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The Novel Reactivity of Haloaminophosphines and Related Diphosphines

Nycz J. E.

Polish Journal of Chemistry

2009

Vol. 83, nr 7

1323-1328

The present study shows novel reactivity of [(Me3Si)2N](Pr2 i N)PCl (1a) and diphosphine [(Me3Si)2N](Pr2i N)P-P(NPr2 i )[N(SiMe3)2] (meso and rac) (2a,b). New reaction between 1a and a sterically hindered stable silylene Si[(NCH2But)2C6H4-1,2] (3) was presented in the study. It is dem on strated that the conversion was unambiguous and led to pi-phosphinyl radical 4 and possibly silicon radical 5, in which 4 and 5 dimerize to form phosphanochlorosilane [(Me3Si)2N](Pr2 i N)P-Si(Cl)[(NCH2But)2C6H4-1,2] (6), 2a,b and disilane [C6H4-1,2(ButCH2N)2](Cl)Si-Si(Cl)[(NCH2But)2C6H4-1,2] (7). The product 6 is labile and decomposed even at room temperature into 7 and 2a,b. The compounds 2a,b were further allowed to react with two precursors of stable S-centered radicals, i.e. tetraethylthiuram disulfide (8) and p-tolyldisulfide (9), and were converted to S-phosphines, ((Me3Si)2N)(Pr2i N)P-S-R [10,11, R = Et2N-C(=S), p-MePh] with high yields through the dimerization of 4 and thio radicals. Unexpectedly, 1a reacts with KBF4 to give a cyclic zwitterionic diphosphine 12. All products were characterized by spectroscopic data.

New Copper(I) Perfluorinated Carboxylates Complexes with Bis(diphenylphosphine)methane

Szłyk E., Kucharek R., Szymańska I.

Polish Journal of Chemistry

2001

Vol. 75, nr 3

337-344

Copper(I) perfluorinated carboxylates complexes with bis(diphenylphosphine)methane (dppm) of general formula [Cu2(ž-dppm)3(RCOO)2] dppm, whereR=C2F5, C4F9, C6F13, C8F17, C9F19, have been prepared and characterized by vibrational, 31P CPMASNMRand 13C CPTOSSB NMR mass spectra in the solid state. 1H, 13C, 19F NMR and variable temperature 31P NMR spectra were measured in solution. Temperature variable 31P NMR spectra revealed at least three dimeric species in equilibrium. IR and mass spectra analyses suggest dimeric complexes with three bridging diphosphines and monodentate carboxylates in the solid state.