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邻甲基苯荒酸四乙基铵盐分别与硝酸银和氯化铜反应,经毗啶重结晶,得到四核银簇合物Ag_4(o-CH_3C_6H_4CS_2)_4(Py)_4(晶体Ⅰ)和二核铜化合物Cu_2(o-CH_3-C_6H_4CSS_2)_2(Py)_(晶体Ⅱ)。用X射线单晶衍射法测定了它们的晶体结构。晶体Ⅰ的空间群为P2/n。晶胞参数:a=14.757(4),b=12.231(3),c=15.183(4)A,β=91.14(2)°,V=2739.95A~3,Z=2。2590个衍射点参与修正,最终偏差因子R=0.087。晶体Ⅱ的空间群为C_1~1-P1。晶胞参数:a=9.307(7),b=9.546(7),c=10.119(8)A,α=95.06(9),β=109.74(10),γ=118.86(10)°,V=705.94A~3,Z=1。1198个衍射点参与修正,最终偏差因子R=0.086。 Ag_4(o-CH_3C_6H_4CS_2)_4(Py)_4分子中Ag_4呈蝴蝶状构型,其配位情况与四核银簇合物Ag_4(a-C_(10)H_7CS_2)_4(Py)_4相似。Cu_2(o-CH_3C_6H_4CSS_2)_2(Py)_2分子构型与Cu_2(a-C_(10)H_7CSS_2)_2(Py)_2十分相似。Cu—Cu键长为2.608A。而且邻甲基苯荒酸与Cu~(2+)反应包括一个氧化还原反应,也与a-萘荒酸与Cu~(2+)反应相似。可以认为邻甲基苯荒酸与a-萘荒酸有相似的空间效应和电子效应。
O-methylbenzenesulfonic acid tetraethylammonium salt was reacted with silver nitrate and copper chloride, respectively, and then recrystallized from pyridine to obtain tetragonal silver cluster Ag_4 (o-CH_3C_6H_4CS_2) _4 (Py) _4 (crystal Ⅰ) and Cu_2 (o-CH_3-C_6H_4CSS_2) _2 (Py) _ (Crystal Ⅱ). Their crystal structures were determined by X-ray single crystal diffraction. The space group I is P2 / n. Cell parameters: a = 14.757 (4), b = 12.231 (3), c = 15.183 (4) A, β = 91.14 (2) °, V = 2739.95A -3, Z = 2.2590 diffraction spots Correction, the final deviation factor R = 0.087. The space group Ⅱ is C_1 ~ 1-P1. Cell parameters: a = 9.307 (7), b = 9.546 (7), c = 10.119 (8) A, α = 95.06 (9), β = 109.74 (10), γ = 118.86 (10) °, 705.94A ~ 3, Z = 1.1198 diffraction points involved in the amendment, the final deviation factor R = 0.086. Ag_4 has a butterfly-like configuration in Ag_4 (o-CH_3C_6H_4CS_2) _4 (Py) _4, and its coordination is similar to that of Ag_4 (a-C_ (10) H_7CS_2) _4 (Py) _4. The structure of Cu_2 (o-CH_3C_6H_4CSS_2) _2 (Py) _2 is very similar to Cu_2 (a-C_ (10) H_7CSS_2) _2 (Py) _2. Cu-Cu bond length of 2.608A. Moreover, the reaction of o-methylbenzoic acid with Cu 2+ includes a redox reaction, which is also similar to the reaction of a-naphthalene and Cu 2+. It can be considered that ortho-methylbenzoic acid has a similar spatial and electronic effect as a-naphthalene-less acid.