Accessing decaphenylmetallocenes of ytterbium, calcium, and barium by desolvation of solvent-separated ion pairs: Overcoming adverse solubility properties

被引:66
作者
Deacon, Glen B. [1 ]
Forsyth, Craig M. [1 ]
Jaroschik, Florian [1 ]
Junk, Peter C. [1 ]
Kay, Danielle L. [1 ,2 ]
Maschmeyer, Thomas [2 ]
Masters, Anthony F. [2 ]
Wang, Jun [1 ]
Field, Leslie D. [3 ]
机构
[1] Monash Univ, Sch Chem, Clayton, Vic 3800, Australia
[2] Univ Sydney, Sch Chem, Sydney, NSW 2006, Australia
[3] Univ New S Wales, Sch Chem, Kensington, NSW 2052, Australia
基金
澳大利亚研究理事会;
关键词
D O I
10.1021/om800501z
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The redox-transmetalation ligand-exchange reaction of ytterbium or calcium metal with 2 equiv of pentaphenylcyclopentadiene (C5Ph5H) and 1 equiv of HgPh2 in thf afforded the solvent-separated ion pairs (SSIPs) [M(thf)(6)][C5Ph5](2) (M = Yb, Ca), which were characterized by single-crystal X-ray analyses. Addition of toluene to the isolated SSIPs led to the precipitation of the homoleptic sandwich complexes [M(C5Ph5)(2)] (M = Yb, Ca). In the reaction of barium metal with C5Ph5H and HgPh2 the corresponding SSIP was observed in situ, and only the sandwich complex [Ba(C5Ph5)(2)] could be isolated. Single-crystal X-ray analyses were carried out for [M(C5Ph5)(2)] (M = Yb, Ba), which confirmed the highly symmetric structure of these complexes with two parallel cyclopentadienyl ligands. Oxidation and metal-ligand exchange reactions were investigated for the divalent ytterbium complexes.
引用
收藏
页码:4772 / 4778
页数:7
相关论文
共 73 条
[41]   Parallels between the chemistry of calcium(II) and ytterbium(II). Synthesis and crystal structure of a calcium alkoxo-phosphide cuboidal complex [J].
Izod, K ;
Clegg, W ;
Liddle, ST .
ORGANOMETALLICS, 2000, 19 (18) :3640-3643
[42]   Synthesis of a new stable, neutral organothulium(II) complex by reduction of a thulium(III) precursor [J].
Jaroschik, F ;
Nief, F ;
Ricard, L .
CHEMICAL COMMUNICATIONS, 2006, (04) :426-428
[43]   Synthesis and reactivity of organometallic complexes of divalent thulium with cyclopentadienyl and phospholyl ligands [J].
Jaroschik, Florian ;
Nief, Francois ;
Le Goff, Xavier-Frederic ;
Ricard, Louis .
ORGANOMETALLICS, 2007, 26 (14) :3552-3558
[44]   Isolation of stable organodysprosium(II) complexes by chemical reduction of dysprosium(III) precursors [J].
Jaroschik, Florian ;
Nief, Francois ;
Le Goff, Xavier-Frederic ;
Ricard, Louis .
ORGANOMETALLICS, 2007, 26 (05) :1123-1125
[45]   β-SiH agostic bonding in sterically crowded lanthanidocene silylamide complexes [J].
Klimpel, MG ;
Görlitzer, HW ;
Tafipolsky, M ;
Spiegler, M ;
Scherer, W ;
Anwander, R .
JOURNAL OF ORGANOMETALLIC CHEMISTRY, 2002, 647 (1-2) :236-244
[46]   Lanthanide-transition metal chalcogenido cluster materials [J].
Kornienko, A ;
Huebner, L ;
Freedman, D ;
Emge, TJ ;
Brennan, JG .
INORGANIC CHEMISTRY, 2003, 42 (25) :8476-8480
[47]   INERT-GAS PURGEBOX FOR FOURIER-TRANSFORM ION-CYCLOTRON RESONANCE MASS-SPECTROMETRY OF AIR-SENSITIVE SOLIDS [J].
MAY, MA ;
MARSHALL, AG .
REVIEW OF SCIENTIFIC INSTRUMENTS, 1994, 65 (03) :612-616
[48]   Superbulky ligands and trapped electrons: New perspectives in divalent lanthanide chemistry [J].
Meyer, Gerd .
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION, 2008, 47 (27) :4962-4964
[49]   Redistribution reactions of heteroleptic barium iodide derivatives:: Synthesis and structures of trans-BaI2(DME)(triglyme), cis-BaI2(DME)(tetraglyme) and [Ba(tetraglyme)2]I2 • C7H8 [J].
Mishra, Shashank ;
Pfalzgraf, Liliane G. Hubert ;
Jeanneau, Erwann .
POLYHEDRON, 2007, 26 (01) :66-72
[50]  
ORZECHOWSKI L, DALTON T IN PRESS