An Rh-105 complex of tetrathiacyclohexadecane diol with potential for formulating bifunctional chelates.
1,5,9,13-Tetrathiacyclohexane-3,11-diol (16S4-diol), a sulfur crown ether analog, was studied as a potential chelating agent to complex no-carrier-added (NCA) grade 105Rh(III) in high yield at low ligand concentrations. trans-[RhCl2(16S4-diol)]chi (chi = Cl, PF6) was prepared using nonradioactive RhCl3.3H2O and characterized by UV-Vis, nuclear magnetic resonance (NMR) and X-ray crystallography. It was shown to have a +1 charge with the Rh(III) metal center coordinated to the four S atoms equatorially and two Cl atoms in trans axial positions. The 105Rh-16S4-diol complex prepared with NCA 105Rh(III)-chloride reagent was found to exhibit identical chromatographic properties as trans-[Rh(III)Cl2(16S4-diol)]+ (including silica and C-18 thin-layer chromatography [TLC] and electrophoresis). The preparation of 105Rh-16S4-diol complex formation optimized for conditions of pH, temperature, time, % ethanol and quantity of 16S4-diol resulted in yields > 90%. Very low quantities of 16S4-diol (3 nmol) complex NCA 105Rh(III) under relatively mild reaction conditions (heating at 64 degrees C for 90 min) in the presence of ethanol (10%), yielded the high specific activity 105Rh-16S4-diol complex as a single cationic species. The 105Rh-16S4-diol complex was shown to be stable for > or = 4 days in physiological buffers at room temperature and in human serum at 37 degrees C.
Venkatesh
M
M
Isotope Division, B.A.R.C., Trombay, Bombay, India.
Goswami
N
N
Volkert
W A
WA
Schlemper
E O
EO
Ketring
A R
AR
Barnes
C L
CL
Jurisson
S
S
D002614:Chelating Agents / Q000737:chemistry*; D002855:Chromatography, Thin Layer; D004988:Ethers, Cyclic / Q000737:chemistry*; D007553:Isotope Labeling; D009682:Magnetic Resonance Spectroscopy; D009942:Organometallic Compounds / Q000737:chemistry*; D011868:Radioisotopes; D012238:Rhodium / Q000737:chemistry*; D013056:Spectrophotometry, Ultraviolet; D014961:X-Ray Diffraction
D002614:Chelating Agents; D004988:Ethers, Cyclic; D009942:Organometallic Compounds; D011868:Radioisotopes; C103148:rhodium tetrathiacyclohexadecanediol dichloride; D012238:Rhodium