80243-52-3Relevant articles and documents
Oxy and thio phosphorus acid derivatives of tin. 11. Synthesis and properties of di-and triorganotin(IV) derivatives of phenylphosphonic acid phenyl ester
Cunningham,Kelly,Molloy,Zuckerman
, p. 1416 - 1421 (2008/10/08)
Seven di- and triorganotin(IV) phenylphosphonic acid phenyl esters, R2Sn[O2P(C6H5)OC6H 5]2, where R = CH3, n-C4H9, n-C8H17, or C6H5, and R3SnO2P(C6H5)OC6H 5, where R = CH3, n-C4H9, or C6H5, are synthesized in quantitative yield by the action of the corresponding organotin(IV) chlorides or acetates upon the free acid in water or methanol, respectively. The products are colorless, insoluble solids. The diorganotin(IV) derivatives are infusible. In the mass spectra no ions having mass greater than the parent or containing more than one tin atom are detected, but parent molecular ions are found in the spectra of the trimethyl- and triphenyltin(IV) derivatives. The ion of highest abundance arises in all the triorganotins from loss of an organo group from the tin, while for the triphenyl derivative the triphenyltin fragment is most abundant. Successive loss of organic groups from tin is seen, and even-electron ions are preferred. The identity of the phenyl groups lost from the ligands in both series is unknown. No monoorganotin fragments are seen in the spectra of the diorganotin(IV) derivatives. Infrared and Raman data in the v(Sn-C) region are used to assign a linear C-Sn-C configuration and a planar SnC3 configuration in the di- and trimethyltin(IV) derivatives, respectively. Bands at 1080-1063 and 1000-993 cm-1 are also assigned to the vasym- and vsym(PO2) modes, respectively. Tin-119m M?ssbauer isomer shift (IS) values (1.12-1.47 mm s-1) confirm the presence of tetravalent tin; the ρ [ratio of quadrupole splitting (QS) to IS] values (2.73-3.74) and QS values (3.60-4.66 mm s-1) specify higher than four-coordination at tin. The particularly high QS values for the diorganotin(IV) series suggest a six-coordinated, trans-octahedral geometry. Ambient-temperature M?ssbauer spectra for this series indicate intermolecular association, while the absence in the triorganotin analogues suggests an oligomeric structure where five units are the minimum for ring formation accommodating trigonal-bipyramidal and -O-P-O-bridges.
