The synthesis and characterisation of [Pd(S2CNEt2){Ph2P(CH2)nPPh2}]+ salts of some chlorometallate anions (n=1, 3, 4): X-ray crystal structures of the salts [Pd(S2CNEt2){Ph2P(CH2)nPPh2}]2[MCl4] (n=1, 4; M=Cd; n=3; M=Hg)

Solid-State NMR Investigations of the Immobilization of a BF4−Salt of a Palladium(II) Complex on Silica

“…The structure of [Pd(dppp)(dtc)]BF 4 ·2CHCl 3 . (Figure ), as determined by single-crystal X-ray diffraction, shows that the [Pd(dppp)(dtc)] + cation is square planar around the Pd with Pd−S (2.3400(9), 2.3536(9) Å) and Pd−P distances (2.2699(9), 2.2679(9) Å) that are the same within experimental error as those in the same cation in [Pd(dppp)(dtc)] 2 HgCl 4 ·CH 2 Cl 2 ·H 2 O . The S1−Pd−S2 (75.54(3)°) and P1−Pd−P5 angles (90.72(4)°) are essentially the same as those in the HgCl 4 2− compound.…”

Synthesis of carbon-11 radiolabelled transition metal complexes using 11C-dithiocarbamates

“…In order to expand the scope of these 11 C-labelling reactions with other transition metals, a range of well-defined Pd(II) and Pt(II) diphosphine complexes were also investigated. Pd(II) and Pt(II) diphosphine complexes are known to form stable cationic chelating dithiocarbamate complexes, 37,38 and therefore present as suitable complexes for preliminary labelling reactions. We focused on labelling a small library of four Pd(II) and Pt(II) complexes containing the diphosphine ligands, 1,2-bisdiphenylphosphinoethane (dppe) and 1,3-bis-diphenylphosphinopropane (dppp), (Scheme 2).…”

“…Unlabelled reference complexes were prepared via the reaction of sodium N,N-diethyldithiocarbamate with Pd(II) or Pt(II) diphosphine chloride salts. 37,38 Single crystal X-ray crystal structures were obtained for the reference complexes [Pd(S 2 CNEt 2 )(dppp)]Cl and [Pt (S 2 CNEt 2 )(dppp)]Cl (Fig. 3).…”

“…The square planar molecular structures of the two complexes are isostructural and confirm the expected chelation of the dithiocarbamate ligand, varying only slightly in the bond lengths and angles at their respective metal centres (Table 2) and are similar to previously published DTC complexes. 38,39 Unlike the labelling reactions of the Au precursors that proceeded at room temperature, the reaction of 11 (7) were obtained in high RCYs of 96% and 89% respectively (Scheme 2, Table 1 entries 4 and 5). Labelling of the…”

“…The square planar molecular structures of the two complexes are isostructural and confirm the expected chelation of the dithiocarbamate ligand, varying only slightly in the bond lengths and angles at their respective metal centres (Table 2) and are similar to previously published DTC complexes. 38,39 Unlike the labelling reactions of the Au precursors that proceeded at room temperature, the reaction of 11 C-dithiocarbamate 1 with [PdCl 2 (dppe)] or [PtCl 2 (dppe)] required heating to 60 °C to give appreciable RCYs within 5–8 min in DMF to facilitate solubility. Under these conditions the labelled complexes [Pd([ 11 C]S 2 CNEt 2 )(dppe)]Cl ( 6 ) and [Pt([ 11 C]S 2 CNEt 2 )(dppe)]Cl ( 7 ) were obtained in high RCYs of 96% and 89% respectively (Scheme 2, Table 1 entries 4 and 5).…”