The metal-carbon coupling in dehydrohalogenation conditions between Pt(II) or Pd(II)square planar bisphosphine dichloride complexes and 2,6-diethynyl-4-nitroaniline (DENA)yielded organometallic polymers, i.e., -[M(PTol
3)
2(-C
![](/images/entities/tbd1.gif)
C-R-C
![](/images/entities/tbd1.gif)
C-)]
n- with R = p-NH
2C
6H
2NO
2 and M = Pt(II) or Pd(II). Dinuclear platinum complexes were also synthesized asgeometrical models. The polymers and complexes were fully characterized by means ofspectroscopic techniques. Accurate investigations with 2D nuclear magnetic resonance (NMR)spectroscopy were used to define the chemical and spatial structure of the polymeric chainsas a helical conformation for both Pt(II)- and Pd(II)-based organometallic polymers. Opticalabsorption studies and X-ray photoelectron spectroscopy measurements revealed the extentof conjugation and the nature of the ending groups.