Synthetic routes towards novel PCP′ pincer ligands were devised. Ligand 1-(Pr2iPOCH2)- 3-(Bu2tPCH2)(C6H4) is prepared in a three step synthesis from 1, 3-benzenedimethanol and 1-(Pr2iPO)-3-(Bu2tPCH2)(C6H4) is accessible in three steps from 3- hydroxybenzylalcohol. Both their palladium (II) complexes are prepared in good yields but are distinctly different since [PdCl {(C6H3)(OPPr2i)-2-(CH2PBu2t)-6}] possesses two five- ...