Add time:09/01/2019 Source:sciencedirect.com
Crystal structures of the three geometrical isomers (1, 2 and 3) of [RuCl(2eqn)2NO] (H2eqn = 2-ethyl-8-quinolinol) have been determined by X-ray diffraction. The Cl atom is cis to the NO group in 1 and 2, and is trans to the NO group in 3. The N and O atoms of the two quinolinolato ligands for 1, 2 and 3 are in trans(N,N) and cis(O,O), in cis(N,N) and cis(O,O) and in trans(N,N) and trans(O,O) configurations, respectively. Crystallographic data for 1: triclinic, a = 10.140(4), b = 13.498(5), c = 7.902(3) Å; α = 94.08(3),β = 104.19(2), γ = 73.35(3)°, V = 1006.8(6) Å3, Z = 2, space group P1; for 2; monoclinic, a = 14.730(2), b = 10.028(2), c = 13.761(4) Å, β = 92.65(2)°, V = 2030.5(7) Å3, Z = 4, space group P21/a for 3: monoclinic, a = 14.830(4), b = 8.700(2), c = 16.711 (4) Å, β = 110.40(3)°, V = 2021,0(9) Å3, Z = 4, space group Cc. The structures were solved by the heavy-atom method and were refined by fullmatrix (1 and 2) and block-diagonal (3) least-squares procedures to R = 0.0378 (1), 0.0320 (2) and 0.0397 (3) for 5207 (1), 4032 (2) and 1675 (3) reflections with I≥3 σ(I). The variable-temperature 1H NMR spectra in dimethyl sulfoxide-d6 revealed the steric hindrance due to the ethyl group of the quinolinolato ligands, reflecting the results of the crystal structure analysis. At high temperature (373–413 K), the reversible thermal isomerizaion reaction among the three isomers was observed un degassed dimethyl sulfoxide (DMSO). The mole ratio of 1, 2 and 3 was 19:4:1 at 413 K and did not depend on the starting species. Kinetic analysis revealed that the reaction was reversible between any two isomers and the isomerization between 1 and 3 proceeded by a mechanism distinct from the others.
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