Ligand Synthesis and Metalation. Using a procedure modified from the literature, isophthalic acid was treated with thionyl chloride followed by 2,6-diisopropylaniline, which provided the diamide (Scheme 1). Reaction of this compound with P2S5 in toluene at 100 °C yielded the bis(thioamide) 1, in an overall yield of 69% in two steps from commercial starting materials. Treating 1 with a slight excess of Fe(PMe3)4 in Et2O at room temperature led to effervescence and a color change from yellow-brown to dark green, and iron complex 2 was isolated in 93% yield (Scheme 1). Scheme 1. Synthesis and metalation of SCS pincer ligand 1. Dipp = 2,6-diisopropylphenyl.