Abstract
Reaction of LaCl 3·7H 2O containing small amounts of La(NO 3) 3·7H 2O as an impurity with 12-crown-4 or 18-crown-6 in 3:1 CH 3CN:CH 3OH resulted in the isolation of the mixed anion complexes [LaCl 2(NO 3)(12-crown-4)] 2, [La(NO 3)(OH 2) 4(12-crown-4)]Cl 2·CH 3CN and [LaCl 2(NO 3)(18-crown-6)]. The nine-coordinate dimer, [LaCl 2(NO 3)(12-crown-4)] 2, has all of the anions in the inner coordination sphere and La 3+ has a capped square antiprismatic geometry. It crystallizes in the orthorhombic space group Pbca with (at −150 °C) a = 12.938(6), b = 15.704(3), c = 13.962(2) A ̊ , and D calc = 2.08 g cm −3 for Z = 4 . The second complex isolated from the same reaction, [La(NO 3)(OH 2) 4(12-crown-4)]Cl 2·CH 3CN, has the bidentate nitrate anion in the inner coordination sphere but the two chloride anions are in a hydrogen bonded outer sphere. This complex is ten-coordinate 4A,6B-expanded dodecahedral and crystallizes in the monoclinic space group P2 1 with (at 20 °C) a = 7.651(2), b = 11.704(7), c = 11.608(4) A ̊ , β = 95.11(2)°, and D calc = 1.80 g cm −3 for Z = 2 . The 18-crown-6 complex, [LaCl 2(NO 3)(18-crown-6)], has all inner sphere anions and has ten-coordinate 4A,6B-expanded dodecahedral La 3+ centers. It crystallizes in the orthorhombic space group Pbca with (at 20 °C) a = 14.122(7), b = 13.563(5), c = 19.311(9) A ̊ , and D calc = 1.89 g cm −3 for Z = 8 .
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