Abstract
Complexes of LaCl3·7H2O and CeCl3·7H2O directly coordinated to 15-crown-5 were prepared by placing the reactants in 3∶1 CH3CN∶CH3OH on opposite sides of a fine porosity glass frit in a U-shaped cell and passing a 10 μA current through the cell. The crystal structures of the two anhydrous 8-coordinate complexes, [MCl3(15-crown-5)] (M=La, Ce) have been determined. Each contains the lanthanide in a bicapped trigonal prismatic geometry. The two complexes are isostructural crystallizing in the monoclinic space groupP21/c with (at 20°C) for M=La:a=8.217(8),b=14.298(2),c=14.341(9) A, β=104.79(8)°, andD calc=1.90 g cm−3 forZ=4; for M=Ce:a=8.208(9),b=14.263(6),c=14.270(8) A, β=104.74(7)°, andD calc=1.92 g cm−3 forZ=4. Direct reaction of ErCl3·6H2O with 15-crown-5 in 3∶1 CH3CN∶CH3OH resulted in the crystallization of the second sphere hydrogen bonded complex [Er(OH2)8]Cl3·15-crown-5. This complex is monoclinic,P21/n with (at 18°C)a=9.193(3),b=17.235(9),c=15.216(5) A, β=92.48(3)°, andD calc=1.76 g cm−3 forZ=4. The Er3+ ion is dodecahedral.
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