Investigation into Diphosphine Oxides as Ligands in Diorganotin(IV) Adducts. Part 1. Synthesis and Spectroscopic Characterization of 1,2-Bis(diphenylphosphoryl)ethane Tin Complexes and X-Ray Structure of di-n-butyldichlorotin(IV)

Article abstract of DOI:10.1039/DT9830000921

1,2-Bis(diphenylphosphoryl)ethane (dppoe) forms complexes with diorganotin(IV) chlorides of the type SnR2Cl2(dppoe) (R =ⁿPr, ⁿBu, or Ph), the i.r. and tin-119 Moessbauer spectra of which have been recorded.The crystal structure of SnBuⁿ2Cl2(dppoe) has been determined from single-crystal X-ray data collected by counter methods and refined by full-matrix least-squares techniques to R = 0.0461 for 2430 observed reflections.Crystals are triclinic, space group P<*>, with unit-cell dimensions a = 11.775(5), b = 15.987(7), c = 11.006(5) Angstroem, α = 102.12(5), β = 114.55(6), γ = 101.69(5) deg, and Z = 2.Tin is bonded to two Cl^- ions to two C atoms and to two O atoms, to one more loosely than the other.The weaker co-ordination of one of the two OP groups is also reflected in distortions of the geometry of the co-ordination polyhedron.The structure is polymeric in that the dppoe ligand forms bridges between adjacent tin atoms.Tin-119 Moessbauer spectra have been recorded for the three SnR2Cl2(dppoe) complexes in the temperature range 77-150 K, and for the complex (SnPh3Cl)2(dppoe) at 77 K.Quadrupole-splitting data for the former are consistent with a trans-SnC2X4 arrangement about the tin atom in each case.Recoil-free fraction temperature coefficients, a, have also been determined for the three SnR2Cl2 complexes; root-mean-square amplitudes of vibration, , and absolute recoil-free fractions, f, have been estimated at various temperatures for SnBuⁿ2Cl2(dppoe).

Full text of DOI:10.1039/DT9830000921

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