The novel six-coordinate iron(II) complex [Fe II (tpy) 2 ][Fe III (Tp)(CN) 3 ] 2 ·2MeOH (1) was prepared, and its structure was successfully determined by single-crystal X-ray analysis. The compound is triclinic, space group P-1, with two molecules in a unit cell of dimensions a = 8.9547 (16) Å, b = 14.450(3) Å, c = 23.098(5) Å, α = 88.090(11)°, β = 88.822(10)°and γ = 79.093(7)°. The crystal structure of 1 consists of a six-nitrogen-coordinate iron(II) cation, two [Fe III (Tp)(CN) 3 ]¯anions

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... two crystallization methanol molecules. The ligand-metal distances of Fe(II)-N, Fe(III)-N Tp and Fe(III)-C CN indicate that Fe(II) and Fe(III) assume low-spin (LS) states. The magnetic susceptibility measurement shows that the value of χ m T is 1.86 cm 3 Kmol −1 at room temperature, which is consistent with the presence of one Fe(II) LS and two Fe(III) LS moieties.