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| 2. |
- Ivanov, M.A., et al.
(författare)
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Synthesis, structure, and 13C and 31P CP/MAS NMR of the tetraphenylantimony(V) di-iso-propyl phosphorodithioate complex [Sb(C6H5)4{S2P(O-iso-C3H7)2}] and its solvated form [Sb(C6H5)4{S2P(O-iso-C3H7)2}] · 1/2C6H6 : an example of the monodentate coordination of dithio ligands
- 2009
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Ingår i: Russian Journal of Inorganic Chemistry. - 0036-0236 .- 1531-8613. ; 54:5, s. 708-716
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Tidskriftsartikel (refereegranskat)abstract
- The crystalline tetraphenylantimony(V) O,O′-di-iso-propyl phosphorodithioate complex [Sb(C6H5)4{S2P(O-i-C3H7)2}](I) and its solvated form [Sb(C6H5)4{S2P(O-i-C3H7)2}] · 1/2C6H6(II) were synthesized. Solid compounds I and II were studied by MAS NMR (13C, 31P). The 31P NMR chemical shift anisotropy 31P δaniso = (δ zz - δiso) and asymmetry parameter η = (δ yy - δ xx )/(δ zz - δiso) were calculated using χ 2 plots constructed on the basis of the 31P MAS NMR data. The O,O′-di-iso-propyl phosphorodithioate ligands in both complexes are characterized by predominantly the axially symmetric 31P chemical shift tensor (for the case δ zz < δ xx ≈ δ yy ) with close values of anisotropy parameters (δaniso and η), which reflects their identical S-monodentate structural function. X-ray crystallography showed that II has a trigonal-bipyramidal molecular structure with the uncommon monodentate coordination of the Dtph ligands through an S atom in an axial position of the trigonal bipyramid and the benzene molecule in the outer sphere.
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| 3. |
- Ivanov, M.A., et al.
(författare)
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Tetraphenylantimony(V) O,O″-dialkyl dithiophosphates [Sb(C 6H5)4{S2P(OR)2}] (R = s-C4H9, c-C6H11) : synthesis, structures, and 13C and 31P CP/MAS NMR spectra
- 2008
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Ingår i: Russian journal of coordination chemistry. - 1070-3284 .- 1608-3318. ; 34:7, s. 527-535
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Tidskriftsartikel (refereegranskat)abstract
- Tetraphenylantimony(V) O,O′-di-sec-butyl dithiophosphate (I) and tetraphenylantimony(V) O,O′-dicyclohexyl dithiophosphate (II) [Sb(C 6H5)4{S2P(OR)2}] (R = sec-C4H9 or cyclo-C6H11) were obtained. Their structures and spectroscopic properties were studied by X-ray diffraction analysis and 13C and 31P CP/MAS NMR spectroscopy. The dithiophosphate (Dtph) ligands in complexes I and II were found to be coordinated in S-monodentate and S,S′-bidentate fashions, respectively (MAS NMR data). According to X-ray diffraction data, the coordination polyhedron of antimony in molecular structure I is a trigonal bipyramid with unusual monodentate coordination of the Dtph group in the axial position.
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| 4. |
- Ivanov, M.A., et al.
(författare)
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The diethyl dithiophosphate complex of tetraphenylantimony(V) and its solvated form, [Sb(C6H5)(4){S2P(OC2H5)(2)}] center dot 1/2 C6H6: Synthesis, crystal structure, and C-13, P-31 CP/MAS NMR study : an example of monodentate coordination of dithio ligands
- 2013
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Ingår i: Russian Journal of Inorganic Chemistry. - 0036-0236 .- 1531-8613. ; 58:2, s. 197-205
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Tidskriftsartikel (refereegranskat)abstract
- The O,O'-diethyl dithiophosphate complex of tetraphenylantimony(V) [Sb(C6H5)(4){S2P(OC2H5)(2)}] (I) and its benzene-solvated form I center dot 1/2C(6)H(6) (II) were synthesized and studied by high-resolution solid-state C-13 and P-31 NMR (MAS NMR). The diethyl dithiophosphate (Dtph) groups in I and II were quantitatively characterized by the P-31 chemical shift anisotropy (delta(aniso)), the asymmetry parameter (eta), and the principal values of chemical shift tensors (delta (xx) , delta (yy) , delta (zz) ). The calculation of the anisotropy parameters included construction of chi(2) statistic diagrams from full P-31 MAS NMR spectra. In both complexes, the Dtph groups were found to have mainly axially symmetric P-31 chemical shift tensors (for delta (zz) < delta (xx) a parts per thousand delta (yy) ) with similar anisotropy parameters (delta(aniso) and eta), which is due to their identical S-monodentate function. According to X-ray diffraction data, II has a trigonal bipyramidal (TBP) molecular structure with Smonodentate coordination of Dtph in the TBP axial position and outer-sphere position of the benzene molecule. The desorption of the outer-sphere benzene solvent molecules from structure II, which was noted in MAS NMR experiment, passes through the formation of three intermediate solvated forms with benzene content n < 1/2.
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| 5. |
- Sharutin, V. V., et al.
(författare)
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Tetraphenyl- and tetratolylantimony complexes with N,N-dialkyldithiocarbamate ligands : synthesis, X-ray diffraction analysis, and 13C and 15N CP/MAS NMR studies
- 2006
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Ingår i: Russian journal of coordination chemistry. - 1070-3284 .- 1608-3318. ; 32:3:6, s. 87-396
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Tidskriftsartikel (refereegranskat)abstract
- Crystalline tetraphenylantimony and tetratolylantimony complexes with N,N-dialkyldithiocarbamate ligands [Sb(C6H5)4(S2CNR2)] (R = CH3, C2H5, and C3H7 and R2 = (CH2)6) were synthesized by ligand exchange reactions and studied by 13C and 15N CP/MAS NMR spectroscopy. X-ray diffraction analysis revealed that the complex [Sb(n-CH3-C6H4)4{S2CN(C3H7)2}] exists as the single molecular form, while [Sb(C6H5)4{S2CN(CH2)6}] exists as two molecular conformers. The 13C and 15N signals were assigned to the positions of the atoms in the isomeric structures [Sb(C6H5)4{S2CN(CH2)6}] in terms of different degrees of double bonding in the formally single =N-C(S)S-bond.
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