Monophosphine and diphosphine ligands for diplatinum polyynediyl complexes: Efficient syntheses of new functionality-containing systems and model compounds

Coordination‐Driven Self‐Assembly, Structures, and Dynamic Properties of Diplatinum Hexatriynediyl and Butadiynediyl Complexes in which the sp Carbon Chains are Shielded by sp3 Carbon Chains: Towards Endgroup–Endgroup Interactions

“…Syntheses and structures of bridged butadiynediyl complexes: Similar reactions of the butadiynediyl complex PtC 4 Pt and the diphosphines Ar 2 PA C H T U N G T R E N N U N G (CH 2 ) 8 PAr 2 (Ar = Ph, ptol) [28,29] were investigated. As shown in Scheme 3 (bottom), workups gave the target complexes PtC 4 Pt-8/Ph and PtC 4 Pt-8/p-tol in good yields.…”

“…1 6 Pt-8/p-tol): A Schlenk flask was charged with PtC 6 Pt (0.228 g, 0.113 mmol) and THF (75 mL). Solid p-tol 2 PA C H T U N G T R E N N U N G (CH 2 ) 8 Pp-tol 2 (0.144 g, 0.272 mmol) [29] was added in one portion with stirring. After 36 h, the mixture was concentrated (to % 20 mL) and ethanol (50 mL) was added.…”

“…DSC: endotherm: T i = 205.3, T e = 225.4, T c = 244.5, T f = 247.6 8C; TGA (onset of mass loss): T i = 271.1, T e = 283.0, T f = 401. 14 Pp-tol 2 (0.066 g, 0.11 mmol) [29] was added in one portion with stirring. After 6 h, the mixture was concentrated under vacuum and ethanol www.chemeurj.org (30 mL) was added.…”

“…48 mmol) [29] was added in one portion with stirring. After 12 h, the mixture was concentrated under vacuum and ethanol (30 mL) was added.…”

“…The solvent was removed from the product-containing fractions by rotary evaporation. The residue was recrystallized from hexanes and dried by oil pump vacuum to give PtC 4 Pt-8/Ph as a light yellow solid (0.024 g, 0.014 mmol, 53 %), decomp point 160 8C (capillary, onset 13 mmol) [29] in CH 2 Cl 2 (65 mL) was passed through a silica gel pad (2 cm) directly into the Schlenk flask with stirring. After 12 h, the mixture was concentrated (to % 80 mL), and ethanol (50 mL) was added.…”