Analysis and Isolation of Cationic Rhenium(I) and Ruthenium(II) Multinuclear Complexes Using Size-Exclusion Chromatography

Abstract

Various cationic rhenium(I) and ruthenium(II) mono-and multinuclear complexes were successfully separated by sizeexclusion chromatography (SEC), using a 50:50 (v/v) mixture of methanol and acetonitrile with CH3CO2NH4 as an eluent. The logarithms of the molecular weights were accurately linear in the distribution coefficients: for linear-shaped rhenium(I) multinuclear complexes, log MW = -2.86KSEC + 5.24 (r = -0.990 and n = 15); for ring-shaped rhenium(I) multinuclear complexes, log MW = -2.94KSEC + 5.40 (r = -0.999; n = 5); for bimetallic complexes including ruthenium(II), log MW = -0.40KSEC + 3.37 (r = -0.959; n = 6). This separation method is applicable to the preparativescale separation of cationic multinuclear complexes from a mixture.

Rhenium(i) trinuclear rings as highly efficient redox photosensitizers for photocatalytic CO2 reduction

“…The eluent was MeOH–CH 3 CN (1 : 1 v/v) containing CH 3 COONH 4 (0.15 M) and the flow rate was 6.0 mL min –1 . 56 For analytical SEC, we used two sequentially connected Shodex KW-402.5-4F columns (300 mm × 4.6 mm i.d. ), a KW400G-4A guard-column (10 mm × 4.6 mm i.d.…”

Synthesis and Light-Harvesting Functions of Ring-Shaped Re(I) Trinuclear Complexes Connected with an Emissive Ru(II) Complex

“…One equivalent of dppph was added to the reaction solution, which was subsequently refluxed for 24 h, giving the target molecule [Ring-Ru1] 5+ as the major product (process C), as indicated by size-exclusion chromatography (SEC) analysis of the reaction solution ( Figure S1c ). 31 Through recycling size-exclusion chromatography (RSEC) and recrystallization, [Ring-Ru1] (PF 6 ) 5 was isolated in 44% isolated yield. Its 1 H NMR spectrum is shown in Figure 2 .…”

“…and a JAI LC-9201 recycling preparative HPLC apparatus (Japan Analytical Industry Co.) with a JASCO 870-UV detector (the detection wavelength was chosen as 360 nm); the eluent was MeOH–MeCN (1:1 v/v) containing CH 3 COONH 4 (0.15 M), and the flow rate was 6.0 mL min –1 . 31 For analytical SEC, two sequentially connected Shodex KW-402.5-4F columns (300 mm × 4.6 mm i.d.) were used, with a KW400G-4A guard-column (10 mm × 4.6 mm i.d.…”

Ru(ii)–Re(i) binuclear photocatalysts connected by –CH2XCH2– (X = O, S, CH2) for CO2reduction

“…The scan rate was 200 mV s –1 . Analytical SEC 12 was conducted using an HPLC system consisting of a JASCO 880-PU pump, a pair of Shodex PROTEIN KW402.5 columns, a KW-LG guard column, a Rheodyne 7125 injector, and a JASCO MD-2010 plus UV-Vis photodiode-array detector. The column temperature was maintained at 40 °C using a JASCO 860-CO column oven.…”