Reactions of 0.5 equivalent of the dinuclear complexes [(η⁶-arene)Ru(μ-Cl)Cl]₂ (arene = η⁶-C₆H₆, η⁶-p-ⁱPrC₆H₄Me) and [(Cp^*)M(μ-Cl)Cl]₂ (M = Rh, Ir; Cp^* = η⁵-C₅Me₅) with 4,6-disubstituted pyrazolyl-pyrimidine ligands (L) viz. 4,6-bis(pyrazolyl)pyrimidine (L1), 4,6-bis(3-methyl-pyrazolyl)pyrimidine (L2), 4,6-bis(3,5-dimethyl-pyrazolyl)pyrimidine (L3) lead to the formation of the cationic mononuclear complexes [(η⁶-C₆H₆)Ru(L)Cl]⁺ (L = L1, 1; L2, 2; L3, 3), [(η⁶-p-ⁱPrC₆H₄Me)Ru(L)Cl]⁺ (L = L1, 4; L2, 5; L3, 6), [(Cp^*)Rh(L)Cl]⁺ (L = L1, 7; L2, 8; L3, 9) and [(Cp^*)Ir(L)Cl]⁺ (L = L1, 10; L2, 11; L3, 12).In contrast, reactions with 1.0 equivalent of the dinuclear complexes [(η⁶-arene)Ru(μ-Cl)Cl]₂ and [(Cp^*)M(μ-Cl)Cl]₂ give rise to the dicationic dinuclear complexes [{(η⁶-C₆H₆)RuCl}₂(L)]²⁺ (L = L1, 13; L2, 14; L3, 15), [{(η⁶-p-ⁱPrC₆H₄Me)RuCl}₂(L)]²⁺ (L = L1, 16; L2, 17; L3, 18), [{(Cp^*)RhCl}₂(L)]²⁺ (L = L1, 19; L2, 20; L3, 21) and [{(Cp^*)IrCl}₂(L)]²⁺ (L = L1 22; L2, 23; L3 24).The mol. structures of [3]PF₆, [6]PF₆ , [7]PF₆ and [18](PF₆)₂ have been established by single crystal x-ray structure anal.

01 Jan 2008·Inorganic ChemistryQ2 · CHEMISTRY

Self-assembly of Ligands Designed for the Building of a New Type of [2 × 2] Metallic Grid. Anion Encapsulation and Diffusion NMR Spectroscopy

Q2 · CHEMISTRY

Article

Author: Maestro, Miguel A. ; Elguero, José ; Mereiter, Kurt ; Claridge, Tim D. W. ; Ortiz, Isabel M. ; Jalón, Félix A. ; Soriano, M. Laura ; Manzano, Blanca R. ; Gómez de la Torre, Felipe

The ligands 4,6-bis(pyrazol-1-yl)pyrimidine (bpzpm), 4,6-bis(3,5-dimethylpyrazol-1-yl)pyrimidine (bpz(*)pm), 4,6-bis(4-methylpyrazol-1-yl)pyrimidine (Mebpzpm), and 3,6-bis(3,5-dimethylpyrazol-1-yl)pyridazine (ppdMe) were synthesized and were made to react with Cu(I) centers in the presence of different counteranions. Different [2 x 2] metallic grids were obtained. With ligands bpzpm, bpz*pm, and Mebpzpm, a new type of grid was obtained where the facing ligands were divergent and two counteranions (BF(4-) or PF(6-)) were hosted in the resulting cavities and exhibit C-H...F and anion...pi interactions in the solid state. The presence of methyl groups on the pyrazolyl rings induced several distortions in the structure. In complexes with the ligand ppdMe, there were found two groups of parallel ligands in the grid, and the cavities generated were smaller. The counteranions were situated outside the grid, and the facing ligands exhibited aromatic pi-pi stacking interactions. Anion-pi interactions involving the pyridazine ring were found. The behavior in solution of the new derivatives with a special emphasis on the cation-anion interactions was studied by UV-vis and NMR spectroscopy. Diffusion NMR experiments performed for some complexes allowed us to conclude that weak cation-anion interactions exist in solution, with the counteranions undergoing fast exchange on the diffusion time scale between the free and ion-paired states.

01 Jan 2001·New Journal of Chemistry

New complexes with pyrazole-containing ligands and different metallic centres. Comparative study of their fluxional behaviour involving M–N bond rupture

Author: Jose′ Elguero ; Ana Guerrero ; Antonio de la Hoz ; Felipe Gómez de la Torre ; Blanca R. Manzano ; Fe′lix A. Jalón ; Ana Rodríguez

New complexes of palladium(II), silver(I), copper(I) and ruthenium(II) containing the ligands 2-(pyrazol-1-yl)pyridine (pzpy), 2-(pyrazol-1-yl)pyrimidine (pzpm), 2-(3,5-dimethylpyrazol-1-yl)pyrimidine (pz^*pm) and 4,6-bis(pyrazol-1-yl)-pyrimidine (bpzpm) were prepared and characterized.Only the isomer with the least steric hindrance was found for the derivatives PdClR(N-N'), R = Me or COMe, N-N' = pzpy or pzpm, while the two possible isomers were found for similar derivatives with pz^*pm.In the reaction of [RuCl₂(cod)]_n with pzpy, pzpm and bpzpm, the isomer trans-RuCl₂(cod)(N-N') was always formed.Three different isomers were consecutively formed after the reaction of RuCl₂(PPh₃)₃ with bpzpm, with the thermodynamically stable isomer being cis,trans-RuCl₂(PPh₃)₂(bpzpm).A fluxional process involving interchange of the H₄/H₆ pyrimidine protons, which implies M-N(pm) bond rupture, was found in the silver, copper and some palladium derivativesSuch an interchange was not observed in the ruthenium complexes.The trans influence of the group situated trans to the pyrimidine ring is extremely important for Pd-N bond rupture.The isomer interconversion for the derivatives PdClR(pz^*pm), R = Me or COMe, was studied by variable temperature ¹H NMR studies.The process is of higher energy than the H₄/H₆ interchange and is facilitated by the presence of the acyl group.

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