Add time:07/12/2019         Source:sciencedirect.com

The reaction of FeCl2 and xylyl isocyanide (L) (L = 2,6-Me2C6H3NC) gives two products viz. purple FeCl2L4 (1) and orange Fe2Cl5L5 (2). The structural identity of these complexes has been determined by single crystal X-ray diffraction studies. Crystal of 1 are tetragonal, space group P4nc, Z = 2, in a unit cell of dimensions a 13.853(8), c 8.803(8) Å. The structure has been refined to R 0.068 (Rw 0.071) for 613 independent reflections above background. The structure comprises octahedral FeII units with the two chlorines mutually trans. (FeCl 2.318(7), 2.288(6) Å). The four isocyanide ligands, in a cis arrangement around the metal, are essentially linear (FeCN 177.9(7), CNC 173.8(8)°). Crystals of 2 are monoclinic, space group P21/a, Z = 4, in a unit cell of dimensions a 10.310(8), b 20.468(17), c 23.026(23) Å, β 99.0(1)°. The structure has been refined to R 0.077 (Rw 0.081) for 2950 independent reflections above background. The complex is a ‘mixed’ FeII/FeIII species and consists of octahedral [FeClL5]+ cations based on FeII, and tetrahedral [FeCl4]− anions based of FeIII. For the cation, variations in FeC bond lengths between isocyanide ligands trans to one another and trans to chloride are discussed in terms of a trans-effect dominated by the strong τ-acceptor ability of the isocyanide ligands. Further comparisons are drawn with FeC bond lengths observed in 1 and in similar cationic FeII systems. The [FeCl4]− anion has tetrahedral symmetry (mean FeCl 2.157 Å, mean ClFe 109.3°). Previous studies of the tetrahedral [FeCl4]− anion (high spin feIII) show a mean FeCl of 2.180 Å.

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