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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-hexa­oxa-1,10-di­aza­bicyclo­[8.8.8]hexacosa­ne)-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-tetra­kis­(4-chloro­phen­yl)porphyrinato-2κ(4) N]-2-iron(II)-1,3-dipotassium(I) tetra­hydro­furan disolvate with an unknown solvent

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 at...

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Autores principales: Huang, Tingting, Wang, Haimang, Zhao, Jianping
Formato: Online Artículo Texto
Lenguaje:English
Publicado: International Union of Crystallography 2019
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC6895954/
https://www.ncbi.nlm.nih.gov/pubmed/31871757
http://dx.doi.org/10.1107/S2056989019014841
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author Huang, Tingting
Wang, Haimang
Zhao, Jianping
author_facet Huang, Tingting
Wang, Haimang
Zhao, Jianping
author_sort Huang, Tingting
collection PubMed
description 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 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 C(a), C(b), C(m) and C(av) of 0.32 (3), 0.22 (3), 0.56 (2) and 0.37 (14) Å, respectively. The axial Fe—C(cyano) bond lengths are 1.991 (2) and 1.988 (2) Å. The average Fe—N(p) (N(p) is 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 in PLATON [Spek (2015 ▸). Acta Cryst. C71, 9–18], which indicated a solvent cavity of volume 372 Å(3) containing approximately 83 electrons. These solvent mol­ecules are not considered in the given chemical formula and other crystal data.
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spelling pubmed-68959542019-12-23 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-hexa­oxa-1,10-di­aza­bicyclo­[8.8.8]hexacosa­ne)-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-tetra­kis­(4-chloro­phen­yl)porphyrinato-2κ(4) N]-2-iron(II)-1,3-dipotassium(I) tetra­hydro­furan disolvate with an unknown solvent Huang, Tingting Wang, Haimang Zhao, Jianping Acta Crystallogr E Crystallogr Commun Research Communications 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 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 C(a), C(b), C(m) and C(av) of 0.32 (3), 0.22 (3), 0.56 (2) and 0.37 (14) Å, respectively. The axial Fe—C(cyano) bond lengths are 1.991 (2) and 1.988 (2) Å. The average Fe—N(p) (N(p) is 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 in PLATON [Spek (2015 ▸). Acta Cryst. C71, 9–18], which indicated a solvent cavity of volume 372 Å(3) containing approximately 83 electrons. These solvent mol­ecules are not considered in the given chemical formula and other crystal data. International Union of Crystallography 2019-11-26 /pmc/articles/PMC6895954/ /pubmed/31871757 http://dx.doi.org/10.1107/S2056989019014841 Text en © Huang et al. 2019 http://creativecommons.org/licenses/by/4.0/ This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.http://creativecommons.org/licenses/by/4.0/
spellingShingle Research Communications
Huang, Tingting
Wang, Haimang
Zhao, Jianping
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-hexa­oxa-1,10-di­aza­bicyclo­[8.8.8]hexacosa­ne)-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-tetra­kis­(4-chloro­phen­yl)porphyrinato-2κ(4) N]-2-iron(II)-1,3-dipotassium(I) tetra­hydro­furan disolvate with an unknown solvent
title 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-hexa­oxa-1,10-di­aza­bicyclo­[8.8.8]hexacosa­ne)-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-tetra­kis­(4-chloro­phen­yl)porphyrinato-2κ(4) N]-2-iron(II)-1,3-dipotassium(I) tetra­hydro­furan disolvate with an unknown solvent
title_full 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-hexa­oxa-1,10-di­aza­bicyclo­[8.8.8]hexacosa­ne)-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-tetra­kis­(4-chloro­phen­yl)porphyrinato-2κ(4) N]-2-iron(II)-1,3-dipotassium(I) tetra­hydro­furan disolvate with an unknown solvent
title_fullStr 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-hexa­oxa-1,10-di­aza­bicyclo­[8.8.8]hexacosa­ne)-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-tetra­kis­(4-chloro­phen­yl)porphyrinato-2κ(4) N]-2-iron(II)-1,3-dipotassium(I) tetra­hydro­furan disolvate with an unknown solvent
title_full_unstemmed 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-hexa­oxa-1,10-di­aza­bicyclo­[8.8.8]hexacosa­ne)-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-tetra­kis­(4-chloro­phen­yl)porphyrinato-2κ(4) N]-2-iron(II)-1,3-dipotassium(I) tetra­hydro­furan disolvate with an unknown solvent
title_short 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-hexa­oxa-1,10-di­aza­bicyclo­[8.8.8]hexacosa­ne)-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-tetra­kis­(4-chloro­phen­yl)porphyrinato-2κ(4) N]-2-iron(II)-1,3-dipotassium(I) tetra­hydro­furan disolvate with an unknown solvent
title_sort 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-hexa­oxa-1,10-di­aza­bicyclo­[8.8.8]hexacosa­ne)-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-tetra­kis­(4-chloro­phen­yl)porphyrinato-2κ(4) n]-2-iron(ii)-1,3-dipotassium(i) tetra­hydro­furan disolvate with an unknown solvent
topic Research Communications
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC6895954/
https://www.ncbi.nlm.nih.gov/pubmed/31871757
http://dx.doi.org/10.1107/S2056989019014841
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