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Single crystals of a new polymorph of 4`-tolyl-2,2`:6`,2 ``-terpyridine (ttpy) have been grown by evaporation of a hexane-ethyl acetate solution of the ligand; the packing features weak pi-stacking and N-Pyridine...HC interactions between stacks of ttpy molecules. Improved syntheses of [M(ttpy)(2)][PFr](2) (M = Fe, Ru), and the single crystal structures of [Fe(ttpy)(2)][PF6](2)center dot 2.2MeCN and [Ru(ttpy)21[PF6](2)center dot 1.75MeCN center dot 0.2H(2)O are reported.
