TY - JOUR
T1 - Structural characterization of triorganotin(IV) complexes with sodium fusidate and DFT calculations
AU - Pellerito, Claudia
AU - Scopelliti, Michelangelo
AU - Pellerito, Lorenzo
AU - Fiore, Tiziana
AU - Casella, Girolamo
AU - Grasso, Giulia
AU - Spinella, Alberto
AU - Abbate, Michele
PY - 2010
Y1 - 2010
N2 - Three new complexes of the steroid sodium fusidate (sodium 2-[(1S,2S,5R,6S,7S,10S,11S,13S,14Z,15R,17R)-13-(acetyloxy)-5,17-dihydroxy-2,6,10,11-tetramethyl tetracyclo[8.7.0.02,7.011,15] heptadecan-14-ylidene]-6-methylhept-5-enoate = (NaFusidate, NaFA)]), with triorganotin(IV) moieties have beenprepared and investigated by conventional techniques as FTIR, Mössbauer, ESI-MS and NMR spectroscopy.The isolated compounds showed stoichiometries organotin(IV)/fusidate 1/1, R3Sn(IV)FA (R = Me,FA1; Bu, FA2; Ph, FA3). The ligand coordination sites were determined by FTIR spectroscopic measurements.In the complexes, the carboxylate group of the fusidate ligand behaves as monodentate monoanionicdonor, binding the Sn(IV) through one oxygen atom.On the basis of C–Sn–OCOO angles, calculated through the rationalization of the 119Sn Mössbauerparameter nuclear quadrupole splitting, it has been confirmed that, in all the solid state complexes,the Sn(IV) was tetracoordinated in a distorted tetrahedral structure.Further data from 119Sn CP-MAS spectra confirmed the distorted tetrahedral arrangement.In MeOH solution, 1H, 13C and 119Sn NMR spectroscopy showed monomeric complexes, where the carboxylategroup mainly acts as monodentate ester-type ligand, and the occurrence of a coordinated solventmolecule to the tin center, as validated by non-relativistic NMR DFT study.
AB - Three new complexes of the steroid sodium fusidate (sodium 2-[(1S,2S,5R,6S,7S,10S,11S,13S,14Z,15R,17R)-13-(acetyloxy)-5,17-dihydroxy-2,6,10,11-tetramethyl tetracyclo[8.7.0.02,7.011,15] heptadecan-14-ylidene]-6-methylhept-5-enoate = (NaFusidate, NaFA)]), with triorganotin(IV) moieties have beenprepared and investigated by conventional techniques as FTIR, Mössbauer, ESI-MS and NMR spectroscopy.The isolated compounds showed stoichiometries organotin(IV)/fusidate 1/1, R3Sn(IV)FA (R = Me,FA1; Bu, FA2; Ph, FA3). The ligand coordination sites were determined by FTIR spectroscopic measurements.In the complexes, the carboxylate group of the fusidate ligand behaves as monodentate monoanionicdonor, binding the Sn(IV) through one oxygen atom.On the basis of C–Sn–OCOO angles, calculated through the rationalization of the 119Sn Mössbauerparameter nuclear quadrupole splitting, it has been confirmed that, in all the solid state complexes,the Sn(IV) was tetracoordinated in a distorted tetrahedral structure.Further data from 119Sn CP-MAS spectra confirmed the distorted tetrahedral arrangement.In MeOH solution, 1H, 13C and 119Sn NMR spectroscopy showed monomeric complexes, where the carboxylategroup mainly acts as monodentate ester-type ligand, and the occurrence of a coordinated solventmolecule to the tin center, as validated by non-relativistic NMR DFT study.
KW - FTIR
KW - Mössbauer spectroscopy
KW - NMR
KW - Steroid carboxylate
KW - Triorganotin(IV)
KW - FTIR
KW - Mössbauer spectroscopy
KW - NMR
KW - Steroid carboxylate
KW - Triorganotin(IV)
UR - http://hdl.handle.net/10447/50933
M3 - Article
VL - 695
SP - 1405
EP - 1413
JO - Journal of Organometallic Chemistry
JF - Journal of Organometallic Chemistry
SN - 0022-328X
ER -