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On reacting PH-functional m ethylenebisphosphanes (iPr)HPCH 2 PH 2  (1) and RHPCH 2 PR 2  (R = CH 2 Ph) with excess Fe 2 (CO) 9  P -C -P-bond cleavage occurs. As a result β-phosphido bridged clusters e.g. Fe 3 (CO) 8 (μ 2 -PRCH 2 PR 2 )(μ 3 -PR)(μ 2 -H) (11) and Fe 4 (μ 4 -P) spiro com pounds with naked phosphorus atoms Fe 4 (CO) 13 (μ 4 -P)(μ 2 -PRCH 2 PR 2 ) (10) or Fe 4 (CO) 14 (μ 4 -P)(μ 2 -P(/Pr)Me) (6) are obtained. Uptake of one molecule of CO by 11 and ametallation of one CH 2 Ph substituent within the PR 2  donor group yields 12. Compound 10 • CH 2 C 12  crystallizes in the space group C2 1 /c with a = 36.357(7), b = 10.752(2), c = 22.879(5) Å , β - 112.45(1)°, Z = 8 {R = 0.050 for 5213 reflections). Both the phosphido atoms of the μ 2 - PRCH 2 PR 2  group and the μ 4 -P atom span the Fe1 -Fe2 bond of a Fe2(CO) 6  species while only the μ 4 -P atom spans the Fe3 -Fe4 bond of a (CO) 4 FeFe(CO) 3  fragment. In addition, the Fe(CO) 3  part of the latter unit is bonded to the tertiary P atom of the μ 2 -PRCH 2 PR 2  group. Compounds 11 and 12 cocrystallize in the space group P1 with a = 11.541(2), b = 17.739(2), c - 19.284(2) Å , a = 78.01(1), β = 78.68(1), y = 90.36(1)°, Z = 2 of each (R = 0.051 for 10234 reflections). A(CO) 3 Fe -Fe(CO)2-Fe(CO) 3  core having an acute Fe11-Fe12 -Fe13 angle of 77.46(3)° at the Fe(CO) 2  group is found for 11. The Fe12 - Fe13 bond is bridged by both the ,μ 3 -PR group and the hydride ligand. The Fe 11 -Fe 13 contact is spanned by the μ 3 -PR ligand and the ,μ 2 -P atom of the ,m 2- PRCH 2 PR 2  species. Three Fe(CO) 3  groups are bridged by the μ 3 -PR ligand in 12. Only two of the Fe(CO) 3  groups appear to be directly bonded. Fe21 -Fe23 is bridged by the μ 2 -P atom of the ,μ 2 -PRCH 2PRCHPh ligand while Fe22 -Fe23 displays a novel Fe22 - P - C -Fe23 linkage

zeitschrift für naturforschung b

Lineare Oligophosphaalkane, XII [1] PH-funktionelle Methylenbisphosphane — eine Quelle für Phosphinidene und Phosphoratome in Clustern und Fe4P-Spiroverbindungen / Linear Oligophosphaalkanes, XII [1] PH-Functional Methylenebisphosphanes — a Source of Phosphinidenes and Phosphorus Atoms in Clusters and Fe4P Spiro Compounds