Synthesis of 1,3-Dimetallo-1,3-diphosphetane-2,4-diones.
X-ray Structure Analysis of
Cp*(CO)<sub>2</sub>FeP[Cr(CO)<sub>5</sub>]C(O)P[Fe(CO)<sub>2</sub>Cp*]C(O)
(Cp* = η<sup>5</sup>-C<sub>5</sub>Me<sub>5</sub>)
Lothar Weber
Bärbel Torwiehe
Gyn Bassmann
Hans-Georg Stammler
Beate Neumann
10.1021/om9505470.s001
https://acs.figshare.com/articles/journal_contribution/Synthesis_of_1_3-Dimetallo-1_3-diphosphetane-2_4-diones_X-ray_Structure_Analysis_of_Cp_CO_sub_2_sub_FeP_Cr_CO_sub_5_sub_C_O_P_Fe_CO_sub_2_sub_Cp_C_O_Cp_sup_5_sup_-C_sub_5_sub_Me_sub_5_sub_/3776178
Reaction of the lithoxy phosphaalkyne (DME)<sub>2</sub>LiOC⋮P
(<b>1</b>) with 1 equiv of the complexes
(η<sup>5</sup>-C<sub>5</sub>R<sub>5</sub>)(CO)<sub>2</sub>FeBr
(<b>2</b>); C<sub>5</sub>R<sub>5</sub> =
C<sub>5</sub>Me<sub>5</sub> (<b>a</b>),
1,3-<i>t</i>-Bu<sub>2</sub>C<sub>5</sub>H<sub>3</sub>
(<b>b</b>),
1,2,4-<i>i</i>-Pr<sub>3</sub>C<sub>5</sub>H<sub>2</sub>
(<b>c</b>)) afforded
the 1,3-diferrio-1,3-diphosphetane-2,4-diones
(η<sup>5</sup>-C<sub>5</sub>R<sub>5</sub>)(CO)<sub>2</sub>FePC(O)P[Fe(CO)<sub>2</sub>(η<sup>5</sup>-C<sub>5</sub>R<sub>5</sub>)]C(O) (<b>3a</b>−<b>c</b>) as red amorphous solids in 32−37%
yield. By treatment with
((<i>Z</i>)-cyclooctene)Cr(CO)<sub>5</sub>, compound <b>3a</b> was converted into the
red complex
Cp*(CO)<sub>2</sub>FeP[Cr(CO)<sub>5</sub>]C(O)P[Fe(CO)<sub>2</sub>Cp*]C(O) (<b>4</b>).
Constitutions and configurations of <b>3a</b>−<b>c</b>
and <b>4</b> were determined by
elemental analyses and spectra (IR, <sup>1</sup>H, <sup>13</sup>C,
and <sup>31</sup>P NMR, MS). The molecular structure
of
<b>4</b> was established by a single-crystal X-ray analysis.
1996-01-09 00:00:00
31 P NMR
DME
Bu 2 C 5 H 3
Pr 3 C 5 H 2
Cp
MS
CO
FeP
C 5
IR