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Anal. Caled for C36H38Cl2N 20Ni4O12 (1, C, 34.6; H, 3.1; N, 22.4. Found: C, 34.6; H, 3.0; N, 22.6, IR (KBr, cm-1, 1100 br (ClO 4, Anal. Caled for C52H56Cl 4N26Ni8O30 (2, C, 29.2; H, 2.6; N, 17.1. Found: C, 29.6; H, 2.8; N, 17.5, IR (KBr, cm-1, 1100 br (ClO4, C17H19MnN2O 6 (2-H2O, C, 50.74; H, 4.76; N, 6.97. Anal. Caled for C74H89Cl4N43Ni12O 38 (3, C, 29.3; H, 3.0; N, 19.8. Found: C, 29.6; H, 3.0; N, 19.6, IR (KBr, cm-1, 2036 s (vs, N=N=N, 1100 br ClO4
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19
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73049114423
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Crystal data for 1: C36H38Cl2N 20Ni4O12 (Mr, 1248.60, triclinic, P1̄, a, 10.444(2) Å, b, 11.355(2) Å, c, 11.697(2) Å, α, 101.92(3)°, β, 101.18(3)°, γ, 112.71(3)°, V, 1193.1(4) Å3, Pcalcd, 1.738 g cm-3, μ, 1.748 mm-1, T, 293 K, MoKα, λ, 0.71073 Å, 9114 measured reflections, 4166 independent reflections, Rint, 0.0868. R1, 0.0939, wR2, 0.2131 (I > 2σ(I, and S, 1.034. Crystal data for 2: C52H56Cl4N26Ni 8O30 (Mr, 2136.71, monoclinic, P2 1/c a, 15.936(3) Å, b, 17.524(4) Å, c, 14.848(3) Å, β, 110.53(3, V, 3883.0(14) Å3, ρcalcd, 1.828 g cm-3, μ, 2.132 mm-1, T= 293 K, Mokα, λ
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int = 0.0893. R1 = 0.0729, wR2 = 0.1671 (I > 2σ(I)) and S = 1.039.
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0001301919
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