Crystal structures of tris-[1-oxo-pyridine-2-olato(1-)]silicon(IV) chloride chloro-form-d 1 disolvate, tris-[1-oxo-pyridine-2-olato(1-)]silicon(IV) chloride aceto-nitrile unqu-anti-fied solvate, and fac-tris-[1-oxo-pyridine-2-thiol-ato(1-)]silicon(IV) chloride chloro-form-d 1 disolvate.

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-pyridin-one, C5H4NO2, and OPTO = 1-oxo-2-pyridine-thione, C5H4NOS), have distorted octa-hedral 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.

SUBMITTER: Kraft BM 

PROVIDER: S-EPMC4719831 | biostudies-other | 2015 Dec

REPOSITORIES: biostudies-other