Darstellung und Charakterisierung komplexierter Triphosphane - Die Kristallstruktur von HP2

Article abstract of DOI:10.1016/0022-328X(91)86332-K

The reaction of M^IP(SiMe3)2 (M^I = Li, Na, K) with R2P(Cl)M'(CO)5 (R = Ph, Et; M' = Cr, W) or of PCl3 with M^IPPh2M'(CO)_n (M^I = Li, K; M' = Cr, W, n = 5; M' = Fe, n = 4) affords triphosphanes of the type HPn>2. 31P NMR investigations of the reaction mixtures show a number of precursor compounds, on which basis the formation mechanism can be discussed.The products were characerized by 1H, 13C, 31P NMR and IR spectroscopy, and mass spectrometry.HP2 (1) crystallises in the space group C2/c, with a 1873.0(7), b 934.8(4), c 2202.5(9) pm, β 113.76 deg (at -95 deg C) and Z = 4.The molecule possesses crystallographic twofold symmetry, but the central PH moiety is disordered across the twofold axis.The P-P bond lengths are 219.5(2) and 223.5(2) pm, with P-P-P 121.2(1) deg.