Chemistry of bis (pentafluorobenzyl) phosphines and phosphine oxides. Single-crystal X-ray diffraction study of -mesitylene-dichloro[bis (pentafluorobenzyl) phosphinous acid]-ruthenium (II) and of 1,2-bis(pentafluorophenyl) ethane
Krafczyk, R; Thonnessen, H; Jones, P; Schmutzler, R
| HERO ID | 854219 |
|---|---|
| In Press | No |
| Year | 1997 |
| Title | Chemistry of bis (pentafluorobenzyl) phosphines and phosphine oxides. Single-crystal X-ray diffraction study of -mesitylene-dichloro[bis (pentafluorobenzyl) phosphinous acid]-ruthenium (II) and of 1,2-bis(pentafluorophenyl) ethane |
| Authors | Krafczyk, R; Thonnessen, H; Jones, P; Schmutzler, R |
| Journal | Journal of Fluorine Chemistry |
| Volume | 83 |
| Issue | 2 |
| Page Numbers | 159-166 |
| Abstract | The reaction of pentafluorobenzyl magnesium bromide with phosphorus trichloride in a 2:1 molar ratio led to the disubstituted product, bis(pentafluorobenzyl)bromophosphine 1, which, upon reaction with lithium aluminium hydride, was converted to bis(pentafluorobenzyl) phosphine 3. The reaction of 3 with oxygen led to bis(pentafluorobenzyl)phosphine oxide 4. The reaction of 1, 3 and 4 with di-mu-chloro-bis-[(eta(6)-mesitylene)chloro-retenium(II)] 5 yielded the eta(6)-mesitylene-phosphinedichloro-ruthenium(II) complexes 6-8. Single-crystal X-ray structure determinations are described for the phosphinous acid-ruthenium(II) complex 8 and for the by-product 1,2-bis (pentafluorophenyl) ethane 2, formed during the Grignard reaction of magnesium and pentafluorobenzylbromide. In 8, the Ru-C bond lengths can be categorised as four short (219-222 pm) and two long (224-228 pm). A weak intramolecular P-OH ... Cl contact (O ... Cl, 304 pm) is observed. (C) 1997 Elsevier Science S.A. |
| Doi | 10.1016/s0022-1139(97)00019-5 |
| Wosid | WOS:A1997XJ43400007 |
| Url | http://linkinghub.elsevier.com/retrieve/pii/S0022113997000195 |
| Is Certified Translation | No |
| Dupe Override | No |
| Is Public | Yes |
| Language Text | English |
| Keyword | The reaction of pentafluorobenzyl magnesium bromide with phosphorus trichloride in a 2:1 molar ratio led to the disubstituted product, bis(pentafluorobenzyl)bromophosphine 1, which, upon reaction with lithium aluminium hydride, was converted to bis(pentafluorobenzyl) phosphine 3. The reaction of 3 with oxygen led to bis(pentafluorobenzyl)phosphine oxide 4. The reaction of 1, 3 and 4 with di-mu-chloro-bis-[(eta(6)-mesitylene)chloro-retenium(II)] 5 yielded the eta(6)-mesitylene-phosphinedichloro-ruthenium(II) complexes 6-8. Single-crystal X-ray structure determinations are described for the phosphinous acid-ruthenium(II) complex 8 and for the by-product 1,2-bis (pentafluorophenyl) ethane 2, formed during the Grignard reaction of magnesium and pentafluorobenzylbromide. In 8, the Ru-C bond lengths can be categorised as four short (219-222 pm) and two long (224-228 pm). A weak intramolecular P-OH ... Cl contact (O ... Cl, 304 pm) is observed. (C) 1997 Elsevier Science S.A. |
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