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Crystal structures of tris[1-oxopyridine-2-olato(1−)]silicon(IV) chloride chloroform-d (1) disolvate, tris[1-oxopyridine-2-olato(1−)]silicon(IV) chloride acetonitrile unquantified solvate, and fac-tris[1-oxopyridine-2-thiolato(1−)]silicon(IV) chloride chloroform-d (1) disolvate
The cations in the title salts, [Si(OPO)(3)]Cl·2CDCl(3), (I), [Si(OPO)(3)]Cl·xCH(3)CN, (II), and fac-[Si(OPTO)(3)]Cl·2CDCl(3), (III) (OPO = 1-oxo-2-pyridinone, C(5)H(4)NO(2), and OPTO = 1-oxo-2-pyridinethione, C(5)H(4)NOS), have distorted octahedral coordination spheres. The first two structures...
Autores principales: | , , , |
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Formato: | Online Artículo Texto |
Lenguaje: | English |
Publicado: |
International Union of Crystallography
2015
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Materias: | |
Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC4719831/ https://www.ncbi.nlm.nih.gov/pubmed/26870422 http://dx.doi.org/10.1107/S2056989015022203 |
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author | Kraft, Bradley M. Brennessel, William W. Ryan, Amy E. Benjamin, Candace K. |
author_facet | Kraft, Bradley M. Brennessel, William W. Ryan, Amy E. Benjamin, Candace K. |
author_sort | Kraft, Bradley M. |
collection | PubMed |
description | The cations in the title salts, [Si(OPO)(3)]Cl·2CDCl(3), (I), [Si(OPO)(3)]Cl·xCH(3)CN, (II), and fac-[Si(OPTO)(3)]Cl·2CDCl(3), (III) (OPO = 1-oxo-2-pyridinone, C(5)H(4)NO(2), and OPTO = 1-oxo-2-pyridinethione, C(5)H(4)NOS), have distorted octahedral coordination spheres. The first two structures contain the same cation and anion, but different solvents of crystallization led to different solvates and packing arrangements. In structures (I) and (III), the silicon complex cations and chloride anions are well separated, while in (II), there are two C—H⋯Cl distances that fall just within the sum of the van der Waals radii of the C and Cl atoms. The pyridine portions of the OPO ligands in (I) and (II) are modeled as disordered with the planar flips of themselves [(I): 0.574 (15):0.426 (15), 0.696 (15):0.304 (15), and 0.621 (15):0.379 (15); (II): 0.555 (13):0.445 (13), 0.604 (14):0.396 (14) and 0.611 (13):0.389 (13)], demonstrating that both fac and mer isomers are co-crystallized. In (II), highly disordered solvent, located in two independent channels along [100], was unable to be modeled. Reflection contributions from this solvent were fixed and added to the calculated structure factors using the SQUEEZE [Spek (2015 ▸). Acta Cryst. C71, 9–18] function of program PLATON, which determined there to be 54 electrons in 225 Å(3) accounted for per unit cell (25 electrons in 109 Å(3) in one channel, and 29 electrons in 115 Å(3) in the other). In (I) and (II), all species lie on general positions. In (III), all species are located along crystallographic threefold axes. |
format | Online Article Text |
id | pubmed-4719831 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2015 |
publisher | International Union of Crystallography |
record_format | MEDLINE/PubMed |
spelling | pubmed-47198312016-02-11 Crystal structures of tris[1-oxopyridine-2-olato(1−)]silicon(IV) chloride chloroform-d (1) disolvate, tris[1-oxopyridine-2-olato(1−)]silicon(IV) chloride acetonitrile unquantified solvate, and fac-tris[1-oxopyridine-2-thiolato(1−)]silicon(IV) chloride chloroform-d (1) disolvate Kraft, Bradley M. Brennessel, William W. Ryan, Amy E. Benjamin, Candace K. Acta Crystallogr E Crystallogr Commun Research Communications The cations in the title salts, [Si(OPO)(3)]Cl·2CDCl(3), (I), [Si(OPO)(3)]Cl·xCH(3)CN, (II), and fac-[Si(OPTO)(3)]Cl·2CDCl(3), (III) (OPO = 1-oxo-2-pyridinone, C(5)H(4)NO(2), and OPTO = 1-oxo-2-pyridinethione, C(5)H(4)NOS), have distorted octahedral coordination spheres. The first two structures contain the same cation and anion, but different