0000000000048377
AUTHOR
Aleš Růžička
Organotin(IV) trifluoromethanesulfonates chemistry: Isolation and characterization of a new di-n-butyl derivative presenting a Sn3O3 core
Abstract Reaction of the dimeric hydroxo di-n-butylstannane trifluoromethanesulfonato complex [n-Bu2Sn(OH)(H2O)(CF3SO3)]2 (1) with a mixture of anthracene (C14H10, Ant) and phenazine (C12H8N2, Phz) in dichloromethane at room temperature yielded the novel di-n-butyltin(IV) trifluoromethanesulfonate salt {[n-Bu2Sn(H2O)]2O·n-Bu2Sn(OH)2}(CF3SO3)2 (2), together with the co-crystallization of phenazinium trifluoromethanesulfonate salts ([C12H9N2][CF3SO3], PhzH) collected in the solid state in two distinct self-assembled architectures, 3 and 4, showing π–π stacking interactions, and involving the intercalation of free molecules of phenazine and anthracene, respectively. Complex 2 is a cationic tri…
C,N-chelated dicyclopentadienylzirconium complexes and their possible use as hydrogenation catalysts
Abstract In situ generated Cp2Zr(n-Bu)Cl (6) reacts with {2-[(CH3)2NCH2]C6H4}2Pb to form exclusively {2-[(CH3)2NCH2]C6H4}Cp2ZrCl (7), [(CH3)2NCH2]C6H5, butene and elemental lead. The further derivatization of chloride (7) to fluoride (8), hydride (9), methyl derivative (10), and a reduction of 7 are also described. The crystal structures of 7–10 were determined. The catalytic activity of 9 and 10 in hydrogenation of styrene was also preliminarily tested.
Triorganotin( iv ) cation-promoted dimethyl carbonate synthesis from CO 2 and methanol: solution and solid-state characterization of an unexpected diorganotin( iv )-oxo cluster
Two novel C,N-chelated organotin(IV) complexes bearing weakly coordinating carborane moieties were prepared by the reaction of the corresponding C,N-chelated organotin(IV) chloride (i.e. LCNR2SnCl, R = n-Bu (1) and Ph (2); LCN = 2-(N,N-dimethylaminomethyl)phenyl)) with monocarba-closo-dodecaborate silver salt (AgCB11H12; Ag·3). Both products of the metathesis, [LCN(n-Bu)2Sn]+[CB11H12]− (4) and [LCNPh2Sn]+ [CB11H12]− (5), respectively, were characterized by both multinuclear NMR spectroscopy and elemental analysis. The instability of 4 and 5 towards water is discussed. The solid-state structure of LCN(n-Bu)2SnOH·B(C6F5)3 (4a) as a model compound with a Sn–O(H)⋯B linkage is also reported. The…
Structure, properties and comparison of C,N-chelated and amido-stabilized plumbylenes
The molecular structure of {2-[(CH3)2NCH2]C6H4}2Pb (1) in the solid state was determined by X-ray diffraction techniques on a single crystalline material. Bulky amido ligand stabilized complexes [(i-C3H7)2C6H3]NHLi (2) and [(i-C3H7)2C6H3N(Me3Si)]2Pb (3) were synthesized and characterized both in the solid state and solution by 1H, 13C, 15N and 207Pb NMR and XRD techniques. The structure of both C,N-chelated and bulky amido plumbylenes is compared.
Reactivity of di-n-butyl-dicyclopentadienylzirconium towards amido stabilized stannylenes
Abstract Reaction of Sn[(N(C 6 H 3 i Pr 2 -2,6)(SiMe 3 )] 2 and [{Sn(N(C 6 H 3 i Pr 2 -2,6)(SiMe 3 )(μ-Cl) 2 ] with di- n -butyl-dicyclopentadienylzirconium yielded the trimetallic a carbene-like complex {[(N(C 6 H 3 i Pr 2 -2,6)(SiMe 3 )]( n -Bu)Sn} 2 Cp 2 Zr. The oxidation of {[(N(C 6 H 3 i Pr 2 -2,6)(SiMe 3 )]( n -Bu)Sn} 2 Cp 2 Zr by oxygen gives the five-membered dioxadistannazirconacyclic complex {[(N(C 6 H 3 i Pr 2 -2,6)(SiMe 3 )]( n -Bu)Sn} 2 O 2 Cp 2 Zr.
C,N-chelated organotin(IV) trifluoroacetates. Instability of the mono- and diorganotin(IV) derivatives.
Abstract The C,N-chelated tri-, di- and monoorganotin(IV) halides react with equimolar amounts of CF3COOAg to give corresponding C,N-chelated organotin(IV) trifluoroacetates. The set of prepared tri-, di- and monoorganotin(IV) trifluoroacetates bearing the LCN ligand (where LCN is 2-(N,N-dimethylaminomethyl)phenyl-) was structurally characterized by X-ray diffraction analyses, multinuclear NMR and IR spectroscopy. In the case of triorganotin(IV) trifluoroacetates and (LCN)2Sn(OC(O)CF3)2, no tendency to form hydrolytic products, or instability towards the moisture was observed. LCNRSn(OC(O)CF3)2 (where R is n-Bu or Ph) and LCNSn(OC(O)CF3)3 forms upon crystallization from THF in the air mainl…
C,N-chelated organotin(IV) trifluoromethanesulfonates: Synthesis, characterization and preliminary studies of its catalytic activity in the direct synthesis of dimethyl carbonate from methanol and CO2
Abstract C,N-chelated tri- and diorganotin(IV) halides react with 1 or 2 mol equiv of silver trifluoromethanesulfonate (triflate, AgOTf, OTf = OSO2CF3−) to give corresponding C,N-chelated organotin(IV) triflates. The triorganotin(IV) triflates of general formula LCNR2SnOTf (R = n-Bu (1), Ph (2)) are presumably more stable towards hydrolysis than the diorganotin(IV) triflates LCNRSn(OTf)2 (R = n-Bu (3), Ph (4)). All prepared organotin(IV) triflates bearing the LCN ligand (where LCN is 2-(N,N-dimethylaminomethyl)phenyl-) were characterized by multinuclear NMR spectroscopy and elemental analysis. In addition, the structure of 3 was determined by the X-ray diffraction analysis. The catalytic ac…
CCDC 1590298: Experimental Crystal Structure Determination
Related Article: Petr Švec, Hélène Cattey, Zdeňka Růžičková, Josef Holub, Aleš Růžička, Laurent Plasseraud|2018|New J.Chem.|42|8253|doi:10.1039/C7NJ05058E
CCDC 1590299: Experimental Crystal Structure Determination
Related Article: Petr Švec, Hélène Cattey, Zdeňka Růžičková, Josef Holub, Aleš Růžička, Laurent Plasseraud|2018|New J.Chem.|42|8253|doi:10.1039/C7NJ05058E
CCDC 1590300: Experimental Crystal Structure Determination
Related Article: Petr Švec, Hélène Cattey, Zdeňka Růžičková, Josef Holub, Aleš Růžička, Laurent Plasseraud|2018|New J.Chem.|42|8253|doi:10.1039/C7NJ05058E