Abstract
The title compound, [Ru2(μ-O2CCH3)4(C5H4ClN)2]PF6·C2H4Cl2, was obtained via a rapid substitution reaction of 3-chloro-pyridine for water in [Ru2(μ-O2CCH3)4(H2O)2]PF6 in 2-propanol and subsequent crystallization from a di-chloro-ethane solution. The cationic diruthenium(II,III) tetra-acetate core lies on a crystallographic inversion center with Ru-Ru and Ru-N bond lengths of 2.2738 (3) and 2.2920 (17) Å, respectively. The Ru-Ru-N bond angle is close to linear at 176.48 (4)°, and a significant π-stacking inter-action of 3.5649 (16) Å is seen between overlapping pyridine rings of adjacent cations.
Highlights
Earlier research in our lab dealt with the chemistry of various mixed-valent diruthenium(II,III) tetraacetate complexes incorporating substituted pyridines and other, biologically relevant, heterocyclic N-donors in the axial coordination positions (Bland et al, 2005; Gilfoy et al, 2001; Minaker et al, 2011; Vamvounis et al, 2000)
The solvated title salt consists of a complex cation with a diruthenium (II,III) tetraacetate core and 3-chloropyridines in the axial positions, a hexafluoridophophate anion, and a 1,2-dichloroethane molecule of solvation (Fig. 1)
Synthesis and crystallization Synthesis of the title compound followed an earlier method developed in our lab (Vamvounis et al, 2000). [Ru2(O2CCH3)4(H2O)2]PF6 (0.100 g, 0.161 mmol) was dissolved in 10 ml of 2-propanol
Summary
Earlier research in our lab dealt with the chemistry of various mixed-valent diruthenium(II,III) tetraacetate complexes incorporating substituted pyridines and other, biologically relevant, heterocyclic N-donors in the axial coordination positions (Bland et al, 2005; Gilfoy et al, 2001; Minaker et al, 2011; Vamvounis et al, 2000). We have been able to characterize both a 3-aminopyridine diadduct (Aquino et al, 2021) and the 3-chloropyridine diadduct is reported here. This is the first crystal structure of a chloro-pyridine diadduct of a diruthenium(II,III) tetracarboxylate that we are aware of. The solvated title salt consists of a complex cation with a diruthenium (II,III) tetraacetate core and 3-chloropyridines in the axial positions, a hexafluoridophophate anion, and a 1,2-dichloroethane molecule of solvation (Fig. 1). 3-chloropyridine (0.0732 g, 0.645 mmol) was added and the solution allowed to stir for 5 min at room temperature. [Ru2(C2H3O2)4(C5H4ClN)2]PF6 909.32 Triclinic, P1 293 8.2737 (1), 10.5784 (3), 11.5534 (1) 100.764 (7), 108.980 (8), 110.525 (7) 842.27 (6) 1 Mo K 1.34 0.43 Â 0.20 Â 0.07
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