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Mono‐organotin(IV) and tin(IV) derivatives of 2‐mercaptopyridine and 2‐mercaptopyrimidine: X‐ray structures of methyl‐tris(2‐pyridinethiolato)tin(IV) and phenyl‐tris(2‐pyridinethiolato)tin(IV)·1.5CHCl 3
Author(s) -
Huber Friedo,
Schmiedgen Ralf,
Schürmann Markus,
Barbieri Renato,
Ruisi Giusseppe,
Silvestri Arturo
Publication year - 1997
Publication title -
applied organometallic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.53
H-Index - 71
eISSN - 1099-0739
pISSN - 0268-2605
DOI - 10.1002/(sici)1099-0739(199710/11)11:10/11<869::aid-aoc655>3.0.co;2-0
Subject(s) - chemistry , tin , octahedron , trigonal bipyramidal molecular geometry , denticity , crystallography , pentagonal bipyramidal molecular geometry , crystal structure , bipyramid , monoclinic crystal system , tris , stereochemistry , organic chemistry , biochemistry
Mono‐organotin(IV) and tin(IV) derivatives of 2‐mercaptopyridine (HSPy) and 2‐mercaptopyrimidine (HSPym), RSnL 3 (R=Me, n‐Bu, Ph; L=SPy, SPym; R=Bz=benzyl, o ‐ClBz, o ‐ClC 6 H 4 , p ‐ClC 6 H 4 , o ‐tolyl, p ‐tolyl; L=SPy), RSnClL 2 (R=Me, n‐Bu, Ph; L=SPy, SPym), RSnCl 2 L (R=Me, n‐Bu; L=SPy, SPym) and SnCl 4− n L n (L=SPy, SPym; n =2, 4) were obtained from RSnCl 3 or SnCl 4 and NaL or by neutralization (R=Ph, p ‐tolyl; L=SPy, SPym). RSnClL 2 and RSnCl 2 L were better prepared by comproportionation of RSnCl 3 and RSnL 3 . MeSn(SPy) 3 and PhSn(SPy) 3 ·1.5CHCl 3 crystals, as determined by single‐crystal X‐ray diffraction, are monoclinic. In the discrete monomeric RSn(SPy) 3 units, three bidentate SPy ligands together with R form a distorted pentagonal bipyramid around tin. One S and the C(R) atom are in the axial positions. Two S atoms and three N atoms form the pentagonal plane. From 119 Sn Mössbauer and IR data, analogous structures are inferred for the other solid RSnL 3 compounds, except for R=Bz, o ‐ClBz, o ‐ClC 6 H 4 and o ‐tolyl, in which tin would be hexacoordinated. In the compounds RSnClL 2 and RSnCl 2 L, tin is at the center of an octahedron or a trigonal bipyramid, respectively. For Sn(SPym) 4 and SnCl 2 (SPym) 2 , the same type of octahedral structure as was previously found for Sn(SPy) 4 ·HSPy and SnCl 2 (SPy) 2 is proposed. According to IR and 1 H, 13 C and 119 Sn NMR data, the solid‐state molecular structures are retained in chloroform and dimethyl sulfoxide solution. © 1997 John Wiley & Sons, Ltd.