SYNTHESIS AND COORDINATION CHEMISTRY OF THE FIRST WATER-SOLUBLE DITHIO-BIS(PHOSPHINE) LIGANDS [(HOH2C)(2)P(CH2)(2)S-X-S(CH2)(2)P(CH2OH)(2)](X=(CH2)(3) OR C6H4) - X-RAY CRYSTAL-STRUCTURE OF )(2)P(CH2)(2)S(CH2)(3)S(CH2)(2)P(CH2OH)(2)](CL)(2)
Cj. Smith et al., SYNTHESIS AND COORDINATION CHEMISTRY OF THE FIRST WATER-SOLUBLE DITHIO-BIS(PHOSPHINE) LIGANDS [(HOH2C)(2)P(CH2)(2)S-X-S(CH2)(2)P(CH2OH)(2)](X=(CH2)(3) OR C6H4) - X-RAY CRYSTAL-STRUCTURE OF )(2)P(CH2)(2)S(CH2)(3)S(CH2)(2)P(CH2OH)(2)](CL)(2), Inorganic chemistry, 36(9), 1997, pp. 1786-1791
The thioether-functionalized, water-soluble, bis(phosphines) (HOH2C)(2
)PCH2CH2S(CH2)(3)SCH2CH2P(CH2OH)(2) (9) and C6H4{1,2-SCH2CH2P(CH2OH)(2
)}(2) (10) were synthesized in near quantitative yields by the formyla
tion of the appropriate phosphine hydrides in the presence of formalde
hyde in ethanol. The reactions of 9 and 10 with Pt(COD)Cl-2 and Pd(C6H
5CN)(2)Cl-2 in biphasic media (aqueous/organic) produced the water-sol
uble Pt(II) and Pd(II) complexes )(2)P(CH2)(2)S(CH2)(3)S(CH2)(2)P(CH2O
H)(2)](Cl)(2) (11), )(2)P(CH2)(2)S(CH2)(3)S(CH2)(2)P(CH2OH)(2)](Cl)(2)
(12), [Pt{(C6H4){1,2-S(CH2)(2)P(CH2OH)(2)}(2)}](Cl)(2) (13), and [Pd{
(C6H4){1,2-S(CH2)(2)P(CH2OH)(2)}(2)}](Cl)(2) (14) in near quantitative
yields. The X-ray crystal structure of 12 confirms a square-planar Pd
(II) structure for this new generation of water-soluble transition met
al complexes. All of the complexes were characterized by MS, H-1, C-13
, and P-31 NMR spectroscopy, X-ray data for 12: triclinic, <P(1)over b
ar>, a = 9.9761(6) Angstrom, b = 10.2049(7) Angstrom, c = 11.6954(7) A
ngstrom, alpha = 67.730(10)degrees, beta = 69.943(10)degrees, gamma =
79.828(10)degrees, Z = 2, R = 0.0307 (R-w = 0.0797).