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Synthesis of {[Zn3(sip)2(temdpy)2(e-urea)4(H2O)2].(e-urea)}n. (1) A mixture of Zn(NO3)3•6H2O (0.3 mmol), NaH2sip (0.2 mmol), tmdpy (0.2 mmol) and e-urea (20 mmol) were sealed in a 25 mL Teflon-lined stainless steel autoclave, heated at 120 °C for 3 days under autogenous pressure. After the reaction was cooled to room temperature, colorless crystals were produced (yield: 71%, based on Zn). Anal. Calc. for 1, C60H74Zn3N16O22 S2: C, 44.13%; H, 4.5%; and N, 13.73%. Found: C, 44.10%; H, 4.48%; and N, 13.42%.
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Synthesis of {[Zn3(sip)2(temdpy)2(e-urea)4(H2O)2].(e-urea)}n. (1) A mixture of Zn(NO3)3•6H2O (0.3 mmol), NaH2sip (0.2 mmol), tmdpy (0.2 mmol) and e-urea (20 mmol) were sealed in a 25 mL Teflon-lined stainless steel autoclave, heated at 120 °C for 3 days under autogenous pressure. After the reaction was cooled to room temperature, colorless crystals were produced (yield: 71%, based on Zn). Anal. Calc. for 1, C60H74Zn3N16O22 S2: C, 44.13%; H, 4.5%; and N, 13.73%. Found: C, 44.10%; H, 4.48%; and N, 13.42%.
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X-ray crystallographic study: diffraction intensities of 1 was collected at 293 K direction methods and difference Fouriersynthese (Mo-Ka, λ = 0.71073). 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: C60H74N16O22S2Zn3, M = 1631.58, monoclinic, a = 9.5755(19) Å, b = 10.066(2) Å, c = 19.233(4) Å, α = 78.790(7)° β = 75.954(7)° γ = 77.907(7)° V = 1738.2(6) Å3, T = 293(2) K, space group P-1, Z = 1, 12089 reflections measured, and 5211 independent reflections (Rint = 0.0262). The final R1 values were 0.0616 (I > 2σ(I)). The final wR(F2) values were 0.1693 (I > 2σ(I)). The final R1 values were 0.0711 (all data). The final wR(F2) values were 0.1773 (all data). The goodness of fit on F2 was 1.070.
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X-ray crystallographic study: diffraction intensities of 1 was collected at 293 K direction methods and difference Fouriersynthese (Mo-Ka, λ = 0.71073). 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: C60H74N16O22S2Zn3, M = 1631.58, monoclinic, a = 9.5755(19) Å, b = 10.066(2) Å, c = 19.233(4) Å, α = 78.790(7)° β = 75.954(7)° γ = 77.907(7)° V = 1738.2(6) Å3, T = 293(2) K, space group P-1, Z = 1, 12089 reflections measured, and 5211 independent reflections (Rint = 0.0262). The final R1 values were 0.0616 (I > 2σ(I)). The final wR(F2) values were 0.1693 (I > 2σ(I)). The final R1 values were 0.0711 (all data). The final wR(F2) values were 0.1773 (all data). The goodness of fit on F2 was 1.070.
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