TY - JOUR
T1 - Synthesis of cationic palladium(II) and platinum(II) complexes with a monodentate trialkylphosphoniumdithiocarboxylate ligand: molecular structure of trans-[Pd(C6F5)(PEt3)2(S2C–PEt3)]ClO4·CHCl3
AU - Usón, Rafael
AU - Forniés, Juan
AU - Navarro, Rafael
AU - Usón, Miguel A.
AU - Garcia, Maria P.
AU - Welch, Alan J.
PY - 1984
Y1 - 1984
N2 - Reaction of trans-[M(OClO3)(C6F5)(PR3) 2] with the zwitterion S2C-PR′3 affords the complexes trans-[M(C6F5)(PR3)2(S 2C-PR′3)]ClO4 (M = Pd; R3 = R′3 = Et3, Bu3, or Et2Ph; R = Bu, R′ = cyclo-C6H11; R = Ph, R′ = Et or cyclo-C6H11 M = Pt, R = R′ = Et or Bu). trans-[Pd(C6F5)(PEt3)2(S 2C-PEt3)]ClO4 is also given by reaction of [Pd(C6F5)(PEt3)3]ClO4 with CS2. Reaction of [M(OClO3)(C6F5)(bipy)] (bipy = 2,2′-bipyridyl) with S2C-PR′3 affords [M(C6F5)(bipy)(S2C-PR′ 3)]ClO4 (M = Pd or Pt; R′ = Et, Bu, or cyclo-C6A11). A crystallographic study of trans-[Pd(C6F5)(PEt3)2(S 2C-PEt3)]ClO4 (as its 1:1 chloroform solvate) shows that the cation contains a unidentate triethylphosphoniumdithiocarboxylate ligand, and 31P n.m.r. spectra of all products with two terminal phosphine ligands are consistent with trans stereochemistries. Crystals of trans-[Pd(C6F5)(PEt3)2(S 2C-PEt3)]ClO4·CHCl3 are monoclinic, space group P21/a, with a = 14.596 5(18), b = 15.356(3), c = 19.324 2(16) Å, β = 109.257(8)°, and Z = 4. Using 4 093 amplitudes the structure has been refined to R = 0.1049. The non-bonding Pd⋯S distance is 3.644(4) Å.
AB - Reaction of trans-[M(OClO3)(C6F5)(PR3) 2] with the zwitterion S2C-PR′3 affords the complexes trans-[M(C6F5)(PR3)2(S 2C-PR′3)]ClO4 (M = Pd; R3 = R′3 = Et3, Bu3, or Et2Ph; R = Bu, R′ = cyclo-C6H11; R = Ph, R′ = Et or cyclo-C6H11 M = Pt, R = R′ = Et or Bu). trans-[Pd(C6F5)(PEt3)2(S 2C-PEt3)]ClO4 is also given by reaction of [Pd(C6F5)(PEt3)3]ClO4 with CS2. Reaction of [M(OClO3)(C6F5)(bipy)] (bipy = 2,2′-bipyridyl) with S2C-PR′3 affords [M(C6F5)(bipy)(S2C-PR′ 3)]ClO4 (M = Pd or Pt; R′ = Et, Bu, or cyclo-C6A11). A crystallographic study of trans-[Pd(C6F5)(PEt3)2(S 2C-PEt3)]ClO4 (as its 1:1 chloroform solvate) shows that the cation contains a unidentate triethylphosphoniumdithiocarboxylate ligand, and 31P n.m.r. spectra of all products with two terminal phosphine ligands are consistent with trans stereochemistries. Crystals of trans-[Pd(C6F5)(PEt3)2(S 2C-PEt3)]ClO4·CHCl3 are monoclinic, space group P21/a, with a = 14.596 5(18), b = 15.356(3), c = 19.324 2(16) Å, β = 109.257(8)°, and Z = 4. Using 4 093 amplitudes the structure has been refined to R = 0.1049. The non-bonding Pd⋯S distance is 3.644(4) Å.
UR - http://www.scopus.com/inward/record.url?scp=37049110544&partnerID=8YFLogxK
U2 - 10.1039/DT9840000345
DO - 10.1039/DT9840000345
M3 - Article
AN - SCOPUS:37049110544
SN - 0300-9246
SP - 345
EP - 350
JO - Journal of the Chemical Society, Dalton Transactions
JF - Journal of the Chemical Society, Dalton Transactions
IS - 3
ER -