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Crystal data for 3: C54H16F 20N6 (Mr, 1129, monoclinic, space group P21/c (No. 14, a, 13.653(5, b, 10.545(3, c, 18.317(7) Å, β, 106.974(15)°, V, 2522.3(14) Å3, Z, 2, ρcalcd, 1.486 gcm-3, T, 123(2) K, R1, 0.0459 (I > 2σ(I, RW, 0.1534 (all data, GOF, 1.119. In this crystal structure there are disordered solvent molecules, and their contribution to the scattering values have been removed by using the PLATON SQUEEZE program.[22] Crystal data for 4: C54H 17F20N6O-(C7H16)(C 6H5CH3, Mr, 1374, orthorhombic, space group Pbcn (No. 60, a, 10.8232(10, b, 35.6043, c
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W = 0.3290 (all data), GOF = 1.218. Since the crystals of 5 were grown from [D]TFA, N-H protons in the crystal structure were replaced by deuterium atoms. CCDC 693211 (3), 693212 (4), and 693213 (5) contain 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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