d,h-μ-Benzylalkoxophosphonato-e-μ-alkoxo-f-μ-oxo-bis[trichloroantimon(V)]-Verbindungen

d, h-μ-Benzylalkoxophosphonato-e-μ-alkoxo-f-μ-oxo-bis[trichloroantimony(V)] Compounds The binuclear antimony(V) complexes Cl₃Sb(O)[R³(R¹O)PO₂](OR²)SbCl₃ 1 – 6 with R¹ = R² = CH₃, C₂H₅ and R³ = C₆H₅CH₂, (CH₃)₃C₆H₂CH₂ in solution slowly exchanges the R² groups between the oxygen atoms of the Sb₂O₂ ring. The SbOPOSb ringsystem makes rapid pseudorotation. The isomeres are detected by nmr spectroscopy. 1 (R¹ = R² = CH₃) crystallizes in the orthorhombic space group Pnma with a = 1247.0, b = 1324.1, c = 1207.9 pm and Z = 4. 2 (R¹ = CH₃, R² = C₂H₅) and 5 (R¹ = R² = CH₃, R³ = (CH₃)₃ · C₆H₂CH₂) crystallizes triclinic in the space group P-1 with a = 984.1, b = 1026.7, c = 1079.9 pm, α = 87.93, β = 75.70, γ = 87.62° and Z = 2 and a = 1164.6, b = 1296.9, c = 1712.9 pm, α = 109.9, β = 96.3, γ = 100.2° and Z = 4 resp., with two crystallographically independent molecules in the asymmetric unit.     

d,h-μ-Carboxilato-e-μ-methoxo-f-μ-oxo-bis[trichloroantimon(V)] Darstellung und Spektren

μd,h-μ-Carboxilato-e-μ-methoxo-f-μ-oxo-bis[trichloroantimony(V)]. Preparation and Spectra The preparation of the unknown d,h-μ-carboxilato-e-μ-methoxo-f-μ-oxo-bis[trichloroantimony(V)] compounds is described (CF₃COO ? 2 , CH₃CH₂COO ? 4 ). The vibrational spectra of 2 and 4 were assigned and compared with those of the corresponding hydroxo compounds 1 and 3 . The mass spectra of 1—4 are measured and the fragmentation pathes are proposed. The formulae of some fragments of 1 with m/e values greater than the molecular weight were determined by high resolution.