6533b85afe1ef96bd12b8b36

RESEARCH PRODUCT

Synthesis and characterization of diorganotin(IV) derivatives of 2-mercaptopyridine and crystal structure of diphenyl pyridine-2-thiolatochlorotin(IV)

Renato BarbieriRalf SchmiedgenHans PreutFriedo HuberGiuseppe Ruisi

subject

Inorganic Chemistrychemistry.chemical_compoundCrystallographyDenticitychemistryPyridineX-ray crystallography2-MercaptopyridineGeneral ChemistryNuclear magnetic resonance spectroscopyCrystal structureBite angleMonoclinic crystal system

description

Diorganotin(IV) derivatives of 2-mercaptopyridine (HSPy), R2Sn(SPy)2, R2SnCl(SPy) (R = Me, iPr, nBu, tBu, Cy, Ph) and Cy2SnBr(SPy), were obtained from R2SnX2 (X = Cl, Br) and NaSPy. Ph2SnCl(SPy) crystals, as determined by singlecrystal X–ray diffraction, are monoclinic in the space group P21/n. Tin forms with the bidentate SPy ligand a four–membered chelate ring with a short NSnS bite angle of 64.8(1)° leading to a heavily distorted trigonal–bipyramidal environment about tin. Apical Cl–Sn–N angle = 156.1(1)° equatorial C–Sn–C angle = 121.9(2)°. From 119Sn Mossbauer and IR data, analogous structures are inferred for the other solid compounds R2SnX(SPy), and distorted octahedral molecular structures for the solid compounds R2Sn(SPy)2 with R in the trans position, and sulfur atoms and nitrogen–donor atoms each in cis positions. According to IR and 1H, 13C and 119Sn NMR data, the solid–state molecular structures are retained in chloroform solution.

https://doi.org/10.1002/aoc.590080414