,2′‐bipyridine, dppy = 2‐(diphenylphosphino)pyridine)

Ooyama, Dai; Sato, Masahito

doi:10.1002/aoc.637

Cited by 6 publications

(2 citation statements)

References 11 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…The existence of carbonyl ligands may influence the orientation of the aromatic rings of 13 because relatively short distances between the noncoordinating nitrogen atom of 13 and the carbonyl carbons are observed (3.068 Å): the analogous complex situating two 13 moieties in mutually trans positions also exhibits a similar trend as shown in Fig. 22(b) (Ooyama & Sato, 2004). …”

Section: Coordination Modesmentioning

confidence: 62%

Role of X-Ray Crystallography in Structural Studies of Pyridyl-Ruthenium Complexes

Oyama¹

2011

Current Trends in X-Ray Crystallography

View full text Add to dashboard Cite

Section: Coordination Modesmentioning

confidence: 62%

Role of X-Ray Crystallography in Structural Studies of Pyridyl-Ruthenium Complexes

Oyama¹

2011

Current Trends in X-Ray Crystallography

View full text Add to dashboard Cite

“…The diphenylpyridylphosphine ligand has been extensively studied and used as a monodentate and bidentate ligand with different metals, including Ru II (Ooyama & Sato, 2004) where the CO 2 -reducing properties of the complex were studied. Another Ru II complex with PPh 2 Py (Kumar et al, 2011) has been studied as an inhibitor of DNA-topoisomerases of the filarial parasite S. cervi.…”

Section: Database Surveymentioning

confidence: 99%

Crystal structures and Hirshfeld surface analysis of [κ²-P,N-{(C₆H₅)₂(C₅H₅N)P}Re(CO)₃Br]·2CHCl₃ and the product of its reaction with piperidine, [P-{(C₆H₅)₂(C₅H₅N)P}(C₅H₁₁N)Re(CO)₃Br]

Palominos¹,

Muñoz²,

Oyarzún³

et al. 2019

Acta Cryst E

View full text Add to dashboard Cite

The coordination of the ligands with respect to the central atom in the complex bromidotricarbonyl[diphenyl(pyridin-2-yl)phosphane-κ2 N,P]rhenium(I) chloroform disolvate, [ReBr(C17H14NP)(CO)3]·2CHCl3 or [κ2-P,N-{(C6H5)2(C5H5N)P}Re(CO)3Br]·2CHCl3, (I·2CHCl3), is best described as a distorted octahedron with three carbonyls in a facial conformation, a bromide atom, and a biting P,N-diphenylpyridylphosphine ligand. Hirshfeld surface analysis shows that C—Cl...H interactions contribute 26%, the distance of these interactions are between 2.895 and 3.213 Å. The reaction between I and piperidine (C5H11N) at 313 K in dichloromethane leads to the partial decoordination of the pyridylphosphine ligand, whose pyridyl group is replaced by a piperidine molecule, and the complex bromidotricarbonyl[diphenyl(pyridin-2-yl)phosphane-κP](piperidine-κN)rhenium(I), [ReBr(C5H11N)(C17H14NP)(CO)3] or [P-{(C6H5)2(C5H5N)P}(C5H11N)Re(CO)3Br] (II). The molecule has an intramolecular N—H...N hydrogen bond between the non-coordinated pyridyl nitrogen atom and the amine hydrogen atom from piperidine with D...A = 2.992 (9) Å. Thermogravimetry shows that I·2CHCl3 losses 28% of its mass in a narrow range between 318 and 333 K, which is completely consistent with two solvating chloroform molecules very weakly bonded to I. The remaining I is stable at least to 573 K. In contrast, II seems to lose solvent and piperidine (12% of mass) between 427 and 463 K, while the additional 33% loss from this last temperature to 573 K corresponds to the release of 2-pyridylphosphine. The contribution to the scattering from highly disordered solvent molecules in II was removed with the SQUEEZE routine [Spek (2015). Acta Cryst. C71, 9-18] in PLATON. The stated crystal data for M r, μ etc. do not take this solvent into account.

