The stereospecific synthesis of Λ-α-{dipyrido[3,2-a:2′3′-c](6,7,8,9-tetrahydro)phenazine[N,N′-di(2-picolyl)-2,5-dimethyl-2S,5S-diaminocyclohexane]ruthenium(ii)} and related β-isomers†
Abstract
The conglomerate Δ,Λ-α-[Ru(picchxnMe2)(dpqC)](ClO4)2·0.5H2O and Λ-α-[Ru(S,S-picchxnMe2)(dpqC)](ClO4)2·0.5H2O (where picchxnMe2
=
N,N′-dimethyl-1,2-di(2′-picolyl)-S,S-diaminocyclohexane and dpqC = dipyrido[3,2-a:2′3′-c](6,7,8,9-tetrahydro)phenazine) have been isolated. Single crystal X-ray structures have been determined, although it was discovered only after initial data had been collected that the Δ,Λ-α-[Ru(picchxnMe2)(dpqC)](ClO4)2·0.5H2O species was in fact a conglomerate. Λ-α-[Ru(S,S-picchxnMe2)(dpqC)](ClO4)2·0.5H2O crystallises in the orthorhombic space group C2221 with a
= 15.127(2), b
= 22.976(4), c
= 25.561(7)
Å, (alternatively a
= 15.187(3), b
= 23.003(6), c
= 25. 685(7)
Å, for the separate determination of a crystal of the conglomerate), Z
= 8, and the Λ-α structure was refined to an R value of 0.059. This structure enables, for the first time, the correlation of the absolute configurations for Ru(II) complexes of the N4 tetradentate with their