Divalent lanthanide chemistry. Bis(pentamethylcyclopentadienyl)europium(II) and -ytterbium(II) derivatives: Crystal structure of bis(pentamethylcyclopentadienyl) (tetrahydrofuran) ytterbium(II)-hemitoluene at 176 K
Red, paramagnetic (diethyl ether)bis(pentamethylcyclopentadienyl)(tetrahydrofuran)europium(II), (Me/sub 5/C/sub 5/)/sub 2/Eu(THF)(Et/sub 2/O), is isolated from reaction of 3 molar equiv of sodium pentamethylcyclopentadienide and europium trichloride in refluxing tetrahyrofuran, after crystallization from diethyl ether. The mono(tetrahydrofuran) complex (Me/sub 5/C/sub 5/)/sub 2/Eu(THF) may be isolated by use of toluene rather than diethyl ether. Red, diamagnetic bis(pentamethylcyclopentadienyl)(tetrahydrofuran)ytterbium(II) is isolated from the reaction of ytterbium dichloride and sodium pentamethylcyclopentadienide in refluxing tetrahydrofuran. The diethyl ether complex (Me/sub 5/C/sub 5/)/sub 2/Yb(OEt/sub 2/) may be isolated by crystallization of the tetrahydrofuran complex from diethyl ether. The hemitoluene complex(Me/sub 5/C/sub 5/)/sub 2/Yb(THF)./sup 1///sub 2/tol can be isolated by recrystallization of the tetrahydrofuran complex from toluene. As these divalent metallocenes are the first hydrocarbon-soluble lanthanide derivatives to be isolated, we have examined the latter complex by X-ray crystallography. Crystals of (Me/sub 5/C/sub 5/)/sub 2/Yb(OC/sub 4/H/sub 8/)./sup 1///sub 2/C/sub 6/H/sub 5/CH/sub 3/ crystallize in the monoclinic system, P2/sub 1//n, with a = 11.358 (8) A, b = 21.756 (19) A, C = 10.691 (7) A, and ..beta.. = 101.84 (5)/sup 0/ at 176 K. For Z = 4 the calculated density is 1.37 g cm/sup -3/. The ytterbium atom is coordinated to the oxygen atom of a tetrahydrofuran molecule and to two pentamethylcyclopentadienyl rings. The molecule has approximate C/sub 2/ symmetry about the Yb-O bond. The Yb-O distance is 2.41 A, the Yb-C distances average 2.66 A, and the Yb-Cp(centroid) distances average 2.37 A. The Me/sub 5/C/sub 5/ rings are in a staggered configuration with respect to each other.
- Research Organization:
- Univ. of California, Berkeley
- DOE Contract Number:
- W-7405-ENG-48
- OSTI ID:
- 6969899
- Journal Information:
- Inorg. Chem.; (United States), Journal Name: Inorg. Chem.; (United States) Vol. 19:10; ISSN INOCA
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
400201* -- Chemical & Physicochemical Properties
400301 -- Organic Chemistry-- Chemical & Physicochemical Properties-- (-1987)
ALKENES
AROMATICS
BOND ANGLE
BOND LENGTHS
COHERENT SCATTERING
COMPLEXES
CRYSTAL LATTICES
CRYSTAL STRUCTURE
CYCLOALKENES
DIFFRACTION
DIMENSIONS
ETHERS
ETHYL ETHER
EUROPIUM COMPLEXES
FURANS
HETEROCYCLIC COMPOUNDS
HYDROCARBONS
LATTICE PARAMETERS
LENGTH
LOW TEMPERATURE
MONOCLINIC LATTICES
ORGANIC COMPOUNDS
ORGANIC OXYGEN COMPOUNDS
RARE EARTH COMPLEXES
SCATTERING
TETRAHYDROFURAN
TOLUENE
X-RAY DIFFRACTION
YTTERBIUM COMPLEXES