10.1021/om201168h.s002 Michael D. Doud Michael D. Doud Kyle A. Grice Kyle A. Grice Alyssia M. Lilio Alyssia M. Lilio Candace S. Seu Candace S. Seu Clifford P. Kubiak Clifford P. Kubiak Versatile Synthesis of P<sup>R</sup><sub>2</sub>N<sup>R′</sup><sub>2</sub> Ligands for Molecular Electrocatalysts with Pendant Bases in the Second Coordination Sphere American Chemical Society 2012 Ni 1 H NMR Pendant Bases Molecular Electrocatalysts Versatile Synthesis PR 2NR Ligands PBn 2NPh phosphine substituent P 2N ligands PMe 2NPh 2012-02-13 00:00:00 Dataset https://acs.figshare.com/articles/dataset/Versatile_Synthesis_of_P_sup_R_sup_sub_2_sub_N_sup_R_sup_sub_2_sub_Ligands_for_Molecular_Electrocatalysts_with_Pendant_Bases_in_the_Second_Coordination_Sphere/2551114 Two 1,5-diaza-3,7-diphosphacyclooctane (P<sub>2</sub>N<sub>2</sub>) ligands with alkyl-substituted phosphines have been synthesized via a versatile method that allows for improved control of the phosphine substituent. The methyl- and benzyl-substituted phosphine P<sub>2</sub>N<sub>2</sub> ligands (P<sup>Me</sup><sub>2</sub>N<sup>Ph</sup><sub>2</sub> and P<sup>Bn</sup><sub>2</sub>N<sup>Ph</sup><sub>2</sub>) were synthesized and characterized by <sup>31</sup>P­{<sup>1</sup>H} NMR, <sup>1</sup>H NMR, and elemental analysis, and their corresponding [Ni­(P<sup>R</sup><sub>2</sub>N<sup>Ph</sup><sub>2</sub>)<sub>2</sub>]­(BF<sub>4</sub>)<sub>2</sub> complexes were synthesized and characterized by <sup>31</sup>P­{<sup>1</sup>H} NMR, <sup>1</sup>H NMR, and electrochemistry. The structure of the complex [Ni­(P<sup>Me</sup><sub>2</sub>N<sup>Ph</sup><sub>2</sub>)<sub>2</sub>]­(CF<sub>3</sub>SO<sub>3</sub>)<sub>2</sub> was characterized by X-ray crystallography.