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用过氧化物法合成了 [Co(3,3-tri)(amp)Cl][ZnCl4]的两个经式异构体,晶体结构解析表明两者互为差向异构体。其中反式异构体 (仲氢相对于 Cl)晶体属单斜晶系,空间群 C2/c, a=2.7663(7)nm, b=0.9505(1)nm, c=1.8288(4)nm,β =105.57(2)°, V=4.632(1)nm3, Dc=1.706g· cm-3, Z=8, F000=2432.00,μ (MoKα )=23.51cm-1, R=0.033, Rw=0.041;顺式异构体 (仲氢相对于 Cl)晶体属三斜晶系,空间群, a=1.0790(2)nm, b=1.1749(1)nm, c=0.8920(1)nm,α =90.73(1)°,β =109.573(9)°,γ =80.60(1)°, V=1.0500(2)nm3, Dc=1.71g· cm-3, Z=2, F000=548.00,μ (MoKα )=25.73cm-1, R=0.022, Rw=0.030。两异构体中 Co3+为六配位,其差异仅表现在 3,3-tri仲胺上氢的取向不同。
Two formal isomers of [Co (3,3-tri) (amp) Cl] [ZnCl4] have been synthesized by peroxide method. The crystal structure analysis shows that they are epimers. The crystal of trans isomer (para to hydrogen relative to Cl) is monoclinic with space group C2 / c, a = 2.7663 (7) nm, b = 0.9505 (1) nm and c = 1.8288 β = 105.57 (2) °, V = 4.632 (1) nm3, Dc = 1.706 g · cm -3, Z = 8, F000 = 2432.00, μ (MoKα) = 23.51 cm -1, R = 0.033, Rw = 0.041 ; The cis isomer (para to hydrogen relative to Cl) crystals are triclinic with a = 1.0790 (2) nm, b = 1.1749 (1) nm, c = 0.8920 (1) ° β = 109.573 (9) ° γ = 80.60 (1) ° V = 1.0500 (2) nm3 Dc = 1.71 g · cm -3 Z = 2 F000 = 548.00 μ (MoKα) = 25.73 cm-1, R = 0.022, Rw = 0.030. The two isomers of Co3 + hexacoordination, the difference is only manifested in 3,3-tri secondary amine on the hydrogen orientation.