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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...

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Autores principales: Kraft, Bradley M., Brennessel, William W., Ryan, Amy E., Benjamin, Candace K.
Formato: Online Artículo Texto
Lenguaje:English
Publicado: International Union of Crystallography 2015
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.
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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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