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66849141923
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Synthesis of [Cd2(Py2S)3(NO 3)4]n 1: Cd(NO3)2 · 4H 2O (25 mg, 0.08 mmol) dissolved in an acetonitrile solution (2 mL) was carefully layered onto a 2 mL CH2Cl2 solution of Py2S (23 mg, 0.12 mmol, Colorless crystals were obtained in two days in ca. 63% yield. FT-IR (KBr, vc=c, 1581 and 1479 cm-1; vN-o, 1833 cm-1. Anal. Calcd, ) for C 30H24Cd2N10O12S 3: C, 34.73; H, 2.33; N, 13.50. Found, C, 34.86; H, 2.46; N, 13.25. Synthesis of, Cd(Py2S)2(DMF)2](ClO 4)2}n 2: Cd(ClO4) 2·6H2O (34 mg, 0.08 mmol) dissolved in a DMF solution (2 mL) was carefully layered onto a 2 mL CH2Cl2 solution of Py2S 30 mg, 0
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5: C, 38.36; H, 2.97; N, 8.60. Found (%): C, 38.12; H, 2.76; N, 8.79.
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0034740392
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35
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66849140838
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Crystal data: 1·CH2Cl2, C 31H26Cd2Cl2N10O 12S3, M, 1122.50, triclinic, space group P1̄, T, 295(2) K, a, 11.2141(1, b, 12.5092(1, c, 17.2612(2) Å, α, 104.4338(4, β, 100.1570(5, γ, 109.3781(5)°, V= 2121.32(4) Å3, Z, 2, μ, 1.345 mm-1, F(000, 1112, 30 381 reflections collected, 9720 independent, Rint, 0.0396, final residuals R1, 0.0560, wR2, 0.1529 [I > 2σ(I, R1, 0.0886, wR2, 0.1878 (all data, Crystal data: 2, C26H30CdCl 2N6O10S2, M, 834.01, mono-clinic, space group P21/c, T, 273(2) K, a, 10.4730(8, b, 19.2211(14, c, 19.0207(11) Å, β, 113.114(3)°, V
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int = 0.0575, final residuals R1 = 0.0364, wR2 = 0.0853 [I > 2σ(I)]; R1 = 0.0407, wR2 = 0.0872 (all data).
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Yitzchaik, S.8
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