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Synthesis of [DyCu(IN)2(Ox)·H2O]n (1, A mixture of Dy(NO3)3·6H2O (0.5 mmol, Cu(NO3)2·3H2O (1 mmol, isonicotinic acid (1 mmol) and oxalic acid (2 mmol) in 10 ml H2O was heated at 160 °C for 60 hrs under autogenous pressure. After the reaction was cooled in 60 hrs to room temperature, pale yellow crystals were produced (yield: 65, based on Cu, Anal. Calc. for 1, C14H10CuDyN2O9: C, 29.18; H, 1.75; N, 4.86, Found: C, 30.01; H, 1.27, N, 4.65, IR bands (cm- 1) for 1: 3442(m, 1611(vs, 1536(m, 1412(vs, 1220(w, 792(m, 770(m, 507(w, Synthesis of [EuCu(IN)2(Ox)·3H2O]n (2, A mixture of Eu(NO3)3·nH2O (0.5 mmol, Cu(NO3)2·3H2O (1 mmol, isonicotinic acid (1 mmol) and oxalic acid
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- 1) for 2: 3455(m), 1653(vs), 1544(s), 1410(vs), 1321(w), 1245(m), 765(m), 479(w).
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77953873057
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X-ray crystallographic study: diffraction intensities of 1 and 2 were collected at 293 K direction methods and difference Fourier syntheses (Mo-Ka, λ, 0.71073 Ǻ, Non-hydrogen atoms were refined anisotropically, and all hydrogen atoms were placed at ideal positions and allowed to ride. The crystallographic calculations were conducted using the SHELXL-97 programs. Crystal data for 1: C14H10CuDyN2O9, M, 576.26, monoclinic, a, 24.2047(1) Ǻ, b, 9.3475(2) Ǻ, c, 16.9878(3) Ǻ α, 90.00° β, 119.326(1)° γ, 90.00° V, 3350.98(9) Ǻ3, T, 293(2) K, space group C2, c, Z, 8,5625 reflections measured, 2897 independent reflections (Rint, 0.0210, The final R1 values were 0.0293 (I > 2σ(I, The final wR(F2) values were 0.0677 (I > 2σ(I, The final wR(F2) values were 0.0718 al
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2 was 1.047.
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0032045192
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Yanagida S., Hasegawa Y., Murakoshi K., Wada Y., Nakashima N., and Yamanaka T. Coord. Chem. Rev. 171 (1999) 461
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0036013965
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Beeby A., Burton-Pye B.P., Faulkner S., Motson G.R., Jeffery J.C., McCleverty J.A., and Ward M.D. Dalton Trans. (2002) 1923
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Beeby, A.1
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