Crystal structures of tris­[1-oxo­pyridine-2-olato(1-)]silicon(IV) chloride chloro­form-d1 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-d1 disolvate

Authors

Bradley M. Kraft, St. John Fisher UniversityFollow
William W. Brennessel, University of RochesterFollow
Amy E. Ryan, St. John Fisher UniversityFollow
Candace K. Benjamin, St. John Fisher UniversityFollow

Document Type

Article

Publication Date

11-2015

Abstract

The cations in the title salts, [Si(OPO)3]Cl·2CDCl3, (I), [Si(OPO)3]Cl·xCH3CN, (II), and fac-[Si(OPTO)3]Cl·2CDCl3, (III) (OPO = 1-oxo-2-pyridin­one, C5H4NO2, and OPTO = 1-oxo-2-pyridine­thione, C5H4NOS), 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-HCl 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 Å3 accounted for per unit cell (25 electrons in 109 Å3 in one channel, and 29 electrons in 115 Å3 in the other). In (I) and (II), all species lie on general positions. In (III), all species are located along crystallographic threefold axes.

DOI

10.1107/S2056989015022203

Comments

This is the authorized electronic report of the article. The final published version is also available through the publisher: https://dx.doi.org/10.1107/S2056989015022203

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Publication Information

Kraft, Bradley M.; Brennessel, William W.; Ryan, Amy E.; and Benjamin, Candace K. (2015). "Crystal structures of tris­[1-oxo­pyridine-2-olato(1-)]silicon(IV) chloride chloro­form-d1 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-d1 disolvate." Acta Crystallographica Section E: Crystallographic Communications E71, 1531-1535.

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