SYNTHESIS AND CRYSTAL STRUCTURE OF cis-equatorialSODIUM (ETHYLENEDIAMINE-N,N,N'- TRIACETATO)CHLORIDORHODATE(III) MONOHYDRATE, Na[RhCl(ed3a)]·H2O

Abstract

This complex was prepared by the procedure applied to make Rh(III) complexes with hexadentate edta-type ligands [1]. Ca3(ed3a)2⋅12H2O (1.99 g; 0.0025 mol) was dissolved in 15 ml of water and solution of 0.60 g (0.015 mol) NaOH in 5 ml of water was added. Ca(OH)2 precipitate was separated by filtration and in filtrate was added the solution of 1.05 g (0.005 mol) RhCl3·xH2O in 5 ml of water. The resulting mixture was stirred at 145 o C for 7 h. After cooling to room temperature, the yellow solution was filtered off and the filtrate was passed through a column supplied with the QAE A-25 Sephadex in the Cl– form. After elution with 0.1 M NaCl, two yellow bands were detected in the column. The first eluate was evaporated and desalted by passage through a Sephadex G-10 column. The elute was evaporated to ca. 3 ml and cis-equatorial-Na[Rh(ed3a)Cl]·H2O was crystallized after adding ethanol and cooling the solution in a refrigerator. Crystal data: monoclinic, space group P21/c, crystal size 0.1895 × 0.0717 × 0.0192 mm, a = 13.4003(6), b = 6.9326(3), c = 14.9772(8) Å, β = 115.328(6) °, V = 1257.62(12) Å3, Z = 4, ρ = 2.168 g cm–3, μ = 13.639 mm–1, R = 0.0511, wR = 0.0810.