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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), Journal Name: Inorg. Chem.; (United States) Vol. 22:6; ISSN INOCA
Country of Publication:
United States
Language:
English

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Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400201* -- Chemical &amp; Physicochemical Properties
400301 -- Organic Chemistry-- Chemical &amp; Physicochemical Properties-- (-1987)
ALKENES
BOND LENGTHS
CHEMICAL PREPARATION
CRYSTAL STRUCTURE
CYCLOALKENES
CYCLOPENTADIENE
DATA
DIENES
DIMENSIONS
EUROPIUM COMPOUNDS
EXPERIMENTAL DATA
HYDROCARBONS
INFORMATION
LENGTH
NUMERICAL DATA
ORGANIC COMPOUNDS
ORGANOMETALLIC COMPOUNDS
PHOSPHINES
PHOSPHORUS COMPOUNDS
POLYENES
RARE EARTH COMPOUNDS
STRUCTURAL CHEMICAL ANALYSIS
SYNTHESIS
YTTERBIUM COMPOUNDS