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Crystallographic analysis: 2 (C90H24Cl 3Cu13N102O18, Mr, 3754.48, green crystal, 0.36 x 0.28 x 0.24 mm3, cubic, space group Pm3m (no. 221, a, 18.595(7) Å, V =6430(4) Å3, Z, 1, F(000, 1850, ρcalcd, 0.970 g cm-3, μMoKα, 1.136 mm-1, λ-(MoKα, 0.71073 Å, T, 159(2) K, 18413 reflections collected (2θmax, 44.83°, 953 independent (Rint, 0.0869, 0 restraints, 62 parameters, wR2, 0.1538 (I > 2σ(I, wR2, 0.1650 (all data, R1, 0.0726 (I > 2 σI, GOF, 1.086. A crystal of 2 was coated with Paratone-N oil, attached to a Kapton loop, transferred to a Siemens SMART APEX diffractometer, and cooled in a nitro
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1, = 0.0726 (I > 2 σ(I)), GOF = 1.086. A crystal of 2 was coated with Paratone-N oil, attached to a Kapton loop, transferred to a Siemens SMART APEX diffractometer, and cooled in a nitrogen stream. A full hemisphere of data was collected, and the unit-cell parameters were refined against all data. The crystal did not show significant decay during data collection. Data were integrated and corrected for Lorentz and polarization effects using SAINT 7.07b, and were corrected for absorption effects using SADABS 2.10. The space-group assignment was based upon systematic absences, E statistics, and successful refinement of the structure. The structure was solved by direct methods and expanded through successive difference Fourier maps. It was refined against all data using the SHELXTL 5.0 software package. Hydrogen atoms were inserted at idealized positions and refined using a riding model with an isotropic thermal parameter 1.2 times that of the attached carbon atom. Thermal parameters for all non-hydrogen atoms in the framework skeleton were refined anisotropically. The oxygen, nitrogen, and methyl carbon atoms in each DMF molecule were disordered over four equivalent sites around the crystallographic four-fold rotation axis, and were consequently refined with 25 % of the normal occupancies. CCDC-624533 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/data_request/cif.
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