Author:
Colton R,McCormick MJ,Pannan CD
Abstract
The reactions of Pd(CO)X (X
= Cl, Br) with bis(diphenylphosphino)methane (dpm) and its arsenic analogue, dam, have been investigated.
The iodo complexes were prepared indirectly. Ligand dpm gives complexes of the formula [Pd(dpm)X]2.
With dam, the nature of the product depends upon the identity of the halogen;
with X = Cl, Br the products are [Pd(dam)X]2CO,
but the iodo derivative is [Pd(dam)I]2.
N.m.r. spectroscopy suggests that [Pd(dam)I]2 has a structure
different to the dpm complexes. ��� [Pd(dam)Cl]2CO,3C6H14
is tetragonal, space group P4I, a 22.0458(1), c 14.4345(1) Ǻ
containing four dimer units per unit cell. The structure was refined to R 0.096
and Rw 0.097 for 1698 independent reflections. The crystals are
molecular being composed of discrete dimeric molecules of the complex and
solvent. The palladium coordination is approximately square planar with two
trans arsenic atoms, terminal halogen and the bridging carbonyl group which is
common to both metal environments. There is no twist about the Pd-Pd axis so
the Pd,As, unit is planar. The Pd-Pd distance of
3.274(8) Ǻ is too long for a direct metal-metal bond. However, the
compound is diamagnetic so spin pairing must occur through the unusual carbonyl
bridge.
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