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78651319372
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note
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Synthesis of 1: A solution of Cd(NO3)2•4H2O (0.0683 g, 0.22 mmol), 4-PyBIm (0.0386 g, 0.02 mmol), H2cam acid (0.0500 g, 0.25 mmol), Na2CO3 (0.0233 g, 0.22 mmol) and H2O (4 mL) was stirred 20 minutes under ambient conditions, then sealed in a Teflon-lined steel autoclave, heated at 160 °C for 3 days. After the vessel was cooled naturally to room temperature, The resulting product was recovered by filtration, washed with distilled water and then colorless block crystals were obtained. (80% yield) Anal. Calcd. for C44H46Cd2N6O8: C, 52.24H, 4.58N, 8.31 %. Found: C, 51.81; H, 4.52; N, 8.29 %.
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78651315498
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note
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X-ray crystallographic study: diffraction intensities of 1 were collected at 293 K direction methods and difference Fourier synthese (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: C44H46Cd2N6O8, M = 1011.67, monoclinic, a = 7.471(2) Å, b = 17.123(5) Å, c = 17.192(5) Å, β = 96.056(4)° V = 2187.0(10) Å, 3, T = 293(2) K, space group P21, Z = 2, Flack parameter = 0.13(4), 17027 reflections measured, 7995 independent reflections (Rint = 0.0207). The final R1 values were 0.0398 (I > 2σ(I)). The final wR(F2) values were 0.0998 (I > 2σ(I)). The final wR(F2) values were 0.1053 (all data). The goodness of fit on F2 was 1.050.
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78651330170
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(a) For definitions of three-letter abbreviations, see Reticular Chemistry Structure Resource (
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(a) For definitions of three-letter abbreviations, see Reticular Chemistry Structure Resource (http://rcsr.anu.edu.au/ )
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78651304399
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0037037520
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Colacio, E.1
Kivekas, R.2
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Sunberg, M.4
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Bardaji, M.6
Laguna, A.7
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