Partial hydrolysis (H 2 O/Ln molar ratio = ¼) of lanthanum di-iso-propylcarbamato complex, [La(O 2 CN i Pr 2) 3 ], 1, afforded the tetranuclear µ-oxo derivative [La 4 O(O 2 CN i Pr 2) 10 ], 2, which was structurally characterized by single crystal X-Ray diffraction studies. The carbonatocarbamato derivative of lanthanum, [La 4 (CO 3)(O 2 CNBu 2) 10 ], 3, was prepared by extraction of lanthanum ions from aqueous solution into heptane by the NHBu 2 /CO 2 system. Partial hydrolysis (H 2 O/Ln molar ratio = ½) of N,N-di-iso-propylcarbamato complexes of neodymium, europium, gadolinium and terbium, [Ln(O 2 CN i Pr 2) 3 ], yielded the derivatives [Ln 2 (CO 3)(O 2 CN i Pr 2) 4 ] (Ln = Nd, 4, Eu, 5, Gd, 6). Exhaustive hydrolysis of [Ln(O 2 CNR 2) 3 ] (Ln = Nd, Tb, R = Bu; Ln = Eu, Gd, R = i Pr, Bu) produced hydrated lanthanide carbonates, Ln 2 (CO 3) 3 · n H 2 O. For sake of comparison with a block d metal, the exhaustive hydrolysis of two copper(II) carbamato complexes, [Cu(O 2 CNEt 2) 2 (NHEt 2)] 2 and [Cu(O 2 CNiPr 2) 2 ], was carried out with formation in both cases of the hydrated basic carbonate Cu 2 (OH) 2 (CO 3)·nH 2 O. The exhaustive hydrolysis of mixtures of cerium and lanthanum or cerium and terbium N,N-dibutylcarbamato complexes allowed the preparation of mixed oxides containing the two metals in the desired molar ratio, via the intermediate formation of the corresponding mixed carbonates.
Exhaustive hydrolysis of a mixture of [La4(CO3)(O2CNBu2)10] and [Cu(O2CNBu2)(py∗)2] (py∗ = 4-dimethylamino pyridine) in molar ratio 1/2 corresponding to a La/Cu molar ratio 2/1 was carried out in toluene at room temperature. The carbamato derivatives of lanthanum and copper can be easily prepared by extraction of the metal ions from aqueous solution into heptane by the NHBu2/CO2 system, according to a method previously reported. The copper precursor was selected among a number of derivatives in respect of its easy tractability. The tetragonal modification T’ of La2CuO4 was obtained by treatment at 600 °C of the intermediate mixed carbonate. The thermal treatment of T’-La2CuO4 at 850 °C, followed by cooling down to room temperature, afforded the orthorhombic modification of the mixed oxide
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