Synthesis, crystal structure and characterizations of di-μ-cyanido-1:2κ(2) N:C;2:3κ(2) C:N-bis-(4,7,13,16,21,24-hexa-oxa-1,10-di-aza-bicyclo-[8.8.8]hexacosa-ne)-1κ(8) N (1),N (10),O (4),O (7),O (13),O (16),O (21),O (24);3κ(8) N (1),N (10),O (4),O (7),O (13),O (16),O (21),O (24)-[5,10,15,20-tetra-kis-(4-chloro-phen-yl)porphyrinato-2κ(4) N]-2-iron(II)-1,3-dipotassium(I) tetra-hydro-furan disolvate with an unknown solvent.

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作者:Huang Tingting, Wang Haimang, Zhao Jianping
The title compound, [Fe(C(44)H(24)N(8)Cl(4))(CN)(2)][K(2)(C(18)H(36)N(2)O(6))(2)]·2C(4)H(8)O was synthesized and characterized by single-crystal X-ray diffraction as well as FTIR and UV-vis spectroscopy. The central Fe(II) ion is coordinated by four pyrrole N atoms of the porphyrin core and two C atoms of the cyano groups in a slightly distorted octa-hedral coordination environment. The complex mol-ecule crystallizes with two tetra-hydro-furan solvent mol-ecules, 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 C(a), C(b), C(m) and C(av) of 0.32†(3), 0.22†(3), 0.56†(2) and 0.37†(14)†à , respectively. The axial Fe-C(cyano) bond lengths are 1.991†(2) and 1.988†(2)†à . The average Fe-N(p) (N(p) is a porphyrin N atom) bond length is 1.964†(10)†à . One of the O atoms and several C atoms of the 222 moiety [222 = 4,7,13,16,21,24-hexa-oxa-1,10-di-aza-bicyclo-[8.8.8]hexa-cosa-ne] 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 mol-ecules were found to be highly disordered and their contribution to the scattering was removed using the SQUEEZE procedure in PLATON [Spek (2015 ▸). Acta Cryst. C71, 9-18], which indicated a solvent cavity of volume 372†à (3) containing approximately 83 electrons. These solvent mol-ecules are not considered in the given chemical formula and other crystal data.

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