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Title: Tertiary phosphine complexes of the f-block metals. Preparation of pentamethylcyclopentadienyl-tertiary phosphine complexes of ytterbium(II), ytterbium(III), and europium(II). Crystal structure of Yb(Me/sub 5/C/sub 5/)/sub 2/Cl(Me/sub 2/PCH/sub 2/PMe/sub 2/)

Journal Article · · Inorg. Chem.; (United States)
DOI:https://doi.org/10.1021/ic00148a002· OSTI ID:6263668

The diphosphine, Me/sub 2/PCH/sub 2/CH/sub 2/PMe/sub 2/, reacts with M(Me/sub 5/C/sub 5/)/sub 2/(OEt/sub 2/) to give insoluble M(Me/sub 5/C/sub 5/)/sub 2/(Me/sub 2/PCH/sub 2/CH/sub 2/PMe/sub 2/), where M is Eu or Yb. In contrast, Me/sub 2/PCH/sub 2/PMe/sub 2/ gives the hydrocarbon-soluble complexes M(Me/sub 5/C/sub 5/)/sub 2/(Me/sub 2/PCH/sub 2/PMe/sub 2/), where M is Eu or Yb. The ytterbium complex reacts with YbCl/sub 3/ in toluene to give Yb(Me/sub 5/C/sub 5/)/sub 2/Cl(Me/sub 2/PCH/sub 2/PMe/sub 2/), and the crystal structure shows that the phosphine is acting as a monodentate ligand. Yb(Me/sub 5/C/sub 5/)/sub 2/Cl(Me/sub 2/PCH/sub 2/PMe/sub 2/) crystallizes in the monoclinic space group P2/sub 1//c with a = 16.358 (6) A, b = 8.595 (4) A, c - 20.712 (7) A, ..beta.. = 104.75 (4)/sup 0/, V = 2816 A/sup 3/, and d(calcd) = 1.45 g cm/sup -3/ for Z = 4 and mol wt = 615.15. Diffraction data were collected with a CAD-4 automated diffractometer, and the structure was refined to R = 0.054 for 3309 reflections with 4/sup 0/ < 2theta < 45/sup 0/ (Mo K..cap alpha.. radiation). The Yb is coordinated to the two Me/sub 5/C/sub 5/ groups, to the chlorine atom, and to one phosphorus atom of the bis(dimethylphosphino)methane ligand. The Yb-P and Yb-Cl distances are 2.94 and 2.53 A, respectively. The centroids of the C/sub 5/Me/sub 5/ ligands and the Cl and P atoms are in an approximate tetrahedral arrangement about the Yb atom.

Research Organization:
Univ. of California, Berkeley
DOE Contract Number:
AC03-76SF00098
OSTI ID:
6263668
Journal Information:
Inorg. Chem.; (United States), Vol. 22:6
Country of Publication:
United States
Language:
English