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Crystal and molecular structure of tetra(triphenylphosphine oxide) sodium hexafluorophosphate

Trzeciak A. M., Lis T., Wojtków W., Ziółkowski J. J.

Bulletin of the Polish Academy of Sciences. Chemistry

2002

Vol. 50, No. 1

27-35

The complex compound of [Na(OPPh3)4]PF(6) formula was obtained in the reaction of triphenylphosphine oxide (OPPhs) with sodium hexafluorophosphate (NaPFg) in dichloromethane (CH(2)Cl(2). The slow crystallization at room temperature produced crystals suitable for X-ray analysis. Crystals are triclinic, space group P1 with a = 12.035(3), b= 14.268(3), c = 19.397(4) A, Alfa = 72.72(2), beta = 89.14(2), gamma = 88.29(2)°, V = 3178.9(12 A3 and Z = 2 at 100 K. The sodium cation is surrounded by four oxygen atoms of OPPh(3) ligands in a tetrahedral fashion. The slight difference of Na-O distances (2.207(2)-2.239(2) A) as well as remarkable difference of P-O-Na angles (137.37(7)-172.55(9)°) found in [Na(OPPh3)4J+ cation are explained by formation of intramolecular C-H.. .O interactions as well as intermolecular interactions of C-H.. .F type between phenyl rings and fluorins of PF-(6).

Synthesis, spectral, magnetic and X-ray powder diffraction structural characterization of [Fe(NCS)3(OPPh3)3]

Ondrejkovicova I., Jorik V., Mroziński J.

Polish Journal of Chemistry

1998

Vol. 72, nr 8

1890-1896

The autocatalytic oxidation of PPh3 with dioxygen in the systems containing some iron compound and NCS(-) anions in acetonitrile leads to the formation of the complexes [Fe(NCS)3(OPPh3)3], where OPPh3 is triphenylphosphine ixide. The complex is also formed by direct interaction of Fe(NCS)3 with )PPh3. This high-spin iron(III) complex acts as oa oxidation catalyst of PPh3. On the basis of elemental analysis, spectral data and X-ray powder diffraction have been proved that the samples of the complex have not only the same composition but possess the same crystal strycture irrespective of the preparation method.