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Di-n-butyltin methyl- and phenylphosphonates

(2001) ORGANOMETALLICS. 20(12). p.2593-2603
Author
Organization
Abstract
The structure of [Bu2Sn(HO3PMe)(2)](2) (1), as determined by single-crystal X-ray diffraction, is based on a dimer containing bridging and terminal hydrogenophosphonate ligands. The tin atoms are formally five-coordinate, but exhibit also two additional remote contacts, d(Sn-O) approximate to 3.14 Angstrom, which results in a "5+2" type coordination. This crystalline compound and the three other amorphous compounds, Bu2Sn(O3PMe) (2), Bu2Sn(HO3PPh)(2) (3), and Bu-2-Sn(O3PPh) (4), have been characterized by solid state P-31 and Sn-119 MAS NMR. Compound 1 exhibits a very well resolved P-31 MAS NMR spectrum in which three different (2)J-(P-31-Sn-119/117)(iso) scalar couplings can be measured. P-31 and Sn-119 NMR, (31)p-Sn-19 HMQC spectroscopy, and various other 2D NMR techniques at variable temperatures were used to unravel the basic structural unit of compounds 2 and 4 in solution, which is proposed to be based on a trigonal bipyramid of the type R2SnO3 with two apical and one equatorial oxygen atom. Compound 1, in solution, displays a similar local geometry at tin and the same dimeric unit as in the crystalline state. In contrast with 2 and 4, however, compounds 1 and 3 display an extremely high degree of stereochemical fluxionality based on fast exchange of the bridging and terminal hydrogenophosphonate ligands.
Keywords
PHOSPHORUS-ACID-DERIVATIVES, NUCLEAR-MAGNETIC-RESONANCE, CHEMICAL-SHIFT ANISOTROPY, MULTIPLE QUANTUM NMR, SOL-GEL ROUTES, CRYSTAL-STRUCTURE, MOLECULAR-STRUCTURE, HYDROTHERMAL SYNTHESIS, ZIRCONIUM PHOSPHONATES, METAL PHOSPHONATES

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Chicago
Ribot, F, C Sanchez, M Biesemans, F Mercier, José Martins, M Gielen, and R Willem. 2001. “Di-n-butyltin Methyl- and Phenylphosphonates.” Organometallics 20 (12): 2593–2603.
APA
Ribot, F., Sanchez, C., Biesemans, M., Mercier, F., Martins, J., Gielen, M., & Willem, R. (2001). Di-n-butyltin methyl- and phenylphosphonates. ORGANOMETALLICS, 20(12), 2593–2603.
Vancouver
1.
Ribot F, Sanchez C, Biesemans M, Mercier F, Martins J, Gielen M, et al. Di-n-butyltin methyl- and phenylphosphonates. ORGANOMETALLICS. 2001;20(12):2593–603.
MLA
Ribot, F, C Sanchez, M Biesemans, et al. “Di-n-butyltin Methyl- and Phenylphosphonates.” ORGANOMETALLICS 20.12 (2001): 2593–2603. Print.
@article{138222,
  abstract     = {The structure of [Bu2Sn(HO3PMe)(2)](2) (1), as determined by single-crystal X-ray diffraction, is based on a dimer containing bridging and terminal hydrogenophosphonate ligands. The tin atoms are formally five-coordinate, but exhibit also two additional remote contacts, d(Sn-O) approximate to 3.14 Angstrom, which results in a {\textacutedbl}5+2{\textacutedbl} type coordination. This crystalline compound and the three other amorphous compounds, Bu2Sn(O3PMe) (2), Bu2Sn(HO3PPh)(2) (3), and Bu-2-Sn(O3PPh) (4), have been characterized by solid state P-31 and Sn-119 MAS NMR. Compound 1 exhibits a very well resolved P-31 MAS NMR spectrum in which three different (2)J-(P-31-Sn-119/117)(iso) scalar couplings can be measured. P-31 and Sn-119 NMR, (31)p-Sn-19 HMQC spectroscopy, and various other 2D NMR techniques at variable temperatures were used to unravel the basic structural unit of compounds 2 and 4 in solution, which is proposed to be based on a trigonal bipyramid of the type R2SnO3 with two apical and one equatorial oxygen atom. Compound 1, in solution, displays a similar local geometry at tin and the same dimeric unit as in the crystalline state. In contrast with 2 and 4, however, compounds 1 and 3 display an extremely high degree of stereochemical fluxionality based on fast exchange of the bridging and terminal hydrogenophosphonate ligands.},
  author       = {Ribot, F and Sanchez, C and Biesemans, M and Mercier, F and Martins, Jos{\'e} and Gielen, M and Willem, R},
  issn         = {0276-7333},
  journal      = {ORGANOMETALLICS},
  language     = {eng},
  number       = {12},
  pages        = {2593--2603},
  title        = {Di-n-butyltin methyl- and phenylphosphonates},
  url          = {http://dx.doi.org/10.1021/om010140x},
  volume       = {20},
  year         = {2001},
}

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