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Synthesis of complexes 1 and 2: A mixture of CuI (0.114 g, KI (0.160 g, Ln2O3 [0.174 g for 1; 0.187 g for 2, Na2C2O4 (0.080 g, H2bic (0.100 g, H2O (10 ml, and 11.6 M HClO4 (pH, 2) was sealed in a 23 mL Teflon reactor and kept under autogenous pressure at 180 °C for 3 days. The mixture was cooled to room temperature at a rate of 5 °C h-1, and colorless plate crystals were obtained. 1: C25H15CuN6O8Sm (741.32, calcd, ) C 40.50, H 2.04, N 11.34; found C 40.39, H 2.24, N 11.52; IR (KBr, cm-1) 1650(s, 1622(s, 1598(w, 1541(s, 1490(w, 1414(s, 1238(w, 1124(w, 840(w, 793(m, 757(w, 693(w, 624(w, 589(w, 540(w, 2: C25H15CuDyN6O8 (753.47, calcd, ) C 39.85, H 2.01, N 11.15; found C 39.83, H 2.06, N 11.32; IR (KBr, cm-1) 1654s
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-1) 3434(m), 1623(s), 1543(s), 1414(s), 1316(w), 1241(w), 851(w), 795(m), 777(m), 696(w), 626(w).
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37
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77952107289
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Crystallographic data for complex 1: triclinic P, 1 with a, 9.879(4) Å, b, 11.941(5) Å, c, 12.257(5) Å, α, 62.107(4, β, 77.789(5, γ, 84.983(5)°, V, 1248.9(9) Å3, Z, 2, Dc, 1.971, F(000, 724, GOF, 1.071, R1(I>2σ(I, 0.0206, and wR2 (all data, 0.0556. 2: triclinic P, 1 with a, 9.7523(6, b, 11.9583(7, c, 12.2461(7) Å, α, 61.8090(10, β, 78.1720(11, γ, 84.9511(10)°, V, 1231.95(13) Å3, Z, 2, Dc, 2.031, F(000, 732, GOF, 1.070, R1(I>2σ(I, 0.0217, wR2 (all data, 0.0526. 3: triclinic P, 1 with a, 10.0261(15, b, 10.6352(16, c, 12.5835(19) Å, α, 66.299(2, β, 75.767(1, γ, 65.549(2)°, V, 1113.3(3) Å3, Z, 2, Dc= 2.028, F(000, 664, GOF, 1.083, R1(I>2σ(I, 0.0290, wR2 all data
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2 (all data) = 0.0862.
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