show abstract

Routes to Ruthenium–Fluoro Cations of the Type [RuL₂(CO)_nF]⁺ (n = 2,3; L = PR₃, NHC): A Play‐Off between Solvent, L and Weakly Coordinating Anion

et al. 2010

View full text Add to dashboard Cite

Interaction of cis,cis,trans‐[RuF2(CO)2(PPh3)2] (1a) with BF3 in acetonitrile affords the dicationic adduct [Ru(NCMe)2(CO)2(PPh3)2](BF4)(B2F7) (2), which can be readily carbonylated to form [Ru(CO)4(PPh3)2](BF4)2 (3). In contrast, reaction of 1a with BF3 in dichloromethane leads to the neutral ruthenium–fluoro species [RuF(FBF3)(CO)2(PPh3)2] (4); facile displacement of the bound FBF3 ligand in 4 occurs on treatment with CO or PPh3 to afford cationic [RuF(CO)2(L)(PPh3)2](BF4) [L = CO (5a), PPh3 (5b)]. On the other hand, reaction of 1a with PF5 in dichloromethane furnishes the coordinatively unsaturated 16‐electron salt [RuF(CO)2(PPh3)2](PF6) (6). Metathesis of the PF6 anion in 6 with KB(ArF)4 [ArF = 3,5‐(CF3)2C6H3] in dichloromethane results in rapid decomposition, while in the presence of CO solvent exchange (CH2Cl2) takes place to yield chloride‐containing [RuCl(CO)3(PPh3)2][B(ArF)4] (7). Unexpectedly, 1a proved unreactive towards tris(pentafluorophenyl)borane in dichloromethane. However, by substituting the triphenylphosphane ligands in 1a with better donor phosphanes or with an N‐heterocyclic carbene (NHC) [to give cis,cis,trans‐[RuF2(CO)2(L)2] [L = PEt2Ph (1b), P(CCPh)Ph2 (1c), IPr (1,3‐bis(2,6‐diisopropylphenyl)imidazol‐2‐ylidene) (1d)], fluoride abstraction could be achieved using B(C6F5)3 to give 16‐electron [RuF(CO)2(L)2][FB(C6F5)3] (L = PEt2Ph (8b), P(CCPh)Ph2 (8c), IPr (8d)]. Carbonylation of 8d proceeds smoothly to generate the coordinatively saturated species [RuF(CO)3(IPr)2][FB(C6F5)3] (9) in high yield. Single crystal X‐ray structures are presented for 2, 3, 5a/3, 7 and 9.

show abstract

Crystallographic report: A synthetic precursor for hetero‐binuclear metal complexes, [Ru(bpy)(dppy)₂(CO)₂](PF₆)₂ (bpy = 2,2′‐bipyridine, dppy = 2‐(diphenylphosphino)pyridine)

Cited by 6 publications

References 11 publications

Role of X-Ray Crystallography in Structural Studies of Pyridyl-Ruthenium Complexes

Role of X-Ray Crystallography in Structural Studies of Pyridyl-Ruthenium Complexes

Crystal structures and Hirshfeld surface analysis of [κ²-P,N-{(C₆H₅)₂(C₅H₅N)P}Re(CO)₃Br]·2CHCl₃ and the product of its reaction with piperidine, [P-{(C₆H₅)₂(C₅H₅N)P}(C₅H₁₁N)Re(CO)₃Br]

Routes to Ruthenium–Fluoro Cations of the Type [RuL₂(CO)_nF]⁺ (n = 2,3; L = PR₃, NHC): A Play‐Off between Solvent, L and Weakly Coordinating Anion

Contact Info

Product

Resources

About

Crystallographic report: A synthetic precursor for hetero‐binuclear metal complexes, [Ru(bpy)(dppy)2(CO)2](PF6)2 (bpy = 2,2′‐bipyridine, dppy = 2‐(diphenylphosphino)pyridine)

Cited by 6 publications

References 11 publications

Role of X-Ray Crystallography in Structural Studies of Pyridyl-Ruthenium Complexes

Role of X-Ray Crystallography in Structural Studies of Pyridyl-Ruthenium Complexes

Crystal structures and Hirshfeld surface analysis of [κ2-P,N-{(C6H5)2(C5H5N)P}Re(CO)3Br]·2CHCl3 and the product of its reaction with piperidine, [P-{(C6H5)2(C5H5N)P}(C5H11N)Re(CO)3Br]

Routes to Ruthenium–Fluoro Cations of the Type [RuL2(CO)nF]+ (n = 2,3; L = PR3, NHC): A Play‐Off between Solvent, L and Weakly Coordinating Anion

Contact Info

Product

Resources

About

Crystallographic report: A synthetic precursor for hetero‐binuclear metal complexes, [Ru(bpy)(dppy)₂(CO)₂](PF₆)₂ (bpy = 2,2′‐bipyridine, dppy = 2‐(diphenylphosphino)pyridine)

Crystal structures and Hirshfeld surface analysis of [κ²-P,N-{(C₆H₅)₂(C₅H₅N)P}Re(CO)₃Br]·2CHCl₃ and the product of its reaction with piperidine, [P-{(C₆H₅)₂(C₅H₅N)P}(C₅H₁₁N)Re(CO)₃Br]

Routes to Ruthenium–Fluoro Cations of the Type [RuL₂(CO)_nF]⁺ (n = 2,3; L = PR₃, NHC): A Play‐Off between Solvent, L and Weakly Coordinating Anion