Synthesis, crystal structure and characterizations of di-μ-cyanido-1:2κ2N:C;2:3κ2C:N-bis(4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane)-1κ8N1,N10,O4,O7,O13,O16,O21,O24;3κ8N1,N10,O4,O7,O13,O16,O21,O24-[5,10,15,20-tetrakis(4-chlorophenyl)porphyrinato-2κ4N]-2-iron(II)-1,3-dipotassium(I) tetrahydrofuran disolvate with an unknown solvent

Abstract

The title compound, [Fe(C44H24N8Cl4)(CN)2][K2(C18H36N2O6)2]·2C4H8O was synthesized and characterized by single-crystal X-ray diffraction as well as FTIR and UV–vis spectroscopy. The central FeIIion is coordinated by four pyrrole N atoms of the porphyrin core and two C atoms of the cyano groups in a slightly distorted octahedral coordination environment. The complex molecule crystallizes with two tetrahydrofuran solvent molecules, one of which was refined as disordered over two sets of sites with refined occupancies of 0.619 (5) and 0.381 (5). It has a distorted porphyrin core with mean absolute core-atom displacements Ca, Cb, Cmand Cavof 0.32 (3), 0.22 (3), 0.56 (2) and 0.37 (14) Å, respectively. The axial Fe—Ccyanobond lengths are 1.991 (2) and 1.988 (2) Å. The average Fe—Np(Npis a porphyrin N atom) bond length is 1.964 (10) Å. One of the O atoms and several C atoms of the 222 moiety [222 = 4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane] were refined as disordered over two sets of sites with occupancy ratios of 0.739 (6):0.261 (6) and 0.832 (4):0.168 (4). Additional solvent molecules were found to be highly disordered and their contribution to the scattering was removed using the SQUEEZE procedure inPLATON[Spek (2015).Acta Cryst. C71, 9–18], which indicated a solvent cavity of volume 372 Å3containing approximately 83 electrons. These solvent molecules are not considered in the given chemical formula and other crystal data.