The Preparation, Spectroscopic Characterization and X-Ray Structure of the Salt [Pt(η1 -C6H9)(Cy2PCH2CH2PCy2)(PPh3)]HCO3·3H2O Containing the Discrete, Uncoordinated, Hydrogen-Bonded Dimeric Bicarbonate Dianion [(HCO3)(H2O)3]22-

Abstract

Reaction of the cyclohexyne–platinum(0) complex [Pt(η²-C₆H₈)(Cy₂PCH₂CH₂PCy₂)]* with water and CO₂ in the presence of triphenylphosphine gives the bicarbonate salt of the (η¹-cyclohexenyl)platinum(II) cation, [Pt(η¹-C₆H₉)(Cy₂PCH₂CH₂ PCy₂)(PPh₃)] [HCO₃] · 3H₂O, which has been characterized by n.m.r. spectroscopy and single-crystal X-ray diffraction at low temperature. Crystals are triclinic, space group P^1– with unit cell dimensions a 20.315(2), b 12.782(1), c 10.694(1) Å, α 66.61(1), β 104.73(1), γ 102.11(1)˚, and Z 2. The structure was refined to a final R value of 0.036 with use of 7553 reflections [I > 3σ(I)]. The cation has the expected, somewhat distorted planar coordination geometry; the anion consists of discrete, hydrogen-bonded dimers [(HCO₃)(H₂O)₃]₂^2-.