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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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Formato: | Online Artículo Texto |
Lenguaje: | English |
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International Union of Crystallography
2019
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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. |
format | Online Article Text |
id | pubmed-6895954 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2019 |
publisher | International Union of Crystallography |
record_format | MEDLINE/PubMed |
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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