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The Importance of Synthetic Conditions on Manganese-Based 12-Metallacrown-4 Formation
Journal of Chemical Crystallography ( IF 0.8 ) Pub Date : 2020-07-06 , DOI: 10.1007/s10870-020-00843-4
David L. Helm , Matthias Zeller , Curtis M. Zaleski

Abstract Alterations to synthetic conditions either by varying stochiometric ratios of the reactants or solvent choice yield two new metallacrowns (MCs): Mn(Hsal) 2 [12-MC Mn III (N)shi -4](DMF) 6 ·4DMF, 1 , where − Hsal is salicylate, shi 3− salicylhydroximate, and DMF is N , N -dimethylformamide, and {Na 2 (OAc) 2 [12-MC Mn III (N)shi -4](MeOH) 4 (H 2 O) 2 2MeOH} n , 2 , where − OAc is acetate and MeOH is methanol. Compound 1 crystallizes in the monoclinic space group C 2/c with a = 19.0264 (6) Å, b = 23.1440 (8) Å, c = 18.6704 (5) Å, α = 90°, β = 90.3600 (10)°, γ = 90°, V = 8221.3 (4) Å 3 , and Z = 4. Compound 2 crystallizes in the triclinic space group P $$\stackrel{-}{1}$$ 1 - with a = 7.8995 (7) Å, b = 11.2374 (10) Å, c = 14.5559 (13) Å, α = 112.535 (3)°, β = 91.987 (3)°, γ = 98.558 (3)°, V = 1174.22 (18) Å 3 , and Z = 1. Compound 1 is a discrete metallacrown molecule that contains four ring Mn III ions and a Mn II ion captured in the metallacrown central cavity. The Mn II ion is tethered to the metallacrown via two salicylate bridges that also bridge to the ring Mn III ions. Compound 2 is a one-dimensional chain of metallacrowns. The metallacrown consists of four ring Mn III ions and two sodium ions which are bound on opposite faces of the metallacrown cavity. Each di-sodium metallacrown is then linked to neighboring metallacrowns through acetate anion bridges to form a one-dimensional chain. Graphic Abstract The complex Na 2 (OAc)2[12-MC Mn III (N)shi -4](MeOH) 4 (H 2 O) 2 ·2MeOH forms a one-dimensional chain of metallacrowns by linking together neighboring metallacrowns through acetate anion bridges.

中文翻译:

合成条件对锰基 12-Metallacrown-4 地层的重要性

摘要 通过改变反应物的化学计量比或溶剂选择来改变合成条件会产生两种新的金属冠 (MC):Mn(Hsal) 2 [12-MC Mn III (N)shi -4](DMF) 6 ·4DMF, 1 ,其中-Hsal是水杨酸盐,shi 3-水杨酸羟肟酸盐,DMF是N,N-二甲基甲酰胺,和{Na 2 (OAc) 2 [12-MC Mn III (N)shi -4](MeOH) 4 (H 2 O ) 2 2MeOH} n , 2 ,其中 - OAc 是醋酸盐,MeOH 是甲醇。化合物 1 在单斜空间群 C 2/c 中结晶,a = 19.0264 (6) Å, b = 23.1440 (8) Å, c = 18.6704 (5) Å, α = 90°, β = 90.3600 (10)°, γ = 90°,V = 8221.3 (4) Å 3 ,Z = 4。化合物 2 在三斜空间群 P $$\stackrel{-}{1}$$ 1 - 结晶,a = 7.8995 (7) Å , b = 11.2374 (10) Å, c = 14.5559 (13) Å, α = 112.535 (3)°, β = 91.987 (3)°, γ = 98.558 (3)°, V = 1174.22 (18) Å并且 Z = 1。化合物 1 是一个离散的金属冠分子,它包含四个环 Mn III 离子和一个捕获在金属冠中心腔中的 Mn II 离子。Mn II 离子通过两个水杨酸盐桥连接到金属冠上,该桥也桥接到环 Mn III 离子。化合物 2 是一维金属冠链。金属冠由四个环 Mn III 离子和两个钠离子组成,它们结合在金属冠腔的相对面上。每个二钠金属冠然后通过乙酸根阴离子桥连接到相邻的金属冠以形成一维链。图形摘要 络合物 Na 2 (OAc)2[12-MC Mn III (N)shi -4](MeOH) 4 (H 2 O) 2 ·2MeOH 通过乙酸将相邻的金属冠连接在一起,形成一维金属冠链阴离子桥。
更新日期:2020-07-06
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