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34249692233
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2O (67 mg, 0.3 mmol), and the resulting solution was heated at 60°C for 20 min. The solution was allowed to stand for several days, and dark-brown columnar crystals of 1 were obtained (yield: 23%).
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52: C, 28.60; H, 3.67; N, 4.90. Found: C, 28.40; H, 3.38; N, 5.15.
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23
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34249682304
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Crystal data for 1: C64H84N 12Cu8Mn12O70, tetragonal I41/amd, a, 24.702(2) Å, c, 20.365(3) Å, V, 12427(2) Å3, Z, 4, d calcd, 1.769 Mg m-3, T, 100 K, λ(synchrotron, 1.000 00 Å, 18 848 reflections measured, 3979 unique reflections (Rint, 0.0310, Final R1, 0.0690 and wR2, 0.2169 [I > 2σ(I, X-ray diffraction data were obtained with a Weissenberg-type imaging plate detector. Crystal data for 2: C68H88CuioMN10O58, dark-brown lozenge (0.4 x 0.15 x 0.1 mm3, M, 2938.55, triclinic P1, a, 14.208(3) Å, b, 14.344-(3) Å, c, 15.912(3) Å, α, 77.549(3)°, β, 64.388(3)°, γ, 75.093-(4)°, V, 2805.59
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int = 0.0226). Final R1 = 0.0570 and wR2 = 0.1697 using reflections with I > 2σ(I).
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24
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0036215663
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MEM analysis was performed with the Enigma program (Tanaka, H.; Tanaka, M.; Nishibori, E.; Kato, K.; Iishi, T.; Sakata, M. J. Appl. Crystallogr. 2002, 35, 282) at a resolution of 128 x 128 x 128 pixels, and the R factor of the final MEM charge density was 0.046.
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MEM analysis was performed with the Enigma program (Tanaka, H.; Tanaka, M.; Nishibori, E.; Kato, K.; Iishi, T.; Sakata, M. J. Appl. Crystallogr. 2002, 35, 282) at a resolution of 128 x 128 x 128 pixels, and the R factor of the final MEM charge density was 0.046.
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25
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34249680525
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Electron counting on each Mn ion was performed within the particular compartment of the space (Voronoi cell), which was defined as a region surrounded by perpendicular bisecting planes of bonds between Mn and neighboring O nuclei. Guerra, C. F.; Handgraaf, J.-W.; Baerends, E. J.; Bicelhaupt, F. M. J. Comput. Chem. 2004, 25, 189.
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Electron counting on each Mn ion was performed within the particular compartment of the space (Voronoi cell), which was defined as a region surrounded by perpendicular bisecting planes of bonds between Mn and neighboring O nuclei. Guerra, C. F.; Handgraaf, J.-W.; Baerends, E. J.; Bicelhaupt, F. M. J. Comput. Chem. 2004, 25, 189.
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16844381084
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