Synthesis, characterization and redox properties of mixed phosphine nitroruthenium(II) complexes. Crystal structure of trans-[Ru(NO2)(terpy)-(PMe3)(PPh3)][ClO 4]·H2O

DOI: 10.1039/DT9960001463

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 1463 - 1470 (1996)

Update date:2022-08-04

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Authors:

Szczepura, Lisa F.

Kubow, Stephen A.

Leising, Randolph A.

Perez, Willie J.

Huynh, My Hang Vo

Lake, Charles H.

Churchill, David G.

Churchill, Melvyn R.

Takeuchi, Kenneth J.

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Article abstract of DOI:10.1039/DT9960001463

The mixed phosphine complexes trans-[Ru(NO₂)(terpy)(PMe₃)(PR₃)][ClO ₄] (terpy = 2,2′:6′,2″-terpyridine; R = Et, Pr, Bz or Ph) were synthesized in high yields by a stepwise addition of each phosphine. These syntheses demonstrate the utility of ruthenium(II) in the preparation of mixed phosphine complexes. The stereochemistry of trans-[Ru(NO₂)(terpy)(PMe₃)(PPh₃)][ClO ₄]·H₂O was confirmed by a single-crystal X-ray diffraction study. This species crystallizes in the monoclinic space group P2₁/c with a = 11.0199(15), b = 18.3888(28), c = 19.3089(25) A, β = 112.845(9)° and Z = 4. The two phosphine ligands are mutually trans, with P-Ru-P 177.5(1)°. The relative redox stabilities of the mixed phosphine complexes and a related series of trans-[Ru(NO₂)(terpy)(PR₃)₂][ClO₄] (R = Et, Pr, Bz or Ph) complexes were evaluated using cyclic voltammetric peak current ratios (i_pc/i_pa) for the ruthenium(III)-ruthenium(II) couples. The rate constants for nitroruthenium(III) decomposition were calculated from the i_pc/i_pa data and the contributions of electronic (E) and steric (S) factors to its rate of decomposition were determined using the relationship ln k - aE + bS + c. The average ratio of steric to electronic ligand effects on In k is approximately 30:70.

Full text of DOI:10.1039/DT9960001463

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Product name:RuCl(P(CH₃)3)(P(CH₂C₆H₅)3)(C₁₅H₁₁N₃)⁽¹⁺⁾*ClO₄^(1-) = [RuCl(P(CH₃)3)(P(CH₂C₆H₅)3)(C₁₅H₁₁N₃)]ClO₄

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