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Cu2(μ-I)2(μ-1,8-nap)(PPh3) 2, 1, To the solution obtained by dissolving CuI (39.8 mg, 0.21 mmol) and PPh3 (131.8 mg, 0.50 mmol) in CH3CN (16 mL) was added 1,8-nap (13.9 mg, 0.11 mmol) to obtain a clear orange solution. After 1 week, red crystals were deposited in 40% yield (45.6 mg, Anal. Calcd for C 44H36N2Cu2I2P 2: C, 51.03; H, 3.50; N, 2.70. Found: C, 50.77; H, 3.59; N, 2.7, Cu2(μ-Br)2(μ-nap)(PPh3)2, 2, To the solution obtained by dissolving CuBr (24.8 mg, 0.17 mmol) and PPh3 (45.7 mg, 0.17 mmol) in CH3CN (16 mL) was added 1,8-nap (11.1 mg, 0.085 mmol) to obtain a clear orange solution. After 1 week, red crystals were deposited in 55% yield 43.4 mg, Anal. Calcd for C 44H36N2Cu2I2P 2: C, 56.12; H
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2: C, 56.12; H, 3.85; N, 2.98. Found: C, 56.24; H, 4.03; N, 3.05. 1 and 2 were substantially insoluble in common organic solvents such as acetonitrile, chloroform, dichloromethane, N,N-dimethylformamide, dimethyl sulfoxide, tetrahydrofuran, and alcohols, which prevented measurement of their properties in solution.
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Crystal data for 1: C44H36Cu 2I2N2P2, M, 1035.63, monoclinic, space group P21/a, a, 18.068(2) Å, b, 9.9984(7) Å, c, 23.394(2) Å, β, 107.103(4)°, V, 4039.3(6) Å3, Z, 4, T, 120°C, 17 545 measured reflections and 7815 independent reflections, and R1, 0.0285 and wR2, 0.0879 for 7350 observed reflections [I > 2σ(I, and 469 parameters. Crystal data for 2: C44H36Cu2Br2N 2P2, M, 941.63, monoclinic, space group P21/a, a, 17.766(3) Å, b, 9.701-(2) Å, c, 23.392(4) Å, β, 107.009(3)°, V, 3855(1) Å3, Z, 4, T, 170°C, 23 521 measured reflections and 8470 independent reflections, and R1, 0
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3, Z = 4, T = -170°C, 23 521 measured reflections and 8470 independent reflections, and R1 = 0.0277 and wR2 = 0.0697 for 6921 observed reflections [I > 2σ(I)] and 469 parameters.
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(a) Maekawa, M.; Munakata, M.; Kitagawa, S.; Kuroda-Sowa, T.; Suenaga, Y.; Yamamoto, M. Inorg. Chim. Acta 1998, 271, 129.
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Maekawa, M.1
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Kitagawa, S.3
Kuroda-Sowa, T.4
Suenaga, Y.5
Yamamoto, M.6
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(b) Munakata, M.; Maekawa, M.; Kitagawa, S.; Adachi, M.; Masuda, H. Inorg. Chim. Acta 1990, 167, 181.
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Kitagawa, S.3
Adachi, M.4
Masuda, H.5
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Preliminary measurements using an integrating sphere showed that the quantum yield of the iodide complex 1 is ca. 0.2 whereas that of the bromide complex 2 is lower than 0.05
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Preliminary measurements using an integrating sphere showed that the quantum yield of the iodide complex 1 is ca. 0.2 whereas that of the bromide complex 2 is lower than 0.05.
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33751157567
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Vitale, M.; Ryu, C. K.; Palke, W. E.; Ford, P. C. Inorg. Chem. 1994, 33, 561.
