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, CA (United States)
- DOE Contract Number:
- W-7405-ENG-48
- OSTI ID:
- 6969899
- Journal Information:
- Inorg. Chem.; (United States), Vol. 19:10
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
YTTERBIUM COMPLEXES
CRYSTAL STRUCTURE
BOND ANGLE
BOND LENGTHS
CYCLOALKENES
ETHYL ETHER
EUROPIUM COMPLEXES
LATTICE PARAMETERS
LOW TEMPERATURE
MONOCLINIC LATTICES
TETRAHYDROFURAN
TOLUENE
X-RAY DIFFRACTION
ALKENES
AROMATICS
COHERENT SCATTERING
COMPLEXES
CRYSTAL LATTICES
DIFFRACTION
DIMENSIONS
ETHERS
FURANS
HETEROCYCLIC COMPOUNDS
HYDROCARBONS
LENGTH
ORGANIC COMPOUNDS
ORGANIC OXYGEN COMPOUNDS
RARE EARTH COMPLEXES
SCATTERING
400201* - Chemical & Physicochemical Properties
400301 - Organic Chemistry- Chemical & Physicochemical Properties- (-1987)