10.1021/om400335a.s001
Brennen A. Harding
Brennen A.
Harding
Patrick R. Melvin
Patrick R.
Melvin
William Dougherty
William
Dougherty
Scott Kassel
Scott
Kassel
Felix E. Goodson
Felix E.
Goodson
Capturing a Ghost. Synthesis and Structural Characterization
of Pd(dba)[P(<i>o</i>‑Tol)<sub>3</sub>]<sub>2</sub>
American Chemical Society
2013
dba
Pd
tris
literature synthesis
alternative synthesis
Structural Characterization
phosphine ligands
polymerization reactions
palladium compound
palladium complexes
2013-06-24 00:00:00
Journal contribution
https://acs.figshare.com/articles/journal_contribution/Capturing_a_Ghost_Synthesis_and_Structural_Characterization_of_Pd_dba_P_i_o_i_Tol_sub_3_sub_sub_2_sub_/2402773
In
an effort to improve upon a literature synthesis of bis[tris(<i>o</i>-tolyl)phosphine]palladium(0) (<b>1</b>) from tris(<i>o</i>-tolyl)phosphine and Pd<sub>2</sub>(dba)<sub>3</sub>, we
instead isolated a new compound which proved to have the composition
Pd(dba)[P(<i>o</i>-Tol)<sub>3</sub>]<sub>2</sub> (<b>2</b>), upon analysis by X-ray crystallography. While this is
not the first known palladium compound containing both dba and phosphine
ligands, it is, to our knowledge, the first containing dba and tris(<i>o</i>-tolyl)phosphine. This is significant, because mixtures
of Pd<sub>2</sub>(dba)<sub>3</sub> and tris(<i>o</i>-tolyl)phosphine
are routinely used in cross-coupling protocols, and palladium complexes
containing dba and tris(<i>o</i>-tolyl)phosphine have been
cited as intermediates in organometallic and polymerization reactions.
The most interesting crystallographic parameter for <b>2</b> is an abnormally long Pd–P bond length of 2.388(1) Å,
which we believe is the cause of this complex’s metastability.
We also present an alternative synthesis of <b>1</b> that does
not require a large excess of phosphine.