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39
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70350566494
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Synthesis. Complexes 1-4 were prepared by using a similar procedure as described below. To a DMF (5 mL) solution of 3,4-Hpybz (0.05 mmol) was added a CH3OH (10 mL) solution of metal salt (0.10 mmol, MnCl2·4H2O for 1, Zn(NO3)2·6H2O for 2, Cd(NO3)2·4H2O for 3, and Pb(NO3)2 for 4, After stirring for ca. 30 min, the mixture was filtered and left to stand at room temperature. Colorless block (for 1-3) or needle-shaped (for 4) crystals were obtained by slow evaporation of the solvents for ca. two weeks. Yield: 43% for 1, 51% for 2, 39% for 3, and 66% for 4. Anal. Calcd for C48H34Mn2N4O9 (1, Mr=920.67, C, 62.62; H, 3.72; N, 6.09, Found: C, 62.50; H, 3.64; N, 6.16, IR cm-1, 3447b, 1619vs, 1556s, 1426s, 1398vs, 1328s, 1192m, 1101m, 1031m, 1006m, 817s, 780s, 754s, 705s, 643m, 473s. An
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-1): 1594s, 1548s, 1432w, 1353vs, 1195m, 1130m, 1003w, 867w, 843m, 778s, 703m, 667w, 622w, 551w, 528w, 474 m.
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40
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70350572152
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Crystallographic data for 1: C48H34Mn2N4O9, M=920.67, 0.18×0.14×0.13 mm3, monoclinic, space group C2/c, a=11.982(3, b=15.316(4, c=21.926(5) Å, β=95.607(4)°, V=4005(2) Å3, Z=4, Dc=1.527 g/cm3, F(000)=1888, GOF=1.141, μ=0.698 mm-1, R=0.0670, and wR=0.1607. Crystallographic data for 2: C48H34Zn2N4O9, M=941.57, 0.24×0.20×0.18 mm3, monoclinic, space group C2/c, a=11.863(2, b=15.487(3, c=21.635(5) Å, β=94.938(4)°, V=3960(1) Å3, Z=4, Dc=1.579 g/cm3, F(000)=1928, GOF=1.048, μ=1.279 mm-1, R=0.0274, and wR=0.0661. Crystallographic data for 3: C48H34Cd2N4O9, M=1035.61, 0.24×0.22×0.18 mm3, monoclinic, space group C2/c, a=12.0223
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-1, R=0.0160, and wR=0.0353.
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43
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20444450209
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Xu Y.-Q., Yuan D.-Q., Han L., Ma E., Wu M.-Y., Lin Z.-Z., and Hong M.-C. Eur. J. Inorg. Chem. (2005) 2054
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34250758147
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34248392311
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48
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70350570345
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For the three-letter net codes, see
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For the three-letter net codes, see Ref. [5] and the associated website 〈http://rcsr.anu.edu.au/〉.
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5] and the associated website
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Ref1
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50
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70350564123
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2/ncm.
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2/ncm.
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