Premium
Formation and Structure of Thulium(III) Cyclopentadienides as Products of Reactions Directed Towards the Synthesis of Thulium(II) Cyclopentadienides
Author(s) -
Fedushkin Igor L.,
Girgsdies Frank,
Schumann Herbert,
Bochkarev Mikhail N.
Publication year - 2001
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/1099-0682(200109)2001:9<2405::aid-ejic2405>3.0.co;2-n
Subject(s) - chemistry , thulium , dimethoxyethane , yield (engineering) , solvent , molecule , mass spectrometry , medicinal chemistry , nuclear magnetic resonance spectroscopy , spectroscopy , inorganic chemistry , crystallography , stereochemistry , organic chemistry , physics , materials science , optoelectronics , electrode , doping , chromatography , quantum mechanics , electrolyte , metallurgy
TmI 2 (THF) 2 and [C 5 Me 5 ]K react in THF to yield the Tm III complex (C 5 Me 5 ) 2 TmI(THF) ( 1 ). The reaction of 1 with excess sodium in 1,2‐dimethoxyethane (DME) leads, through Tm II intermediates and a reductive splitting of DME solvent molecules, to the trisodium dithulium(III) complex [(DME) 2 Na(µη 5 :η 5 ‐C 5 Me 5 )Tm(η 5 ‐C 5 Me 5 )(µ 2 ‐OMe) 2 (Na‐µ‐η 5 :η 5 ‐C 5 Me 5 )Na(µ‐OMe) 2 Tm(η 5 ‐C 5 Me 5 ) 2 ] ( 2 ). Treatment of TmI 2 (THF) 2 with [(Me 3 Si) 2 C 5 H 3 ]MgCl ( 3 ) in THF yields the dimeric Tm III complex [{1,3‐(Me 3 Si) 2 C 5 H 3 } 2 TmCl] 2 ( 4 ), while TmI 3 (THF) 3 reacts with [C 5 H 4 CH 2 CH 2 NMe 2 ]K(THF) ( 5 ) to yield solvent‐free (C 5 H 4 CH 2 CH 2 NMe 2 ) 2 TmI ( 6 ). The new Tm III compounds have been characterized by elemental analysis, IR spectroscopy, and mass spectrometry. The molecular structures of 2 , 4 , 5 , and 6 have been determined by single‐crystal X‐ray diffraction analysis.