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84906358329
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2 (0.203 g, 0.50 mmol) in 6.25 mL of water. Dark-green single crystals suitable for X-ray structure analysis were grown for a few days at room temperature. Anal, calcd for 1: C, 44.75; H, 4.36; N, 8.70. Found; C, 44.57; H, 4.64: N, 8.92. Anal, calcd For 2: C, 43.82; H, 4.83; N, 8.18. Found: C, 43.34; H. 4.93; N, 7.79.
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2 (0.203 g, 0.50 mmol) in 6.25 mL of water. Dark-green single crystals suitable for X-ray structure analysis were grown for a few days at room temperature. Anal, calcd for 1: C, 44.75; H, 4.36; N, 8.70. Found; C, 44.57; H, 4.64: N, 8.92. Anal, calcd For 2: C, 43.82; H, 4.83; N, 8.18. Found: C, 43.34; H. 4.93; N, 7.79.
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84906372764
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Sheldrick, G. M. SHELXTL-97. Program for Structure Refinement, University of Göttingen, Göttingen, Germany, 1998.
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Sheldrick, G. M. SHELXTL-97. Program for Structure Refinement, University of Göttingen, Göttingen, Germany, 1998.
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84906358330
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All crystallographic measurements were made on Bruker SMART APEX CCD area detectors with graphite-monochromated Mo Kα radiation (λ, 0.71073 Å for 1 and 2) operated at 1500 W power (50 kV, 30 mA, Both structures were solved by direct method and full-matrix least-squares analysis (SHELXTL-97, Anisotropic thermal factors were assigned to all the non-hydrogen atoms. Crystal data for 1: C27H36CuN 4O11S2, monoclinic, space group P2 1 (No. 4, a, 7.890(50, b, 15.945(50, c, 13.063(50) Å, β, 94.588(5)°, V, 1638.1(13) Å3, Z, 2, Mw, 720.26, Dc, 1.46 g cm-3. The final R1 and wR 2 are 0.0690 and 0.1841 for 401 parameters and 7832 independent reflections. For 2: C52H72Cu2N 8O22S4
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2 are 0.0468 and 0.1272 for 435 parameters and 6214 independent reflections. The data collection was performed at 140 K (1) and 295 K (2) on Bruker Smart CCD. Data collection for 1 was also performed at 295 K and the framework structure was almost the same as that at 140 K. The lattice constants along the a and b axis are a little longer, and along the c axis a little shorter than that at 140 K. The unit cell volume of 1 at 295 K is 1.018 times that at 140 K.
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