SYNTHESIS AND CRYSTAL STRUCTURE OF cis-equatorialAQUAETHYLENEDIAMINE-N,N,N'-TRIACETATORHODIUM(III) MONOHYDRATE, [Rh(ed3a)H2O]xH2O

Abstract

This complex was prepared by the procedure used to make Rh(III) complexes with hexadentate edta-type of ligands [1]. Ca3(ed3a)212H2O (1.99 g; 0.0025 mol) was dissolved in 15 mL of water and solution of 0.6 g (0,015 mol) NaOH in 5 mL of water was added. The deposited Ca(OH)2 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 145oC for 7h. 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 Clform. After elution with water, one yellow band was isolated. The band was evaporated to ca. 1 mL and cis-equatorial-[Rh(ed3a)H2O]xH2O was crystallized after adding ethanol and cooling the solution in a refrigerator. Crystal data: monoclinic, space group P21/n, crystal size 0.1918 × 0.0712 × 0.0460 mm3 , a = 6.94313(8), b = 15.71268(18), c = 11.09315(11) Å, β = 96.9886(10)°, V = 1201.22(2) Å3 , Z = 4, ρx = 2.047 g cm-3 , μ = 1.462 mm-1 , R1 = 0.0358, wR2 = 0.0527