solvents of crystallization led to different solvates and packing arrangements. In structures (I) and (III), the silicon complex cations and chloride anions are well separated, while in (II), there are two C—H⋯Cl distances that fall just within the sum of the van der Waals radii of the C and Cl atoms. The pyridine portions of the OPO ligands in (I) and (II) are modeled as disordered with the planar flips of themselves [(I): 0.574 (15):0.426 (15), 0.696 (15):0.304 (15), and 0.621 (15):0.379 (15); (II): 0.555 (13):0.445 (13), 0.604 (14):0.396 (14) and 0.611 (13):0.389 (13)], demonstrating that both fac and mer isomers are co-crystallized. In (II), highly disordered solvent, located in two independent channels along [100], was unable to be modeled. Reflection contributions from this solvent were fixed and added to the calculated structure factors using the SQUEEZE [Spek (2015 ▸). Acta Cryst. C71, 9–18] function of program PLATON, which determined there to be 54 electrons in 225 Å(3) accounted for per unit cell (25 electrons in 109 Å(3) in one channel, and 29 electrons in 115 Å(3) in the other). In (I) and (II), all species lie on general positions. In (III), all species are located along crystallographic threefold axes. International Union of Crystallography 2015-11-28 /pmc/articles/PMC4719831/ /pubmed/26870422 http://dx.doi.org/10.1107/S2056989015022203 Text en © Kraft et al. 2015 http://creativecommons.org/licenses/by/2.0/uk/ 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/2.0/uk/ |
spellingShingle | Research Communications Kraft, Bradley M. Brennessel, William W. Ryan, Amy E. Benjamin, Candace K. Crystal structures of tris[1-oxopyridine-2-olato(1−)]silicon(IV) chloride chloroform-d (1) disolvate, tris[1-oxopyridine-2-olato(1−)]silicon(IV) chloride acetonitrile unquantified solvate, and fac-tris[1-oxopyridine-2-thiolato(1−)]silicon(IV) chloride chloroform-d (1) disolvate |
title | Crystal structures of tris[1-oxopyridine-2-olato(1−)]silicon(IV) chloride chloroform-d
(1) disolvate, tris[1-oxopyridine-2-olato(1−)]silicon(IV) chloride acetonitrile unquantified solvate, and fac-tris[1-oxopyridine-2-thiolato(1−)]silicon(IV) chloride chloroform-d
(1) disolvate |
title_full | Crystal structures of tris[1-oxopyridine-2-olato(1−)]silicon(IV) chloride chloroform-d
(1) disolvate, tris[1-oxopyridine-2-olato(1−)]silicon(IV) chloride acetonitrile unquantified solvate, and fac-tris[1-oxopyridine-2-thiolato(1−)]silicon(IV) chloride chloroform-d
(1) disolvate |
title_fullStr | Crystal structures of tris[1-oxopyridine-2-olato(1−)]silicon(IV) chloride chloroform-d
(1) disolvate, tris[1-oxopyridine-2-olato(1−)]silicon(IV) chloride acetonitrile unquantified solvate, and fac-tris[1-oxopyridine-2-thiolato(1−)]silicon(IV) chloride chloroform-d
(1) disolvate |
title_full_unstemmed | Crystal structures of tris[1-oxopyridine-2-olato(1−)]silicon(IV) chloride chloroform-d
(1) disolvate, tris[1-oxopyridine-2-olato(1−)]silicon(IV) chloride acetonitrile unquantified solvate, and fac-tris[1-oxopyridine-2-thiolato(1−)]silicon(IV) chloride chloroform-d
(1) disolvate |
title_short | Crystal structures of tris[1-oxopyridine-2-olato(1−)]silicon(IV) chloride chloroform-d
(1) disolvate, tris[1-oxopyridine-2-olato(1−)]silicon(IV) chloride acetonitrile unquantified solvate, and fac-tris[1-oxopyridine-2-thiolato(1−)]silicon(IV) chloride chloroform-d
(1) disolvate |
title_sort | crystal structures of tris[1-oxopyridine-2-olato(1−)]silicon(iv) chloride chloroform-d
(1) disolvate, tris[1-oxopyridine-2-olato(1−)]silicon(iv) chloride acetonitrile unquantified solvate, and fac-tris[1-oxopyridine-2-thiolato(1−)]silicon(iv) chloride chloroform-d
(1) disolvate |
topic | Research Communications |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC4719831/ https://www.ncbi.nlm.nih.gov/pubmed/26870422 http://dx.doi.org/10.1107/S2056989015022203 |
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