Synthesis and characterization of a mixed-ring bis-cyclopentadienyl derivative of neodymium. X-ray crystal structures of (eta-C5Me5)NdI2(py)(3) and (eta-C5Me5)(eta-C5H4SiMe3)NdI(py)

Citation
Dl. Clark et al., Synthesis and characterization of a mixed-ring bis-cyclopentadienyl derivative of neodymium. X-ray crystal structures of (eta-C5Me5)NdI2(py)(3) and (eta-C5Me5)(eta-C5H4SiMe3)NdI(py), POLYHEDRON, 18(10), 1999, pp. 1389-1396
Citations number
49
Language
INGLESE
art.tipo
Article
Categorie Soggetti
Inorganic & Nuclear Chemistry
Journal title
POLYHEDRON
ISSN journal
0277-5387 → ACNP
Volume
18
Issue
10
Year of publication
1999
Pages
1389 - 1396
Database
ISI
SICI code
0277-5387(1999)18:10<1389:SACOAM>2.0.ZU;2-H
Abstract
Reaction of neodymium metal with 1.5 equiv of elemental iodine in iso-propa nol, followed by crystallization from THF, leads to isolation of NdI3(TKF)( x) (1). Compound 1 reacts with one equiv of KC5Me5 to produce the mono-pent amethylcyclopentadienyl derivative (eta-C5Me5)NdI2(THF)(3) (2) in moderate yield. Treatment of 2 with an excess of pyridine in toluene leads to displa cement of the THF ligands and formation of the tris-pyridine adduct (eta-C5 Me5)NdI2(py)(3) (3). Compound 3 reacts with one equiv of KC5H4SiMe3 to yiel d the mixed-ring complex (eta-C5Me5)(eta-C5H4SiMe3)NdI(py) (4). Single crys tal X-ray diffraction studies have been performed on complexes 3 and 4. (et a-C5Me5)NdI2(py)(3) (3) adopts a pseudo-octahedral geometry in the solid st ate, with the cyclopentadienyl ligand occupying one coordination site, the three pyridine ligands in a mer-configuration, and the iodide ligands trans to one another. The Nd-I distance is 3.1603(5) Angstrom, while Nd-N bond l engths to the pyridine ligands are 2.631(4) and 2.678(6) Angstrom. The soli d state structure of (eta-C5Me5)(eta-C5H4SiMe3)NdI(py) (4) features a typic al bent metallocene Cp2MX2 geometry with Nd-I and Nd-N distances of 3.0664( 4) and 2.555(4) Angstrom, respectively. (C) 1999 Elsevier Science Ltd. All rights reserved.