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Vitale, M.1
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Frisch, M. J, Trucks, G. W, Schlegel, H. B, Scuseria, G. E, Robb, M. A, Cheeseman, J. R, Montgomery, J. A, Jr, Vreven, T, Kudin, K. N, Burant, J. C, Millam, J. M, Iyengar, S. S, Tomasi, J, Barone, V, Mennucci, B, Cossi, M, Scalmani, G, Rega, N, Petersson, G. A, Nakatsuji, H, Hada, M, Ehara, M, Toyota, K, Fukuda, R, Hasegawa, J, Ishida, M, Nakajima, T, Honda, Y, Kitao, O, Nakai, H, Klene, M, Li, X, Knox, J. E, Hratchian, H. P, Cross, J. B, Bakken, V, Adamo, C, Jaramillo, J, Gomperts, R, Stratmann, R. E, Yazyev, O, Austin, A. J, Cammi, R, Pomelli, C, Ochterski, J. W, Ayala, P. Y, Morokuma, K, Voth, G. A, Salvador, P, Dannenberg, J. J, Zakrzewski, V. G, Dapprich, S, Daniels, A. D, Strain, M. C, Farkas, O, Malick, D. K, Rabuck, A. D, Raghavachari, K, Foresman, J. B, Ortiz, J. V, Cut, Q, Baboul, A. G, Clifford, S, Cioslowski, J, Stefanov, B. B, Liu, G, Liashenko, A, Piskorz, P, Komaromi, I, Martin, R. L, Fox, D. J, Keit
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Frisch, M. J.; Trucks, G. W.; Schlegel, H. B.; Scuseria, G. E.; Robb, M. A.; Cheeseman, J. R.; Montgomery, J. A., Jr.; Vreven, T.; Kudin, K. N.; Burant, J. C.; Millam, J. M.; Iyengar, S. S.; Tomasi, J.; Barone, V.; Mennucci, B.; Cossi, M.; Scalmani, G.; Rega, N.; Petersson, G. A.; Nakatsuji, H.; Hada, M.; Ehara, M.; Toyota, K.; Fukuda, R.; Hasegawa, J.; Ishida, M.; Nakajima, T.; Honda, Y.; Kitao, O.; Nakai, H.; Klene, M.; Li, X.; Knox, J. E.; Hratchian, H. P.; Cross, J. B.; Bakken, V.; Adamo, C.; Jaramillo, J.; Gomperts, R.; Stratmann, R. E.; Yazyev, O.; Austin, A. J.; Cammi, R.; Pomelli, C.; Ochterski, J. W.; Ayala, P. Y.; Morokuma, K.; Voth, G. A.; Salvador, P.; Dannenberg, J. J.; Zakrzewski, V. G.; Dapprich, S.; Daniels, A. D.; Strain, M. C.; Farkas, O.; Malick, D. K.; Rabuck, A. D.; Raghavachari, K.; Foresman, J. B.; Ortiz, J. V.; Cut, Q.; Baboul, A. G.; Clifford, S.; Cioslowski, J.; Stefanov, B. B.; Liu, G.; Liashenko, A.; Piskorz, P.; Komaromi, I.; Martin, R. L.; Fox, D. J.; Keith, T.; Al-Laham, M. A.; Peng, C. Y.; Nanayakkara, A.; Challacombe, M.; Gill, P. M. W.; Johnson, B.; Chen, W.; Wong, M. W.; Gonzalez, C.; Pople, J. A. Gaussian 03, revision C.02; Gaussian, Inc.: Wallingford, CT, 2004.
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TD-DFT calculations show that the energies and oscillator strengths of S0 → S1 are 1.04 eV (1193 nm) and 0.0008 and 1.07 eV (1162 nm) and 0.0005 for iodide and bromide complexes, respectively (Tables S4 and S5 in the Supporting Information, However, the substantially lowest allowed transitions are S0 → S7; their calculated energies and oscillator strengths are 2.22 eV (559 nm) and 0.0355 and 2.31 eV (536 nm) and 0.0404 for iodide and bromide complexes, respectively. Besides the acceptable oscillator strengths, considerable agreement of the calculated and observed energies also supports the assignments of the lowest absorptions of 1 and 2. The S0 → S1 and S0 → S7 transitions mainly correspond to HOMO-LUMO and (H, 5)-LUMO transitions for both iodide and bromide complexes Tables S4 and S5 in the Supporting Information
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7 transitions mainly correspond to HOMO-LUMO and (H - 5)-LUMO transitions for both iodide and bromide complexes (Tables S4 and S5 in the Supporting Information).
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Using the single-crystal structure data, we calculate the transition energies of the pyridine complexes, Cu2X2}(PPh 3)2(pyridine)2, which have diamond {Cu 2X2} cores. The oscillator strengths of S0 → S1, which correspond to the HOMO-LUMO transition, are 0.0183 and 0.0191 for X, I and Br, respectively
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1, which correspond to the HOMO-LUMO transition, are 0.0183 and 0.0191 for X = I and Br, respectively.
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