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Crystal structure determination: [(DMT-TTF-py)2Cu2(OAc)4]·2C6H6 (1), Mw = 1422.86, monoclinic, space group P21/c with a = 28.767(8), b = 13.198(4), c = 8.482(3) Å, β = 92.273(9) °, V = 3217.7(12) Å3. Z = 2, F000 = 1468; R1 for 4506 reflections [I > 2σ(I)] = 0.1034, wR2 for all 5668 unique = 0.2568, GOF 1.174. [(DMT-TTF-py)2Cu(PhCOO)2(CH3OH)2]·2CH2Cl2 (2), Mw = 1286.87, monoclinic, space group P21/c with a = 14.180(3), b = 19.139(4), c = 10.430(2) Å, β = 108.962(5)°, V = 2677(1) Å3. Z = 2, F000 = 1318; R1 for 3735 reflections [I > 2σ(I)] = 0.1200, wR2 for all 4898 unique = 0.2949, GOF 1.169.
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